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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Jon Zubieta'
_publ_contact_author_email       JAZUBIET@SYR.EDU

_publ_section_title              
;
Hydrothermal Chemistry of Vanadium Oxides
with Aromatic di- and tri-Phosphonates in the Presence
of Secondary Metal-Organic Subunits
;
loop_
_publ_author_name
'Jon Zubieta'
'Paul DeBurgomaster'
'Hongxue Liu.'
"Charles O'Connor"
'Wayne Ouellette'

# Attachment 'AllCIFrevised[Zubieta].doc'

data_1
_database_code_depnum_ccdc_archive 'CCDC 734621'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H20 Cu2 N4 O11 P2 V2'
_chemical_formula_sum            'C30 H20 Cu2 N4 O11 P2 V2'
_chemical_formula_weight         903.40

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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/n
_symmetry_space_group_name_Hall  -P2yac

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

_cell_length_a                   9.5731(9)
_cell_length_b                   9.5962(10)
_cell_length_c                   16.5163(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.070(2)
_cell_angle_gamma                90.00
_cell_volume                     1511.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3090
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.20

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_T_max  0.8810
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            14518
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         28.00
_reflns_number_total             3643
_reflns_number_gt                3600
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0156P)²+23.7794P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         3643
_refine_ls_number_parameters     232
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0968
_refine_ls_wR_factor_ref         0.1847
_refine_ls_wR_factor_gt          0.1843
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_restrained_S_all      1.409
_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 0.77464(9) 0.63071(9) 0.00801(5) 0.0077(2) Uani 1 1 d . . .
V1 V 1.10826(13) 0.24430(12) 0.17116(7) 0.0096(3) Uani 1 1 d . . .
P1 P 1.06081(18) 0.55874(18) 0.11515(11) 0.0076(4) Uani 1 1 d . . .
O1 O 0.9288(5) 0.6405(6) 0.0910(3) 0.0129(10) Uani 1 1 d . . .
O2 O 1.1537(5) 0.5284(5) 0.0477(3) 0.0117(10) Uani 1 1 d . . .
O3 O 1.0273(5) 0.4207(5) 0.1605(3) 0.0090(9) Uani 1 1 d . . .
O4 O 1.2500 0.2447(8) 0.2500 0.026(2) Uani 1 2 d S . .
O5 O 0.9878(6) 0.1349(6) 0.1916(3) 0.0193(12) Uani 1 1 d . . .
O6 O 1.1631(6) 0.2041(6) 0.0831(3) 0.0174(11) Uani 1 1 d . . .
N1 N 0.6693(6) 0.7759(6) 0.0682(4) 0.0101(12) Uani 1 1 d . . .
N2 N 0.5834(6) 0.6091(6) -0.0533(4) 0.0099(11) Uani 1 1 d . . .
C1 C 1.2500 0.8766(11) 0.2500 0.014(2) Uani 1 2 d S . .
H1 H 1.2500 0.9735 0.2500 0.017 Uiso 1 2 calc SR . .
C2 C 1.1597(8) 0.8048(7) 0.1940(4) 0.0118(14) Uani 1 1 d . . .
H2 H 1.0982 0.8540 0.1578 0.014 Uiso 1 1 calc R . .
C3 C 1.1610(7) 0.6600(7) 0.1917(4) 0.0088(13) Uani 1 1 d . . .
C4 C 1.2500 0.5918(10) 0.2500 0.0087(18) Uani 1 2 d S . .
H4 H 1.2500 0.4949 0.2500 0.010 Uiso 1 2 calc SR . .
C16 C 0.5426(7) 0.5249(8) -0.1136(4) 0.0109(14) Uani 1 1 d . . .
H16 H 0.6062 0.4589 -0.1291 0.013 Uiso 1 1 calc R . .
C15 C 0.4081(8) 0.5288(7) -0.1562(4) 0.0113(14) Uani 1 1 d U . .
H15 H 0.3841 0.4686 -0.1993 0.014 Uiso 1 1 calc R . .
C14 C 0.3150(8) 0.6239(8) -0.1320(5) 0.0168(15) Uani 1 1 d . . .
H14 H 0.2256 0.6286 -0.1589 0.020 Uiso 1 1 calc R . .
C12 C 0.3509(8) 0.7143(8) -0.0674(5) 0.0136(14) Uani 1 1 d . . .
C13 C 0.4889(7) 0.7049(8) -0.0302(4) 0.0114(14) Uani 1 1 d . . .
C11 C 0.2584(8) 0.8168(9) -0.0363(5) 0.0157(15) Uani 1 1 d . . .
H11 H 0.1673 0.8251 -0.0604 0.019 Uiso 1 1 calc R . .
C10 C 0.3005(8) 0.9001(8) 0.0263(4) 0.0141(15) Uani 1 1 d . . .
H10 H 0.2383 0.9648 0.0447 0.017 Uiso 1 1 calc R . .
C8 C 0.4418(8) 0.8907(8) 0.0657(5) 0.0133(14) Uani 1 1 d . . .
C9 C 0.5346(8) 0.7916(7) 0.0358(4) 0.0117(14) Uani 1 1 d . . .
C7 C 0.4949(9) 0.9734(8) 0.1306(5) 0.0170(15) Uani 1 1 d . . .
H7 H 0.4381 1.0396 0.1525 0.020 Uiso 1 1 calc R . .
C6 C 0.6307(8) 0.9566(8) 0.1619(4) 0.0152(15) Uani 1 1 d . . .
H6 H 0.6670 1.0124 0.2047 0.018 Uiso 1 1 calc R . .
C5 C 0.7151(8) 0.8562(8) 0.1298(4) 0.0160(15) Uani 1 1 d . . .
H5 H 0.8068 0.8453 0.1525 0.019 Uiso 1 1 calc R . .


_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 1.926(5) . ?
Cu1 O2 1.939(5) 3_765 ?
Cu1 N2 2.023(6) . ?
Cu1 N1 2.031(6) . ?
Cu1 O6 2.301(5) 3_765 ?
V1 O5 1.617(6) . ?
V1 O6 1.635(5) . ?
V1 O4 1.7957(12) . ?
V1 O3 1.863(5) . ?
P1 O1 1.511(5) . ?
P1 O2 1.514(5) . ?
P1 O3 1.569(5) . ?
P1 C3 1.803(7) . ?
O2 Cu1 1.939(5) 3_765 ?
O4 V1 1.7957(12) 2_755 ?
O6 Cu1 2.301(5) 3_765 ?
N1 C5 1.319(9) . ?
N1 C9 1.360(9) . ?
N2 C16 1.315(9) . ?
N2 C13 1.367(9) . ?
C1 C2 1.392(9) . ?
C1 C2 1.392(9) 2_755 ?
C1 H1 0.9300 . ?
C2 C3 1.391(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(8) . ?
C4 C3 1.391(8) 2_755 ?
C4 H4 0.9300 . ?
C16 C15 1.413(10) . ?
C16 H16 0.9300 . ?
C15 C14 1.361(11) . ?
C15 H15 0.9300 . ?
C14 C12 1.393(11) . ?
C14 H14 0.9300 . ?
C12 C13 1.409(10) . ?
C12 C11 1.448(10) . ?
C13 C9 1.410(10) . ?
C11 C10 1.340(11) . ?
C11 H11 0.9300 . ?
C10 C8 1.452(10) . ?
C10 H10 0.9300 . ?
C8 C7 1.392(11) . ?
C8 C9 1.419(10) . ?
C7 C6 1.366(11) . ?
C7 H7 0.9300 . ?
C6 C5 1.392(10) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?

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 O2 95.5(2) . 3_765 ?
O1 Cu1 N2 164.5(2) . . ?
O2 Cu1 N2 91.4(2) 3_765 . ?
O1 Cu1 N1 90.0(2) . . ?
O2 Cu1 N1 169.9(2) 3_765 . ?
N2 Cu1 N1 81.3(2) . . ?
O1 Cu1 O6 101.9(2) . 3_765 ?
O2 Cu1 O6 96.3(2) 3_765 3_765 ?
N2 Cu1 O6 91.1(2) . 3_765 ?
N1 Cu1 O6 90.9(2) . 3_765 ?
O5 V1 O6 108.8(3) . . ?
O5 V1 O4 110.9(3) . . ?
O6 V1 O4 111.3(2) . . ?
O5 V1 O3 108.1(3) . . ?
O6 V1 O3 107.1(2) . . ?
O4 V1 O3 110.4(3) . . ?
O1 P1 O2 116.0(3) . . ?
O1 P1 O3 111.3(3) . . ?
O2 P1 O3 110.3(3) . . ?
O1 P1 C3 106.6(3) . . ?
O2 P1 C3 108.0(3) . . ?
O3 P1 C3 103.8(3) . . ?
P1 O1 Cu1 137.1(3) . . ?
P1 O2 Cu1 139.1(3) . 3_765 ?
P1 O3 V1 135.3(3) . . ?
V1 O4 V1 179.7(5) 2_755 . ?
V1 O6 Cu1 122.8(3) . 3_765 ?
C5 N1 C9 118.5(6) . . ?
C5 N1 Cu1 129.3(5) . . ?
C9 N1 Cu1 112.2(5) . . ?
C16 N2 C13 117.7(6) . . ?
C16 N2 Cu1 129.6(5) . . ?
C13 N2 Cu1 112.6(5) . . ?
C2 C1 C2 120.7(10) . 2_755 ?
C2 C1 H1 119.7 . . ?
C2 C1 H1 119.7 2_755 . ?
C3 C2 C1 120.4(7) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 117.3(7) . . ?
C4 C3 P1 119.2(6) . . ?
C2 C3 P1 123.5(5) . . ?
C3 C4 C3 123.9(9) 2_755 . ?
C3 C4 H4 118.1 2_755 . ?
C3 C4 H4 118.1 . . ?
N2 C16 C15 123.9(6) . . ?
N2 C16 H16 118.0 . . ?
C15 C16 H16 118.0 . . ?
C14 C15 C16 117.6(6) . . ?
C14 C15 H15 121.2 . . ?
C16 C15 H15 121.2 . . ?
C15 C14 C12 121.3(7) . . ?
C15 C14 H14 119.4 . . ?
C12 C14 H14 119.4 . . ?
C14 C12 C13 116.9(7) . . ?
C14 C12 C11 125.2(7) . . ?
C13 C12 C11 117.9(7) . . ?
N2 C13 C12 122.6(7) . . ?
N2 C13 C9 116.4(6) . . ?
C12 C13 C9 121.0(7) . . ?
C10 C11 C12 121.8(7) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C10 C8 120.9(7) . . ?
C11 C10 H10 119.6 . . ?
C8 C10 H10 119.6 . . ?
C7 C8 C9 116.9(7) . . ?
C7 C8 C10 124.9(7) . . ?
C9 C8 C10 118.2(7) . . ?
N1 C9 C13 117.2(6) . . ?
N1 C9 C8 122.6(7) . . ?
C13 C9 C8 120.2(7) . . ?
C6 C7 C8 119.6(7) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C7 C6 C5 120.2(7) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
N1 C5 C6 122.3(7) . . ?
N1 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?

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
O2 P1 O1 Cu1 50.2(6) . . . . ?
O3 P1 O1 Cu1 -76.9(5) . . . . ?
C3 P1 O1 Cu1 170.5(5) . . . . ?
O2 Cu1 O1 P1 -2.8(5) 3_765 . . . ?
N2 Cu1 O1 P1 113.2(9) . . . . ?
N1 Cu1 O1 P1 168.6(5) . . . . ?
O6 Cu1 O1 P1 -100.4(5) 3_765 . . . ?
O1 P1 O2 Cu1 -117.9(5) . . . 3_765 ?
O3 P1 O2 Cu1 9.7(6) . . . 3_765 ?
C3 P1 O2 Cu1 122.5(5) . . . 3_765 ?
O1 P1 O3 V1 150.5(4) . . . . ?
O2 P1 O3 V1 20.3(5) . . . . ?
C3 P1 O3 V1 -95.2(5) . . . . ?
O5 V1 O3 P1 -155.2(4) . . . . ?
O6 V1 O3 P1 -38.0(5) . . . . ?
O4 V1 O3 P1 83.3(4) . . . . ?
O5 V1 O4 V1 46.2(8) . . . 2_755 ?
O6 V1 O4 V1 -75.2(9) . . . 2_755 ?
O3 V1 O4 V1 166.0(8) . . . 2_755 ?
O5 V1 O6 Cu1 143.5(3) . . . 3_765 ?
O4 V1 O6 Cu1 -93.9(4) . . . 3_765 ?
O3 V1 O6 Cu1 26.8(4) . . . 3_765 ?
O1 Cu1 N1 C5 11.5(7) . . . . ?
O2 Cu1 N1 C5 134.4(12) 3_765 . . . ?
N2 Cu1 N1 C5 178.7(7) . . . . ?
O6 Cu1 N1 C5 -90.3(7) 3_765 . . . ?
O1 Cu1 N1 C9 -171.1(5) . . . . ?
O2 Cu1 N1 C9 -48.2(15) 3_765 . . . ?
N2 Cu1 N1 C9 -3.9(5) . . . . ?
O6 Cu1 N1 C9 87.0(5) 3_765 . . . ?
O1 Cu1 N2 C16 -123.4(9) . . . . ?
O2 Cu1 N2 C16 -6.9(6) 3_765 . . . ?
N1 Cu1 N2 C16 -179.8(6) . . . . ?
O6 Cu1 N2 C16 89.4(6) 3_765 . . . ?
O1 Cu1 N2 C13 61.6(11) . . . . ?
O2 Cu1 N2 C13 178.2(5) 3_765 . . . ?
N1 Cu1 N2 C13 5.2(5) . . . . ?
O6 Cu1 N2 C13 -85.5(5) 3_765 . . . ?
C2 C1 C2 C3 -1.7(5) 2_755 . . . ?
C1 C2 C3 C4 3.3(10) . . . . ?
C1 C2 C3 P1 -173.7(4) . . . . ?
O1 P1 C3 C4 151.3(5) . . . . ?
O2 P1 C3 C4 -83.4(5) . . . . ?
O3 P1 C3 C4 33.7(5) . . . . ?
O1 P1 C3 C2 -31.8(7) . . . . ?
O2 P1 C3 C2 93.5(7) . . . . ?
O3 P1 C3 C2 -149.4(6) . . . . ?
C2 C3 C4 C3 -1.6(5) . . . 2_755 ?
P1 C3 C4 C3 175.4(6) . . . 2_755 ?
C13 N2 C16 C15 0.7(10) . . . . ?
Cu1 N2 C16 C15 -174.0(5) . . . . ?
N2 C16 C15 C14 -1.3(11) . . . . ?
C16 C15 C14 C12 0.1(11) . . . . ?
C15 C14 C12 C13 1.6(11) . . . . ?
C15 C14 C12 C11 -178.8(7) . . . . ?
C16 N2 C13 C12 1.1(10) . . . . ?
Cu1 N2 C13 C12 176.7(6) . . . . ?
C16 N2 C13 C9 178.6(6) . . . . ?
Cu1 N2 C13 C9 -5.8(8) . . . . ?
C14 C12 C13 N2 -2.3(11) . . . . ?
C11 C12 C13 N2 178.1(7) . . . . ?
C14 C12 C13 C9 -179.7(7) . . . . ?
C11 C12 C13 C9 0.7(11) . . . . ?
C14 C12 C11 C10 179.8(8) . . . . ?
C13 C12 C11 C10 -0.5(11) . . . . ?
C12 C11 C10 C8 0.0(12) . . . . ?
C11 C10 C8 C7 179.6(7) . . . . ?
C11 C10 C8 C9 0.4(11) . . . . ?
C5 N1 C9 C13 179.7(7) . . . . ?
Cu1 N1 C9 C13 2.0(8) . . . . ?
C5 N1 C9 C8 0.0(11) . . . . ?
Cu1 N1 C9 C8 -177.6(5) . . . . ?
N2 C13 C9 N1 2.5(9) . . . . ?
C12 C13 C9 N1 -179.9(7) . . . . ?
N2 C13 C9 C8 -177.8(6) . . . . ?
C12 C13 C9 C8 -0.3(10) . . . . ?
C7 C8 C9 N1 0.1(11) . . . . ?
C10 C8 C9 N1 179.4(6) . . . . ?
C7 C8 C9 C13 -179.5(7) . . . . ?
C10 C8 C9 C13 -0.2(10) . . . . ?
C9 C8 C7 C6 0.3(11) . . . . ?
C10 C8 C7 C6 -178.9(7) . . . . ?
C8 C7 C6 C5 -0.9(12) . . . . ?
C9 N1 C5 C6 -0.6(11) . . . . ?
Cu1 N1 C5 C6 176.6(6) . . . . ?
C7 C6 C5 N1 1.1(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.190

data_2
_database_code_depnum_ccdc_archive 'CCDC 734622'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_sum            'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_weight         561.72

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'
V V 0.3005 0.5294 '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
_symmetry_space_group_name_Hall  -P2ybc

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                   9.4396(8)
_cell_length_b                   15.8795(13)
_cell_length_c                   13.8189(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.147(2)
_cell_angle_gamma                90.00
_cell_volume                     2032.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5654
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      28.29

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7254
_exptl_absorpt_correction_T_max  0.8472
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            20876
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         28.29
_reflns_number_total             5047
_reflns_number_gt                4973
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0202P)²+5.5902P] where P=(Fo²+2Fc²)/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         5047
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_restrained_S_all      1.291
_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 0.79389(4) 0.29621(2) 0.35518(2) 0.01166(9) Uani 1 1 d . . .
V1 V 0.72613(5) 0.22085(3) 0.58973(3) 0.01187(11) Uani 1 1 d . . .
P2 P 0.68122(8) 0.11481(4) 0.40352(5) 0.01171(14) Uani 1 1 d . . .
P1 P 0.51628(8) -0.20918(4) 0.28014(5) 0.01186(14) Uani 1 1 d . . .
N1 N 1.0075(3) 0.27951(15) 0.39980(17) 0.0138(5) Uani 1 1 d . . .
N2 N 0.8555(3) 0.41828(15) 0.35781(18) 0.0143(5) Uani 1 1 d . . .
O1 O 0.4053(2) -0.17233(13) 0.19715(14) 0.0138(4) Uani 1 1 d . . .
O2 O 0.4505(2) -0.22462(14) 0.37369(15) 0.0170(4) Uani 1 1 d . . .
O3 O 0.5901(2) -0.28900(13) 0.25553(16) 0.0169(4) Uani 1 1 d . . .
O4 O 0.5172(2) 0.12369(13) 0.38330(16) 0.0154(4) Uani 1 1 d . . .
O5 O 0.7393(2) 0.12348(13) 0.51725(15) 0.0161(4) Uani 1 1 d . . .
O6 O 0.7585(2) 0.17454(12) 0.34664(15) 0.0147(4) Uani 1 1 d . . .
O7 O 0.8556(2) 0.22188(14) 0.68588(15) 0.0168(4) Uani 1 1 d . . .
O8 O 0.7449(2) 0.30080(13) 0.51974(15) 0.0168(4) Uani 1 1 d . . .
C1 C 0.6547(3) -0.13207(17) 0.3182(2) 0.0125(5) Uani 1 1 d . . .
C2 C 0.7994(3) -0.15229(18) 0.3217(2) 0.0153(5) Uani 1 1 d . . .
H2 H 0.8247 -0.2071 0.3034 0.018 Uiso 1 1 calc R . .
C3 C 0.9068(3) -0.09264(19) 0.3519(2) 0.0171(6) Uani 1 1 d . . .
H3 H 1.0052 -0.1067 0.3545 0.021 Uiso 1 1 calc R . .
C4 C 0.8694(3) -0.01254(19) 0.3780(2) 0.0172(6) Uani 1 1 d . . .
H4 H 0.9430 0.0279 0.3990 0.021 Uiso 1 1 calc R . .
C5 C 0.7251(3) 0.00948(17) 0.3740(2) 0.0129(5) Uani 1 1 d . . .
C6 C 0.6180(3) -0.05129(18) 0.3446(2) 0.0127(5) Uani 1 1 d . . .
H6 H 0.5196 -0.0374 0.3425 0.015 Uiso 1 1 calc R . .
C7 C 0.7752(3) 0.48709(19) 0.3371(2) 0.0181(6) Uani 1 1 d . . .
H7 H 0.6731 0.4814 0.3225 0.022 Uiso 1 1 calc R . .
C8 C 0.8354(4) 0.5676(2) 0.3360(3) 0.0234(7) Uani 1 1 d . . .
H8 H 0.7747 0.6155 0.3215 0.028 Uiso 1 1 calc R . .
C9 C 0.9832(4) 0.57693(19) 0.3561(3) 0.0236(7) Uani 1 1 d . . .
H9 H 1.0254 0.6311 0.3545 0.028 Uiso 1 1 calc R . .
C10 C 1.0713(3) 0.50532(19) 0.3791(2) 0.0190(6) Uani 1 1 d . . .
C11 C 1.0018(3) 0.42766(18) 0.3798(2) 0.0148(5) Uani 1 1 d . . .
C12 C 1.2271(3) 0.5070(2) 0.4001(3) 0.0238(7) Uani 1 1 d . . .
H12 H 1.2760 0.5593 0.3996 0.029 Uiso 1 1 calc R . .
C13 C 1.3047(3) 0.4354(2) 0.4206(2) 0.0220(6) Uani 1 1 d . . .
H13 H 1.4072 0.4382 0.4338 0.026 Uiso 1 1 calc R . .
C14 C 1.2351(3) 0.35518(19) 0.4228(2) 0.0164(6) Uani 1 1 d . . .
C15 C 1.0834(3) 0.35208(18) 0.4022(2) 0.0135(5) Uani 1 1 d . . .
C16 C 1.3090(3) 0.2783(2) 0.4422(2) 0.0189(6) Uani 1 1 d . . .
H16 H 1.4115 0.2771 0.4567 0.023 Uiso 1 1 calc R . .
C17 C 1.2315(3) 0.2051(2) 0.4401(2) 0.0211(6) Uani 1 1 d . . .
H17 H 1.2801 0.1528 0.4531 0.025 Uiso 1 1 calc R . .
C18 C 1.0803(3) 0.2078(2) 0.4187(2) 0.0196(6) Uani 1 1 d . . .
H18 H 1.0279 0.1566 0.4176 0.023 Uiso 1 1 calc R . .
H4' H 0.484(6) 0.154(4) 0.329(4) 0.072(18) Uiso 1 1 d . . .


_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 1.945(2) 2_655 ?
Cu1 O6 1.960(2) . ?
Cu1 N1 2.009(2) . ?
Cu1 N2 2.022(2) . ?
Cu1 O8 2.408(2) . ?
V1 O7 1.622(2) . ?
V1 O8 1.626(2) . ?
V1 O2 1.834(2) 3_656 ?
V1 O5 1.859(2) . ?
P2 O6 1.507(2) . ?
P2 O4 1.525(2) . ?
P2 O5 1.567(2) . ?
P2 C5 1.789(3) . ?
P1 O1 1.514(2) . ?
P1 O3 1.516(2) . ?
P1 O2 1.558(2) . ?
P1 C1 1.794(3) . ?
N1 C18 1.329(4) . ?
N1 C15 1.354(4) . ?
N2 C7 1.329(4) . ?
N2 C11 1.364(4) . ?
O1 Cu1 1.9445(19) 2_645 ?
O2 V1 1.834(2) 3_656 ?
O4 H4' 0.89(6) . ?
C1 C2 1.395(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.391(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.401(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.408(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(4) . ?
C10 C12 1.443(4) . ?
C11 C15 1.427(4) . ?
C12 C13 1.354(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.435(4) . ?
C13 H13 0.9500 . ?
C14 C16 1.406(4) . ?
C14 C15 1.406(4) . ?
C16 C17 1.370(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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 O6 95.14(8) 2_655 . ?
O1 Cu1 N1 171.47(9) 2_655 . ?
O6 Cu1 N1 92.16(9) . . ?
O1 Cu1 N2 90.82(9) 2_655 . ?
O6 Cu1 N2 172.28(9) . . ?
N1 Cu1 N2 81.55(10) . . ?
O1 Cu1 O8 89.71(8) 2_655 . ?
O6 Cu1 O8 91.44(8) . . ?
N1 Cu1 O8 94.52(9) . . ?
N2 Cu1 O8 93.50(8) . . ?
O7 V1 O8 109.14(11) . . ?
O7 V1 O2 110.78(10) . 3_656 ?
O8 V1 O2 110.34(10) . 3_656 ?
O7 V1 O5 109.35(10) . . ?
O8 V1 O5 107.61(10) . . ?
O2 V1 O5 109.55(10) 3_656 . ?
O6 P2 O4 115.00(12) . . ?
O6 P2 O5 110.91(12) . . ?
O4 P2 O5 108.75(12) . . ?
O6 P2 C5 108.22(12) . . ?
O4 P2 C5 108.42(13) . . ?
O5 P2 C5 105.02(12) . . ?
O1 P1 O3 115.72(12) . . ?
O1 P1 O2 111.15(12) . . ?
O3 P1 O2 109.19(12) . . ?
O1 P1 C1 108.45(12) . . ?
O3 P1 C1 107.23(12) . . ?
O2 P1 C1 104.43(12) . . ?
C18 N1 C15 118.3(2) . . ?
C18 N1 Cu1 128.6(2) . . ?
C15 N1 Cu1 112.96(19) . . ?
C7 N2 C11 118.0(3) . . ?
C7 N2 Cu1 129.4(2) . . ?
C11 N2 Cu1 112.58(19) . . ?
P1 O1 Cu1 131.33(13) . 2_645 ?
P1 O2 V1 138.84(13) . 3_656 ?
P2 O4 H4' 112(4) . . ?
P2 O5 V1 124.50(12) . . ?
P2 O6 Cu1 133.07(13) . . ?
V1 O8 Cu1 126.93(11) . . ?
C2 C1 C6 119.6(3) . . ?
C2 C1 P1 120.4(2) . . ?
C6 C1 P1 120.0(2) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 P2 119.5(2) . . ?
C6 C5 P2 121.7(2) . . ?
C1 C6 C5 120.5(2) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
N2 C7 C8 122.5(3) . . ?
N2 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C9 C8 C7 119.5(3) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 117.2(3) . . ?
C11 C10 C12 118.5(3) . . ?
C9 C10 C12 124.4(3) . . ?
N2 C11 C10 123.4(3) . . ?
N2 C11 C15 115.9(3) . . ?
C10 C11 C15 120.6(3) . . ?
C13 C12 C10 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
C10 C12 H12 119.5 . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C16 C14 C15 117.1(3) . . ?
C16 C14 C13 124.2(3) . . ?
C15 C14 C13 118.6(3) . . ?
N1 C15 C14 123.2(3) . . ?
N1 C15 C11 116.7(2) . . ?
C14 C15 C11 120.0(3) . . ?
C17 C16 C14 119.3(3) . . ?
C17 C16 H16 120.3 . . ?
C14 C16 H16 120.3 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
N1 C18 C17 122.3(3) . . ?
N1 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?

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
O1 Cu1 N1 C18 -152.1(5) 2_655 . . . ?
O6 Cu1 N1 C18 -3.2(3) . . . . ?
N2 Cu1 N1 C18 -178.8(3) . . . . ?
O8 Cu1 N1 C18 88.4(3) . . . . ?
O1 Cu1 N1 C15 22.2(7) 2_655 . . . ?
O6 Cu1 N1 C15 171.00(19) . . . . ?
N2 Cu1 N1 C15 -4.52(19) . . . . ?
O8 Cu1 N1 C15 -97.39(19) . . . . ?
O1 Cu1 N2 C7 4.6(3) 2_655 . . . ?
O6 Cu1 N2 C7 145.2(6) . . . . ?
N1 Cu1 N2 C7 -179.2(3) . . . . ?
O8 Cu1 N2 C7 -85.1(3) . . . . ?
O1 Cu1 N2 C11 -171.9(2) 2_655 . . . ?
O6 Cu1 N2 C11 -31.3(8) . . . . ?
N1 Cu1 N2 C11 4.31(19) . . . . ?
O8 Cu1 N2 C11 98.37(19) . . . . ?
O3 P1 O1 Cu1 78.76(19) . . . 2_645 ?
O2 P1 O1 Cu1 -46.5(2) . . . 2_645 ?
C1 P1 O1 Cu1 -160.76(15) . . . 2_645 ?
O1 P1 O2 V1 7.5(2) . . . 3_656 ?
O3 P1 O2 V1 -121.3(2) . . . 3_656 ?
C1 P1 O2 V1 124.3(2) . . . 3_656 ?
O6 P2 O5 V1 62.54(18) . . . . ?
O4 P2 O5 V1 -64.87(18) . . . . ?
C5 P2 O5 V1 179.23(15) . . . . ?
O7 V1 O5 P2 -153.63(15) . . . . ?
O8 V1 O5 P2 -35.20(18) . . . . ?
O2 V1 O5 P2 84.78(16) 3_656 . . . ?
O4 P2 O6 Cu1 71.2(2) . . . . ?
O5 P2 O6 Cu1 -52.7(2) . . . . ?
C5 P2 O6 Cu1 -167.44(16) . . . . ?
O1 Cu1 O6 P2 -71.06(18) 2_655 . . . ?
N1 Cu1 O6 P2 113.36(18) . . . . ?
N2 Cu1 O6 P2 148.5(6) . . . . ?
O8 Cu1 O6 P2 18.78(17) . . . . ?
O7 V1 O8 Cu1 115.49(14) . . . . ?
O2 V1 O8 Cu1 -122.55(13) 3_656 . . . ?
O5 V1 O8 Cu1 -3.07(17) . . . . ?
O1 Cu1 O8 V1 105.70(15) 2_655 . . . ?
O6 Cu1 O8 V1 10.56(15) . . . . ?
N1 Cu1 O8 V1 -81.72(15) . . . . ?
N2 Cu1 O8 V1 -163.50(15) . . . . ?
O1 P1 C1 C2 -126.4(2) . . . . ?
O3 P1 C1 C2 -0.8(3) . . . . ?
O2 P1 C1 C2 115.0(2) . . . . ?
O1 P1 C1 C6 53.7(2) . . . . ?
O3 P1 C1 C6 179.3(2) . . . . ?
O2 P1 C1 C6 -64.9(2) . . . . ?
C6 C1 C2 C3 0.4(4) . . . . ?
P1 C1 C2 C3 -179.5(2) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
C3 C4 C5 C6 1.1(4) . . . . ?
C3 C4 C5 P2 -177.4(2) . . . . ?
O6 P2 C5 C4 49.1(3) . . . . ?
O4 P2 C5 C4 174.4(2) . . . . ?
O5 P2 C5 C4 -69.5(3) . . . . ?
O6 P2 C5 C6 -129.4(2) . . . . ?
O4 P2 C5 C6 -4.0(3) . . . . ?
O5 P2 C5 C6 112.1(2) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
P1 C1 C6 C5 -179.8(2) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
P2 C5 C6 C1 177.4(2) . . . . ?
C11 N2 C7 C8 0.8(4) . . . . ?
Cu1 N2 C7 C8 -175.6(2) . . . . ?
N2 C7 C8 C9 0.6(5) . . . . ?
C7 C8 C9 C10 -1.1(5) . . . . ?
C8 C9 C10 C11 0.2(5) . . . . ?
C8 C9 C10 C12 179.1(3) . . . . ?
C7 N2 C11 C10 -1.7(4) . . . . ?
Cu1 N2 C11 C10 175.2(2) . . . . ?
C7 N2 C11 C15 179.6(3) . . . . ?
Cu1 N2 C11 C15 -3.4(3) . . . . ?
C9 C10 C11 N2 1.2(5) . . . . ?
C12 C10 C11 N2 -177.7(3) . . . . ?
C9 C10 C11 C15 179.8(3) . . . . ?
C12 C10 C11 C15 0.9(4) . . . . ?
C11 C10 C12 C13 -0.4(5) . . . . ?
C9 C10 C12 C13 -179.3(3) . . . . ?
C10 C12 C13 C14 -0.4(5) . . . . ?
C12 C13 C14 C16 179.1(3) . . . . ?
C12 C13 C14 C15 0.6(5) . . . . ?
C18 N1 C15 C14 0.6(4) . . . . ?
Cu1 N1 C15 C14 -174.3(2) . . . . ?
C18 N1 C15 C11 178.9(3) . . . . ?
Cu1 N1 C15 C11 4.0(3) . . . . ?
C16 C14 C15 N1 -0.4(4) . . . . ?
C13 C14 C15 N1 178.3(3) . . . . ?
C16 C14 C15 C11 -178.7(3) . . . . ?
C13 C14 C15 C11 0.0(4) . . . . ?
N2 C11 C15 N1 -0.4(4) . . . . ?
C10 C11 C15 N1 -179.1(3) . . . . ?
N2 C11 C15 C14 178.0(2) . . . . ?
C10 C11 C15 C14 -0.7(4) . . . . ?
C15 C14 C16 C17 0.1(4) . . . . ?
C13 C14 C16 C17 -178.5(3) . . . . ?
C14 C16 C17 C18 0.0(5) . . . . ?
C15 N1 C18 C17 -0.4(4) . . . . ?
Cu1 N1 C18 C17 173.6(2) . . . . ?
C16 C17 C18 N1 0.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.098

data_3
_database_code_depnum_ccdc_archive 'CCDC 734623'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 Cu2 N6 O11 P2 V2'
_chemical_formula_sum            'C36 H26 Cu2 N6 O11 P2 V2'
_chemical_formula_weight         1009.53

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'
V V 0.3005 0.5294 '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   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   18.0260(15)
_cell_length_b                   17.9783(15)
_cell_length_c                   11.9993(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.1390(10)
_cell_angle_gamma                90.00
_cell_volume                     3548.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5425
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      28.18

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_T_max  0.8506
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            17437
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         28.08
_reflns_number_total             4308
_reflns_number_gt                4161
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0284P)²+50.3458P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         4308
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1428
_refine_ls_goodness_of_fit_ref   1.358
_refine_ls_restrained_S_all      1.358
_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 0.70135(3) 0.86164(3) 0.51805(5) 0.00812(15) Uani 1 1 d . . .
V1 V 0.56003(5) 0.75593(4) 0.68413(7) 0.00847(18) Uani 1 1 d . . .
P1 P 0.62515(7) 0.69451(7) 0.48957(10) 0.0079(2) Uani 1 1 d . . .
O1 O 0.6355(2) 0.77396(19) 0.4559(3) 0.0127(7) Uani 1 1 d . . .
O2 O 0.7022(2) 0.64955(19) 0.5428(3) 0.0124(7) Uani 1 1 d . . .
O3 O 0.5823(2) 0.69175(19) 0.5791(3) 0.0119(7) Uani 1 1 d . . .
O4 O 0.5110(2) 0.8282(2) 0.6079(3) 0.0172(7) Uani 1 1 d . . .
O5 O 0.5000 0.7067(3) 0.7500 0.0128(9) Uani 1 2 d S . .
O6 O 0.6451(2) 0.7839(2) 0.7928(3) 0.0152(7) Uani 1 1 d . . .
N1 N 0.7721(2) 0.8447(2) 0.6997(4) 0.0110(8) Uani 1 1 d . . .
N2 N 0.7266(2) 0.9644(2) 0.5736(4) 0.0107(8) Uani 1 1 d . . .
N3 N 0.6368(2) 0.9167(2) 0.3618(4) 0.0109(8) Uani 1 1 d . . .
C1 C 0.5000 0.6866(4) 0.2500 0.0093(12) Uani 1 2 d S . .
H1 H 0.5000 0.7395 0.2500 0.011 Uiso 1 2 calc SR . .
C2 C 0.5543(3) 0.6485(3) 0.3523(4) 0.0094(8) Uani 1 1 d . . .
C3 C 0.5545(3) 0.5711(3) 0.3513(4) 0.0122(9) Uani 1 1 d . . .
H3 H 0.5919 0.5447 0.4199 0.015 Uiso 1 1 calc R . .
C4 C 0.5000 0.5317(4) 0.2500 0.0160(14) Uani 1 2 d S . .
H4 H 0.5000 0.4789 0.2500 0.019 Uiso 1 2 calc SR . .
C5 C 0.7955(3) 0.7799(3) 0.7583(4) 0.0138(9) Uani 1 1 d . . .
H5 H 0.7754 0.7351 0.7143 0.017 Uiso 1 1 calc R . .
C6 C 0.8481(3) 0.7756(3) 0.8811(4) 0.0151(10) Uani 1 1 d . . .
H6 H 0.8639 0.7286 0.9199 0.018 Uiso 1 1 calc R . .
C7 C 0.8768(3) 0.8403(3) 0.9457(5) 0.0186(10) Uani 1 1 d . . .
H7 H 0.9118 0.8388 1.0301 0.022 Uiso 1 1 calc R . .
C8 C 0.8541(3) 0.9075(3) 0.8855(4) 0.0178(10) Uani 1 1 d . . .
H8 H 0.8743 0.9528 0.9280 0.021 Uiso 1 1 calc R . .
C9 C 0.8017(3) 0.9087(3) 0.7632(4) 0.0134(9) Uani 1 1 d . . .
C10 C 0.7756(3) 0.9773(3) 0.6900(4) 0.0131(9) Uani 1 1 d . . .
C11 C 0.7982(3) 1.0501(3) 0.7308(5) 0.0189(11) Uani 1 1 d . . .
H11 H 0.8321 1.0600 0.8140 0.023 Uiso 1 1 calc R . .
C12 C 0.7699(3) 1.1078(3) 0.6461(5) 0.0168(10) Uani 1 1 d . . .
H12 H 0.7860 1.1576 0.6711 0.020 Uiso 1 1 calc R . .
C13 C 0.7177(3) 1.0930(3) 0.5245(4) 0.0128(9) Uani 1 1 d . . .
H13 H 0.6968 1.1320 0.4666 0.015 Uiso 1 1 calc R . .
C14 C 0.6976(3) 1.0193(3) 0.4915(4) 0.0112(9) Uani 1 1 d . . .
C15 C 0.6462(3) 0.9918(3) 0.3682(4) 0.0104(9) Uani 1 1 d . . .
C16 C 0.6115(3) 1.0366(3) 0.2656(5) 0.0185(11) Uani 1 1 d . . .
H16 H 0.6174 1.0891 0.2719 0.022 Uiso 1 1 calc R . .
C17 C 0.5680(4) 1.0027(3) 0.1534(5) 0.0256(13) Uani 1 1 d . . .
H17 H 0.5433 1.0320 0.0817 0.031 Uiso 1 1 calc R . .
C18 C 0.5610(4) 0.9256(3) 0.1469(5) 0.0239(12) Uani 1 1 d . . .
H18 H 0.5333 0.9013 0.0708 0.029 Uiso 1 1 calc R . .
C19 C 0.5954(3) 0.8852(3) 0.2540(4) 0.0139(9) Uani 1 1 d . . .
H19 H 0.5891 0.8327 0.2503 0.017 Uiso 1 1 calc R . .


_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 1.931(3) . ?
Cu1 N2 1.954(4) . ?
Cu1 N3 2.016(4) . ?
Cu1 N1 2.049(4) . ?
Cu1 O2 2.153(3) 7_666 ?
V1 O4 1.626(4) . ?
V1 O6 1.634(3) . ?
V1 O5 1.811(2) . ?
V1 O3 1.870(3) . ?
P1 O2 1.504(3) . ?
P1 O1 1.516(3) . ?
P1 O3 1.559(3) . ?
P1 C2 1.819(5) . ?
O2 Cu1 2.153(3) 7_666 ?
O5 V1 1.811(2) 2_656 ?
N1 C5 1.336(6) . ?
N1 C9 1.363(6) . ?
N2 C10 1.332(6) . ?
N2 C14 1.339(6) . ?
N3 C19 1.327(6) . ?
N3 C15 1.358(6) . ?
C1 C2 1.396(5) . ?
C1 C2 1.396(5) 2_655 ?
C1 H1 0.9500 . ?
C2 C3 1.391(7) . ?
C3 C4 1.403(6) . ?
C3 H3 0.9500 . ?
C4 C3 1.403(6) 2_655 ?
C4 H4 0.9500 . ?
C5 C6 1.390(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.476(7) . ?
C10 C11 1.398(7) . ?
C11 C12 1.395(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.474(6) . ?
C15 C16 1.387(7) . ?
C16 C17 1.391(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(7) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?

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 N2 157.60(16) . . ?
O1 Cu1 N3 90.69(15) . . ?
N2 Cu1 N3 79.54(16) . . ?
O1 Cu1 N1 107.83(15) . . ?
N2 Cu1 N1 79.68(16) . . ?
N3 Cu1 N1 159.06(17) . . ?
O1 Cu1 O2 104.33(14) . 7_666 ?
N2 Cu1 O2 95.54(15) . 7_666 ?
N3 Cu1 O2 88.26(14) . 7_666 ?
N1 Cu1 O2 96.26(14) . 7_666 ?
O4 V1 O6 108.68(19) . . ?
O4 V1 O5 110.57(17) . . ?
O6 V1 O5 109.58(14) . . ?
O4 V1 O3 109.33(17) . . ?
O6 V1 O3 109.75(17) . . ?
O5 V1 O3 108.91(17) . . ?
O2 P1 O1 115.3(2) . . ?
O2 P1 O3 108.76(19) . . ?
O1 P1 O3 111.27(19) . . ?
O2 P1 C2 108.9(2) . . ?
O1 P1 C2 107.7(2) . . ?
O3 P1 C2 104.30(19) . . ?
P1 O1 Cu1 142.1(2) . . ?
P1 O2 Cu1 129.8(2) . 7_666 ?
P1 O3 V1 138.4(2) . . ?
V1 O5 V1 121.5(3) 2_656 . ?
C5 N1 C9 118.4(4) . . ?
C5 N1 Cu1 127.9(3) . . ?
C9 N1 Cu1 113.6(3) . . ?
C10 N2 C14 122.3(4) . . ?
C10 N2 Cu1 119.0(3) . . ?
C14 N2 Cu1 118.6(3) . . ?
C19 N3 C15 119.1(4) . . ?
C19 N3 Cu1 125.3(3) . . ?
C15 N3 Cu1 115.1(3) . . ?
C2 C1 C2 121.2(6) . 2_655 ?
C2 C1 H1 119.4 . . ?
C2 C1 H1 119.4 2_655 . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 P1 117.3(3) . . ?
C1 C2 P1 123.6(4) . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C3 119.4(6) 2_655 . ?
C3 C4 H4 120.3 2_655 . ?
C3 C4 H4 120.3 . . ?
N1 C5 C6 122.5(5) . . ?
N1 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C7 C6 C5 119.1(5) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 118.8(5) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C9 119.7(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
N1 C9 C8 121.5(5) . . ?
N1 C9 C10 114.6(4) . . ?
C8 C9 C10 123.9(5) . . ?
N2 C10 C11 120.2(5) . . ?
N2 C10 C9 113.1(4) . . ?
C11 C10 C9 126.7(4) . . ?
C12 C11 C10 118.3(5) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
C11 C12 C13 120.4(5) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 117.7(4) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
N2 C14 C13 121.0(4) . . ?
N2 C14 C15 112.8(4) . . ?
C13 C14 C15 126.2(4) . . ?
N3 C15 C16 121.7(4) . . ?
N3 C15 C14 113.7(4) . . ?
C16 C15 C14 124.5(4) . . ?
C15 C16 C17 118.4(5) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C16 C17 C18 119.4(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 118.4(5) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
N3 C19 C18 122.8(5) . . ?
N3 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?

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
O2 P1 O1 Cu1 -47.2(4) . . . . ?
O3 P1 O1 Cu1 77.2(4) . . . . ?
C2 P1 O1 Cu1 -169.0(3) . . . . ?
N2 Cu1 O1 P1 -117.1(4) . . . . ?
N3 Cu1 O1 P1 179.4(4) . . . . ?
N1 Cu1 O1 P1 -10.5(4) . . . . ?
O2 Cu1 O1 P1 91.1(4) 7_666 . . . ?
O1 P1 O2 Cu1 -46.4(3) . . . 7_666 ?
O3 P1 O2 Cu1 -172.2(2) . . . 7_666 ?
C2 P1 O2 Cu1 74.7(3) . . . 7_666 ?
O2 P1 O3 V1 110.5(3) . . . . ?
O1 P1 O3 V1 -17.5(4) . . . . ?
C2 P1 O3 V1 -133.4(3) . . . . ?
O4 V1 O3 P1 55.8(4) . . . . ?
O6 V1 O3 P1 -63.3(4) . . . . ?
O5 V1 O3 P1 176.7(3) . . . . ?
O4 V1 O5 V1 -39.85(15) . . . 2_656 ?
O6 V1 O5 V1 79.92(15) . . . 2_656 ?
O3 V1 O5 V1 -160.01(12) . . . 2_656 ?
O1 Cu1 N1 C5 24.2(4) . . . . ?
N2 Cu1 N1 C5 -177.6(4) . . . . ?
N3 Cu1 N1 C5 175.4(4) . . . . ?
O2 Cu1 N1 C5 -83.1(4) 7_666 . . . ?
O1 Cu1 N1 C9 -160.3(3) . . . . ?
N2 Cu1 N1 C9 -2.1(3) . . . . ?
N3 Cu1 N1 C9 -9.1(6) . . . . ?
O2 Cu1 N1 C9 92.5(3) 7_666 . . . ?
O1 Cu1 N2 C10 114.5(5) . . . . ?
N3 Cu1 N2 C10 180.0(4) . . . . ?
N1 Cu1 N2 C10 2.5(4) . . . . ?
O2 Cu1 N2 C10 -92.8(4) 7_666 . . . ?
O1 Cu1 N2 C14 -69.2(6) . . . . ?
N3 Cu1 N2 C14 -3.8(3) . . . . ?
N1 Cu1 N2 C14 178.8(4) . . . . ?
O2 Cu1 N2 C14 83.4(4) 7_666 . . . ?
O1 Cu1 N3 C19 -24.3(4) . . . . ?
N2 Cu1 N3 C19 175.9(4) . . . . ?
N1 Cu1 N3 C19 -177.0(4) . . . . ?
O2 Cu1 N3 C19 80.0(4) 7_666 . . . ?
O1 Cu1 N3 C15 164.1(3) . . . . ?
N2 Cu1 N3 C15 4.4(3) . . . . ?
N1 Cu1 N3 C15 11.4(7) . . . . ?
O2 Cu1 N3 C15 -91.6(3) 7_666 . . . ?
C2 C1 C2 C3 0.6(3) 2_655 . . . ?
C2 C1 C2 P1 -178.8(4) 2_655 . . . ?
O2 P1 C2 C3 35.1(4) . . . . ?
O1 P1 C2 C3 160.7(4) . . . . ?
O3 P1 C2 C3 -80.9(4) . . . . ?
O2 P1 C2 C1 -145.6(3) . . . . ?
O1 P1 C2 C1 -19.9(4) . . . . ?
O3 P1 C2 C1 98.4(3) . . . . ?
C1 C2 C3 C4 -1.1(6) . . . . ?
P1 C2 C3 C4 178.2(3) . . . . ?
C2 C3 C4 C3 0.6(3) . . . 2_655 ?
C9 N1 C5 C6 0.5(7) . . . . ?
Cu1 N1 C5 C6 175.8(4) . . . . ?
N1 C5 C6 C7 0.6(8) . . . . ?
C5 C6 C7 C8 -1.6(8) . . . . ?
C6 C7 C8 C9 1.5(8) . . . . ?
C5 N1 C9 C8 -0.5(7) . . . . ?
Cu1 N1 C9 C8 -176.5(4) . . . . ?
C5 N1 C9 C10 177.4(4) . . . . ?
Cu1 N1 C9 C10 1.4(5) . . . . ?
C7 C8 C9 N1 -0.5(8) . . . . ?
C7 C8 C9 C10 -178.2(5) . . . . ?
C14 N2 C10 C11 0.4(7) . . . . ?
Cu1 N2 C10 C11 176.5(4) . . . . ?
C14 N2 C10 C9 -178.5(4) . . . . ?
Cu1 N2 C10 C9 -2.5(5) . . . . ?
N1 C9 C10 N2 0.6(6) . . . . ?
C8 C9 C10 N2 178.4(5) . . . . ?
N1 C9 C10 C11 -178.3(5) . . . . ?
C8 C9 C10 C11 -0.5(8) . . . . ?
N2 C10 C11 C12 -1.6(8) . . . . ?
C9 C10 C11 C12 177.3(5) . . . . ?
C10 C11 C12 C13 2.2(8) . . . . ?
C11 C12 C13 C14 -1.7(8) . . . . ?
C10 N2 C14 C13 0.0(7) . . . . ?
Cu1 N2 C14 C13 -176.1(4) . . . . ?
C10 N2 C14 C15 178.7(4) . . . . ?
Cu1 N2 C14 C15 2.6(5) . . . . ?
C12 C13 C14 N2 0.6(7) . . . . ?
C12 C13 C14 C15 -177.8(5) . . . . ?
C19 N3 C15 C16 2.1(7) . . . . ?
Cu1 N3 C15 C16 174.2(4) . . . . ?
C19 N3 C15 C14 -176.4(4) . . . . ?
Cu1 N3 C15 C14 -4.3(5) . . . . ?
N2 C14 C15 N3 1.2(6) . . . . ?
C13 C14 C15 N3 179.8(5) . . . . ?
N2 C14 C15 C16 -177.2(5) . . . . ?
C13 C14 C15 C16 1.3(8) . . . . ?
N3 C15 C16 C17 -1.8(8) . . . . ?
C14 C15 C16 C17 176.5(5) . . . . ?
C15 C16 C17 C18 -0.5(9) . . . . ?
C16 C17 C18 C19 2.3(10) . . . . ?
C15 N3 C19 C18 -0.1(8) . . . . ?
Cu1 N3 C19 C18 -171.3(4) . . . . ?
C17 C18 C19 N3 -2.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.152

data_4
_database_code_depnum_ccdc_archive 'CCDC 734624'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H24 Cu2 F N6 O9 P2 V, H2 O'
_chemical_formula_sum            'C26 H26 Cu2 F N6 O10 P2 V'
_chemical_formula_weight         841.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   10.6351(8)
_cell_length_b                   14.8733(11)
_cell_length_c                   18.7757(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8310(10)
_cell_angle_gamma                90.00
_cell_volume                     2963.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    8118
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5973
_exptl_absorpt_correction_T_max  0.8170
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            29065
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         28.08
_reflns_number_total             7202
_reflns_number_gt                7010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0198P)²+21.9708P] where P=(Fo²+2Fc²)/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         7202
_refine_ls_number_parameters     457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1335
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_restrained_S_all      1.336
_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
O90 O 0.8692(4) 0.9579(2) 0.0346(2) 0.0159(7) Uani 1 1 d . . .
Cu1 Cu 0.48143(5) 0.93869(4) 0.10911(3) 0.00683(13) Uani 1 1 d . . .
Cu2 Cu 1.06051(5) 0.60705(4) 0.10256(3) 0.00684(13) Uani 1 1 d . . .
V1 V 1.06843(8) 0.74724(5) -0.05200(4) 0.01034(17) Uani 1 1 d . . .
P1 P 0.53016(11) 0.87317(7) -0.01426(6) 0.0062(2) Uani 1 1 d . . .
P2 P 0.86191(11) 0.58625(8) -0.03549(6) 0.0073(2) Uani 1 1 d . . .
F1 F 0.9388(3) 0.8316(2) -0.05966(17) 0.0191(6) Uani 1 1 d . . .
O1 O 0.4006(3) 0.8850(2) 0.01810(17) 0.0105(6) Uani 1 1 d . . .
O2 O 0.6227(3) 0.9078(2) 0.04666(17) 0.0093(6) Uani 1 1 d . . .
O3 O 0.5431(3) 0.9173(2) -0.08576(17) 0.0099(6) Uani 1 1 d . . .
O4 O 0.9100(3) 0.5790(2) 0.04207(16) 0.0086(6) Uani 1 1 d . . .
O5 O 0.9388(3) 0.6552(2) -0.07670(17) 0.0105(6) Uani 1 1 d . . .
O6 O 0.8491(3) 0.4985(2) -0.07589(19) 0.0144(7) Uani 1 1 d . . .
O7 O 1.1248(4) 0.7038(3) 0.0226(2) 0.0241(9) Uani 1 1 d . . .
O8 O 1.1565(4) 0.7191(3) -0.1161(2) 0.0239(9) Uani 1 1 d . . .
O40 O 1.1695(4) 0.8652(3) -0.0387(3) 0.0266(10) Uani 1 1 d . . .
N1 N 0.5937(3) 0.9622(3) 0.1948(2) 0.0078(7) Uani 1 1 d . . .
N2 N 0.4538(4) 0.9038(3) 0.2755(2) 0.0115(8) Uani 1 1 d . . .
N3 N 0.3345(4) 0.9289(3) 0.1667(2) 0.0090(7) Uani 1 1 d . . .
N4 N 0.9593(4) 0.6848(3) 0.1636(2) 0.0099(8) Uani 1 1 d . . .
N5 N 1.0764(4) 0.6369(3) 0.2677(2) 0.0111(8) Uani 1 1 d . . .
N6 N 1.2058(4) 0.6382(3) 0.1711(2) 0.0089(7) Uani 1 1 d . . .
C1 C 0.5566(4) 0.7544(3) -0.0264(2) 0.0083(8) Uani 1 1 d . . .
C2 C 0.4551(4) 0.6953(3) -0.0367(3) 0.0121(9) Uani 1 1 d . . .
H2 H 0.3712 0.7167 -0.0349 0.014 Uiso 1 1 calc R . .
C3 C 0.4776(5) 0.6053(3) -0.0496(3) 0.0156(10) Uani 1 1 d . . .
H3 H 0.4087 0.5652 -0.0581 0.019 Uiso 1 1 calc R . .
C4 C 0.6000(5) 0.5731(3) -0.0503(3) 0.0128(9) Uani 1 1 d . . .
H4 H 0.6136 0.5111 -0.0592 0.015 Uiso 1 1 calc R . .
C5 C 0.7031(4) 0.6298(3) -0.0383(2) 0.0097(9) Uani 1 1 d . . .
C6 C 0.6788(4) 0.7218(3) -0.0283(2) 0.0079(8) Uani 1 1 d . . .
H6 H 0.7476 0.7625 -0.0226 0.009 Uiso 1 1 calc R . .
C7 C 0.7051(5) 1.0025(3) 0.1834(3) 0.0123(9) Uani 1 1 d . . .
H7 H 0.7238 1.0161 0.1358 0.015 Uiso 1 1 calc R . .
C8 C 0.7921(5) 1.0245(4) 0.2382(3) 0.0178(10) Uani 1 1 d . . .
H8 H 0.8703 1.0514 0.2287 0.021 Uiso 1 1 calc R . .
C9 C 0.7631(5) 1.0065(4) 0.3077(3) 0.0191(11) Uani 1 1 d . . .
H9 H 0.8213 1.0214 0.3465 0.023 Uiso 1 1 calc R . .
C10 C 0.6499(5) 0.9670(3) 0.3203(3) 0.0142(10) Uani 1 1 d . . .
H10 H 0.6286 0.9548 0.3677 0.017 Uiso 1 1 calc R . .
C11 C 0.5666(5) 0.9449(3) 0.2620(2) 0.0103(9) Uani 1 1 d . . .
C12 C 0.3390(4) 0.9067(3) 0.2363(2) 0.0099(9) Uani 1 1 d . . .
C13 C 0.2306(5) 0.8866(4) 0.2709(3) 0.0169(10) Uani 1 1 d . . .
H13 H 0.2366 0.8678 0.3194 0.020 Uiso 1 1 calc R . .
C14 C 0.1148(5) 0.8941(4) 0.2344(3) 0.0166(10) Uani 1 1 d . . .
H14 H 0.0401 0.8808 0.2573 0.020 Uiso 1 1 calc R . .
C15 C 0.1082(5) 0.9214(4) 0.1627(3) 0.0166(10) Uani 1 1 d . . .
H15 H 0.0293 0.9285 0.1365 0.020 Uiso 1 1 calc R . .
C16 C 0.2188(5) 0.9375(3) 0.1321(3) 0.0146(10) Uani 1 1 d . . .
H16 H 0.2146 0.9560 0.0835 0.018 Uiso 1 1 calc R . .
C17 C 0.8631(5) 0.7331(3) 0.1329(3) 0.0145(10) Uani 1 1 d . . .
H17 H 0.8577 0.7397 0.0825 0.017 Uiso 1 1 calc R . .
C18 C 0.7725(5) 0.7732(3) 0.1709(3) 0.0165(10) Uani 1 1 d . . .
H18 H 0.7063 0.8071 0.1474 0.020 Uiso 1 1 calc R . .
C19 C 0.7802(5) 0.7629(3) 0.2443(3) 0.0172(10) Uani 1 1 d . . .
H19 H 0.7170 0.7878 0.2717 0.021 Uiso 1 1 calc R . .
C20 C 0.8797(5) 0.7165(3) 0.2776(3) 0.0136(9) Uani 1 1 d . . .
H20 H 0.8867 0.7095 0.3280 0.016 Uiso 1 1 calc R . .
C21 C 0.9705(4) 0.6796(3) 0.2350(2) 0.0089(8) Uani 1 1 d . . .
C22 C 1.1956(5) 0.6424(3) 0.2421(2) 0.0099(9) Uani 1 1 d . . .
C23 C 1.3012(5) 0.6533(3) 0.2899(3) 0.0149(10) Uani 1 1 d . . .
H23 H 1.2930 0.6522 0.3400 0.018 Uiso 1 1 calc R . .
C24 C 1.4166(5) 0.6657(4) 0.2630(3) 0.0194(11) Uani 1 1 d . . .
H24 H 1.4893 0.6747 0.2944 0.023 Uiso 1 1 calc R . .
C25 C 1.4270(5) 0.6649(4) 0.1894(3) 0.0187(11) Uani 1 1 d . . .
H25 H 1.5062 0.6741 0.1699 0.022 Uiso 1 1 calc R . .
C26 C 1.3199(5) 0.6507(3) 0.1458(3) 0.0135(9) Uani 1 1 d . . .
H26 H 1.3268 0.6496 0.0957 0.016 Uiso 1 1 calc R . .
H40A H 1.134(8) 0.915(6) -0.040(4) 0.05(2) Uiso 1 1 d . . .
H40B H 1.235(7) 0.870(5) -0.021(4) 0.025(18) Uiso 1 1 d . . .
H90A H 0.802(7) 0.943(5) 0.037(3) 0.021(18) Uiso 1 1 d . . .
H90B H 0.899(5) 0.924(4) 0.006(3) 0.000(12) Uiso 1 1 d . . .
H2' H 0.452(6) 0.888(4) 0.313(3) 0.012(15) Uiso 1 1 d . . .
H5' H 1.077(6) 0.631(4) 0.307(3) 0.014(16) Uiso 1 1 d . . .


_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
O90 H90A 0.75(7) . ?
O90 H90B 0.82(6) . ?
Cu1 N3 1.964(4) . ?
Cu1 N1 1.969(4) . ?
Cu1 O2 2.020(3) . ?
Cu1 O1 2.025(3) . ?
Cu1 O3 2.199(3) 3_675 ?
Cu2 O6 1.925(3) 3_765 ?
Cu2 O4 1.945(3) . ?
Cu2 N4 1.994(4) . ?
Cu2 N6 1.998(4) . ?
Cu2 O7 2.220(4) . ?
V1 O7 1.621(4) . ?
V1 O8 1.627(4) . ?
V1 F1 1.863(3) . ?
V1 O5 1.975(3) . ?
V1 O40 2.064(4) . ?
P1 O3 1.509(3) . ?
P1 O2 1.546(3) . ?
P1 O1 1.553(3) . ?
P1 C1 1.806(5) . ?
P2 O6 1.511(3) . ?
P2 O4 1.515(3) . ?
P2 O5 1.551(3) . ?
P2 C5 1.806(5) . ?
O3 Cu1 2.198(3) 3_675 ?
O6 Cu2 1.925(3) 3_765 ?
O40 H40A 0.83(9) . ?
O40 H40B 0.76(7) . ?
N1 C11 1.338(6) . ?
N1 C7 1.358(6) . ?
N2 C12 1.382(6) . ?
N2 C11 1.386(6) . ?
N2 H2' 0.74(6) . ?
N3 C12 1.347(6) . ?
N3 C16 1.358(6) . ?
N4 C21 1.340(6) . ?
N4 C17 1.348(6) . ?
N5 C22 1.388(6) . ?
N5 C21 1.399(6) . ?
N5 H5' 0.75(6) . ?
N6 C26 1.345(6) . ?
N6 C22 1.346(6) . ?
C1 C6 1.390(6) . ?
C1 C2 1.395(6) . ?
C2 C3 1.384(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.376(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.401(7) . ?
C10 H10 0.9500 . ?
C12 C13 1.394(7) . ?
C13 C14 1.373(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.402(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.372(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.377(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.405(7) . ?
C20 H20 0.9500 . ?
C22 C23 1.400(6) . ?
C23 C24 1.371(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.374(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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
H90A O90 H90B 106(6) . . ?
N3 Cu1 N1 91.43(16) . . ?
N3 Cu1 O2 162.30(15) . . ?
N1 Cu1 O2 94.63(14) . . ?
N3 Cu1 O1 97.26(14) . . ?
N1 Cu1 O1 163.59(15) . . ?
O2 Cu1 O1 73.19(13) . . ?
N3 Cu1 O3 95.40(14) . 3_675 ?
N1 Cu1 O3 92.71(14) . 3_675 ?
O2 Cu1 O3 100.89(13) . 3_675 ?
O1 Cu1 O3 100.26(13) . 3_675 ?
O6 Cu2 O4 94.53(14) 3_765 . ?
O6 Cu2 N4 157.08(16) 3_765 . ?
O4 Cu2 N4 90.31(15) . . ?
O6 Cu2 N6 88.76(15) 3_765 . ?
O4 Cu2 N6 175.28(15) . . ?
N4 Cu2 N6 85.36(16) . . ?
O6 Cu2 O7 99.85(16) 3_765 . ?
O4 Cu2 O7 91.32(13) . . ?
N4 Cu2 O7 102.42(17) . . ?
N6 Cu2 O7 91.45(15) . . ?
O7 V1 O8 109.8(2) . . ?
O7 V1 F1 124.35(19) . . ?
O8 V1 F1 125.13(19) . . ?
O7 V1 O5 97.97(17) . . ?
O8 V1 O5 94.33(17) . . ?
F1 V1 O5 86.98(14) . . ?
O7 V1 O40 94.28(19) . . ?
O8 V1 O40 89.3(2) . . ?
F1 V1 O40 79.24(16) . . ?
O5 V1 O40 165.20(16) . . ?
O3 P1 O2 114.97(19) . . ?
O3 P1 O1 115.78(19) . . ?
O2 P1 O1 102.15(18) . . ?
O3 P1 C1 106.81(19) . . ?
O2 P1 C1 108.8(2) . . ?
O1 P1 C1 108.0(2) . . ?
O6 P2 O4 115.72(19) . . ?
O6 P2 O5 110.7(2) . . ?
O4 P2 O5 111.82(19) . . ?
O6 P2 C5 104.0(2) . . ?
O4 P2 C5 107.96(19) . . ?
O5 P2 C5 105.7(2) . . ?
P1 O1 Cu1 92.11(16) . . ?
P1 O2 Cu1 92.52(16) . . ?
P1 O3 Cu1 125.77(19) . 3_675 ?
P2 O4 Cu2 139.2(2) . . ?
P2 O5 V1 136.4(2) . . ?
P2 O6 Cu2 143.6(2) . 3_765 ?
V1 O7 Cu2 136.9(2) . . ?
V1 O40 H40A 122(6) . . ?
V1 O40 H40B 126(5) . . ?
H40A O40 H40B 109(8) . . ?
C11 N1 C7 118.5(4) . . ?
C11 N1 Cu1 125.4(3) . . ?
C7 N1 Cu1 116.0(3) . . ?
C12 N2 C11 129.3(4) . . ?
C12 N2 H2' 115(5) . . ?
C11 N2 H2' 113(5) . . ?
C12 N3 C16 117.4(4) . . ?
C12 N3 Cu1 125.1(3) . . ?
C16 N3 Cu1 117.3(3) . . ?
C21 N4 C17 118.2(4) . . ?
C21 N4 Cu2 121.8(3) . . ?
C17 N4 Cu2 119.1(3) . . ?
C22 N5 C21 123.3(4) . . ?
C22 N5 H5' 114(5) . . ?
C21 N5 H5' 117(5) . . ?
C26 N6 C22 118.5(4) . . ?
C26 N6 Cu2 118.8(3) . . ?
C22 N6 Cu2 122.6(3) . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 P1 119.9(3) . . ?
C2 C1 P1 120.5(4) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 121.3(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 117.5(4) . . ?
C4 C5 P2 120.9(4) . . ?
C6 C5 P2 121.6(4) . . ?
C1 C6 C5 121.5(4) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
N1 C7 C8 122.6(4) . . ?
N1 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C7 C8 C9 118.5(5) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 118.7(5) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N1 C11 N2 120.0(4) . . ?
N1 C11 C10 121.9(5) . . ?
N2 C11 C10 118.1(4) . . ?
N3 C12 N2 119.8(4) . . ?
N3 C12 C13 121.9(4) . . ?
N2 C12 C13 118.3(4) . . ?
C14 C13 C12 119.4(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 117.7(5) . . ?
C16 C15 H15 121.1 . . ?
C14 C15 H15 121.1 . . ?
N3 C16 C15 124.1(5) . . ?
N3 C16 H16 118.0 . . ?
C15 C16 H16 118.0 . . ?
N4 C17 C18 123.3(5) . . ?
N4 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C17 C18 C19 118.2(5) . . ?
C17 C18 H18 120.9 . . ?
C19 C18 H18 120.9 . . ?
C20 C19 C18 120.0(5) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 118.3(4) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
N4 C21 N5 118.7(4) . . ?
N4 C21 C20 121.9(4) . . ?
N5 C21 C20 119.4(4) . . ?
N6 C22 N5 118.5(4) . . ?
N6 C22 C23 121.8(4) . . ?
N5 C22 C23 119.7(4) . . ?
C24 C23 C22 118.6(5) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C23 C24 C25 119.8(5) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 118.3(5) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
N6 C26 C25 122.9(5) . . ?
N6 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?

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
O3 P1 O1 Cu1 -124.10(17) . . . . ?
O2 P1 O1 Cu1 1.60(18) . . . . ?
C1 P1 O1 Cu1 116.23(18) . . . . ?
N3 Cu1 O1 P1 -166.00(17) . . . . ?
N1 Cu1 O1 P1 -44.6(6) . . . . ?
O2 Cu1 O1 P1 -1.25(14) . . . . ?
O3 Cu1 O1 P1 97.14(16) 3_675 . . . ?
O3 P1 O2 Cu1 124.62(17) . . . . ?
O1 P1 O2 Cu1 -1.61(18) . . . . ?
C1 P1 O2 Cu1 -115.68(18) . . . . ?
N3 Cu1 O2 P1 60.4(5) . . . . ?
N1 Cu1 O2 P1 170.04(16) . . . . ?
O1 Cu1 O2 P1 1.26(14) . . . . ?
O3 Cu1 O2 P1 -96.29(16) 3_675 . . . ?
O2 P1 O3 Cu1 -60.5(3) . . . 3_675 ?
O1 P1 O3 Cu1 58.4(3) . . . 3_675 ?
C1 P1 O3 Cu1 178.7(2) . . . 3_675 ?
O6 P2 O4 Cu2 109.2(3) . . . . ?
O5 P2 O4 Cu2 -18.9(4) . . . . ?
C5 P2 O4 Cu2 -134.8(3) . . . . ?
O6 Cu2 O4 P2 -80.4(3) 3_765 . . . ?
N4 Cu2 O4 P2 122.1(3) . . . . ?
N6 Cu2 O4 P2 145.5(17) . . . . ?
O7 Cu2 O4 P2 19.6(3) . . . . ?
O6 P2 O5 V1 -140.5(3) . . . . ?
O4 P2 O5 V1 -9.9(4) . . . . ?
C5 P2 O5 V1 107.4(3) . . . . ?
O7 V1 O5 P2 25.1(3) . . . . ?
O8 V1 O5 P2 135.8(3) . . . . ?
F1 V1 O5 P2 -99.2(3) . . . . ?
O40 V1 O5 P2 -120.5(7) . . . . ?
O4 P2 O6 Cu2 -55.8(5) . . . 3_765 ?
O5 P2 O6 Cu2 72.8(4) . . . 3_765 ?
C5 P2 O6 Cu2 -174.1(4) . . . 3_765 ?
O8 V1 O7 Cu2 -118.2(4) . . . . ?
F1 V1 O7 Cu2 71.1(4) . . . . ?
O5 V1 O7 Cu2 -20.7(4) . . . . ?
O40 V1 O7 Cu2 151.0(4) . . . . ?
O6 Cu2 O7 V1 101.8(4) 3_765 . . . ?
O4 Cu2 O7 V1 7.0(4) . . . . ?
N4 Cu2 O7 V1 -83.6(4) . . . . ?
N6 Cu2 O7 V1 -169.2(4) . . . . ?
N3 Cu1 N1 C11 17.5(4) . . . . ?
O2 Cu1 N1 C11 -145.9(4) . . . . ?
O1 Cu1 N1 C11 -104.6(6) . . . . ?
O3 Cu1 N1 C11 113.0(4) 3_675 . . . ?
N3 Cu1 N1 C7 -159.8(3) . . . . ?
O2 Cu1 N1 C7 36.9(3) . . . . ?
O1 Cu1 N1 C7 78.1(6) . . . . ?
O3 Cu1 N1 C7 -64.3(3) 3_675 . . . ?
N1 Cu1 N3 C12 -24.5(4) . . . . ?
O2 Cu1 N3 C12 85.6(6) . . . . ?
O1 Cu1 N3 C12 141.5(4) . . . . ?
O3 Cu1 N3 C12 -117.4(4) 3_675 . . . ?
N1 Cu1 N3 C16 161.5(4) . . . . ?
O2 Cu1 N3 C16 -88.4(6) . . . . ?
O1 Cu1 N3 C16 -32.5(4) . . . . ?
O3 Cu1 N3 C16 68.6(4) 3_675 . . . ?
O6 Cu2 N4 C21 30.9(6) 3_765 . . . ?
O4 Cu2 N4 C21 133.3(4) . . . . ?
N6 Cu2 N4 C21 -44.8(4) . . . . ?
O7 Cu2 N4 C21 -135.3(4) . . . . ?
O6 Cu2 N4 C17 -138.1(4) 3_765 . . . ?
O4 Cu2 N4 C17 -35.7(4) . . . . ?
N6 Cu2 N4 C17 146.2(4) . . . . ?
O7 Cu2 N4 C17 55.8(4) . . . . ?
O6 Cu2 N6 C26 59.3(4) 3_765 . . . ?
O4 Cu2 N6 C26 -166.4(16) . . . . ?
N4 Cu2 N6 C26 -142.9(4) . . . . ?
O7 Cu2 N6 C26 -40.5(4) . . . . ?
O6 Cu2 N6 C22 -116.9(4) 3_765 . . . ?
O4 Cu2 N6 C22 17(2) . . . . ?
N4 Cu2 N6 C22 40.9(4) . . . . ?
O7 Cu2 N6 C22 143.3(4) . . . . ?
O3 P1 C1 C6 79.2(4) . . . . ?
O2 P1 C1 C6 -45.5(4) . . . . ?
O1 P1 C1 C6 -155.6(3) . . . . ?
O3 P1 C1 C2 -98.3(4) . . . . ?
O2 P1 C1 C2 137.1(4) . . . . ?
O1 P1 C1 C2 26.9(4) . . . . ?
C6 C1 C2 C3 -0.8(7) . . . . ?
P1 C1 C2 C3 176.6(4) . . . . ?
C1 C2 C3 C4 1.8(8) . . . . ?
C2 C3 C4 C5 -0.1(8) . . . . ?
C3 C4 C5 C6 -2.5(7) . . . . ?
C3 C4 C5 P2 177.3(4) . . . . ?
O6 P2 C5 C4 21.7(4) . . . . ?
O4 P2 C5 C4 -101.8(4) . . . . ?
O5 P2 C5 C4 138.4(4) . . . . ?
O6 P2 C5 C6 -158.5(4) . . . . ?
O4 P2 C5 C6 78.1(4) . . . . ?
O5 P2 C5 C6 -41.8(4) . . . . ?
C2 C1 C6 C5 -1.9(7) . . . . ?
P1 C1 C6 C5 -179.4(3) . . . . ?
C4 C5 C6 C1 3.5(7) . . . . ?
P2 C5 C6 C1 -176.3(3) . . . . ?
C11 N1 C7 C8 1.4(7) . . . . ?
Cu1 N1 C7 C8 178.9(4) . . . . ?
N1 C7 C8 C9 -1.5(8) . . . . ?
C7 C8 C9 C10 0.5(8) . . . . ?
C8 C9 C10 C11 0.6(8) . . . . ?
C7 N1 C11 N2 -180.0(4) . . . . ?
Cu1 N1 C11 N2 2.8(6) . . . . ?
C7 N1 C11 C10 -0.2(7) . . . . ?
Cu1 N1 C11 C10 -177.4(3) . . . . ?
C12 N2 C11 N1 -28.8(7) . . . . ?
C12 N2 C11 C10 151.5(5) . . . . ?
C9 C10 C11 N1 -0.8(7) . . . . ?
C9 C10 C11 N2 179.0(4) . . . . ?
C16 N3 C12 N2 -175.0(4) . . . . ?
Cu1 N3 C12 N2 11.0(6) . . . . ?
C16 N3 C12 C13 4.7(7) . . . . ?
Cu1 N3 C12 C13 -169.3(4) . . . . ?
C11 N2 C12 N3 21.3(7) . . . . ?
C11 N2 C12 C13 -158.5(5) . . . . ?
N3 C12 C13 C14 -3.5(7) . . . . ?
N2 C12 C13 C14 176.2(5) . . . . ?
C12 C13 C14 C15 0.3(8) . . . . ?
C13 C14 C15 C16 1.4(8) . . . . ?
C12 N3 C16 C15 -2.9(7) . . . . ?
Cu1 N3 C16 C15 171.5(4) . . . . ?
C14 C15 C16 N3 -0.1(8) . . . . ?
C21 N4 C17 C18 -3.5(7) . . . . ?
Cu2 N4 C17 C18 165.9(4) . . . . ?
N4 C17 C18 C19 -0.4(8) . . . . ?
C17 C18 C19 C20 2.5(8) . . . . ?
C18 C19 C20 C21 -0.8(8) . . . . ?
C17 N4 C21 N5 -174.0(4) . . . . ?
Cu2 N4 C21 N5 16.9(6) . . . . ?
C17 N4 C21 C20 5.3(7) . . . . ?
Cu2 N4 C21 C20 -163.7(3) . . . . ?
C22 N5 C21 N4 36.1(6) . . . . ?
C22 N5 C21 C20 -143.2(5) . . . . ?
C19 C20 C21 N4 -3.3(7) . . . . ?
C19 C20 C21 N5 176.1(4) . . . . ?
C26 N6 C22 N5 174.7(4) . . . . ?
Cu2 N6 C22 N5 -9.1(6) . . . . ?
C26 N6 C22 C23 -4.2(7) . . . . ?
Cu2 N6 C22 C23 172.0(3) . . . . ?
C21 N5 C22 N6 -40.3(6) . . . . ?
C21 N5 C22 C23 138.6(5) . . . . ?
N6 C22 C23 C24 4.1(7) . . . . ?
N5 C22 C23 C24 -174.9(5) . . . . ?
C22 C23 C24 C25 -1.5(8) . . . . ?
C23 C24 C25 C26 -0.7(8) . . . . ?
C22 N6 C26 C25 1.9(7) . . . . ?
Cu2 N6 C26 C25 -174.5(4) . . . . ?
C24 C25 C26 N6 0.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.145

data_5
_database_code_depnum_ccdc_archive 'CCDC 734625'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H22 CU2 F2 N6 O10 P2 V2'
_chemical_formula_sum            'C26 H22 Cu2 F2 N6 O10 P2 V2'
_chemical_formula_weight         907.40

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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 '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   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   19.628(2)
_cell_length_b                   8.5882(9)
_cell_length_c                   19.245(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.378(2)
_cell_angle_gamma                90.00
_cell_volume                     2999.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6962
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.30

_exptl_crystal_description       plate
_exptl_crystal_colour            dark
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4743
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            14477
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         28.07
_reflns_number_total             3667
_reflns_number_gt                3541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0324P)²+26.7388P] where P=(Fo²+2Fc²)/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         3667
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1203
_refine_ls_wR_factor_gt          0.1192
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_restrained_S_all      1.308
_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 0.17809(2) 0.48466(6) 0.08682(2) 0.01249(13) Uani 1 1 d . . .
V1 V 0.29258(3) 0.27521(8) 0.27160(4) 0.01311(16) Uani 1 1 d . . .
P1 P 0.13112(5) 0.45437(11) 0.21962(5) 0.0110(2) Uani 1 1 d . . .
F1 F 0.25538(13) 0.2932(3) 0.16566(13) 0.0201(5) Uani 1 1 d . . .
O1 O 0.13832(15) 0.6251(3) 0.24620(15) 0.0155(6) Uani 1 1 d . . .
O2 O 0.19976(15) 0.3619(4) 0.26629(15) 0.0187(6) Uani 1 1 d . . .
O3 O 0.11178(14) 0.4358(3) 0.13568(14) 0.0131(5) Uani 1 1 d . . .
O4 O 0.20742(18) 0.6585(4) 0.15591(17) 0.0249(7) Uani 1 1 d . . .
O5 O 0.34852(16) 0.4157(4) 0.30679(18) 0.0233(6) Uani 1 1 d . . .
N1 N 0.25296(18) 0.5357(4) 0.04422(18) 0.0150(6) Uani 1 1 d . . .
N2 N 0.2021(2) 0.3742(5) -0.0632(2) 0.0190(7) Uani 1 1 d . . .
N3 N 0.11514(18) 0.3740(4) -0.00589(19) 0.0174(7) Uani 1 1 d . . .
C1 C 0.0000 0.4454(6) 0.2500 0.0118(10) Uani 1 2 d S . .
H1 H 0.0000 0.5560 0.2500 0.014 Uiso 1 2 calc SR . .
C2 C 0.05679(19) 0.3647(4) 0.2381(2) 0.0110(7) Uani 1 1 d . . .
C3 C 0.0553(2) 0.2022(5) 0.2367(2) 0.0184(8) Uani 1 1 d . . .
H3 H 0.0922 0.1460 0.2267 0.022 Uiso 1 1 calc R . .
C4 C 0.0000 0.1231(6) 0.2500 0.0187(11) Uani 1 2 d S . .
H4 H 0.0000 0.0125 0.2500 0.022 Uiso 1 2 calc SR . .
C5 C 0.3086(2) 0.6323(5) 0.0851(2) 0.0202(8) Uani 1 1 d . . .
H5 H 0.3058 0.6808 0.1283 0.024 Uiso 1 1 calc R . .
C6 C 0.3684(2) 0.6634(6) 0.0674(2) 0.0242(9) Uani 1 1 d . . .
H6 H 0.4054 0.7341 0.0966 0.029 Uiso 1 1 calc R . .
C7 C 0.3734(3) 0.5880(6) 0.0049(3) 0.0277(10) Uani 1 1 d . . .
H7 H 0.4157 0.6018 -0.0071 0.033 Uiso 1 1 calc R . .
C8 C 0.3173(2) 0.4950(5) -0.0384(2) 0.0229(9) Uani 1 1 d . . .
H8 H 0.3192 0.4466 -0.0820 0.027 Uiso 1 1 calc R . .
C9 C 0.2563(2) 0.4705(5) -0.0182(2) 0.0158(8) Uani 1 1 d . . .
C10 C 0.1350(2) 0.3338(5) -0.0632(2) 0.0141(7) Uani 1 1 d . . .
C11 C 0.0877(2) 0.2496(5) -0.1255(2) 0.0191(8) Uani 1 1 d . . .
H11 H 0.1044 0.2152 -0.1632 0.023 Uiso 1 1 calc R . .
C12 C 0.0180(3) 0.2176(6) -0.1315(2) 0.0245(9) Uani 1 1 d . . .
H12 H -0.0148 0.1627 -0.1739 0.029 Uiso 1 1 calc R . .
C13 C -0.0048(2) 0.2659(6) -0.0749(2) 0.0227(9) Uani 1 1 d . . .
H13 H -0.0540 0.2487 -0.0790 0.027 Uiso 1 1 calc R . .
C14 C 0.0446(2) 0.3384(5) -0.0133(2) 0.0217(9) Uani 1 1 d . . .
H14 H 0.0294 0.3656 0.0265 0.026 Uiso 1 1 calc R . .
H2' H 0.211(3) 0.347(6) -0.093(3) 0.011(12) Uiso 1 1 d . . .


_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 O3 1.920(3) . ?
Cu1 O4 1.935(3) . ?
Cu1 N3 1.984(3) . ?
Cu1 N1 1.985(3) . ?
Cu1 F1 2.357(2) . ?
V1 O5 1.598(3) . ?
V1 O4 1.718(3) 4_545 ?
V1 F1 1.892(2) . ?
V1 O2 1.934(3) . ?
V1 O1 1.994(3) 4_545 ?
P1 O3 1.521(3) . ?
P1 O2 1.527(3) . ?
P1 O1 1.541(3) . ?
P1 C2 1.801(4) . ?
O1 V1 1.994(3) 4 ?
O4 V1 1.718(3) 4 ?
N1 C9 1.349(5) . ?
N1 C5 1.358(5) . ?
N2 C10 1.362(5) . ?
N2 C9 1.366(5) . ?
N2 H2' 0.70(5) . ?
N3 C10 1.348(5) . ?
N3 C14 1.372(5) . ?
C1 C2 1.403(4) 2 ?
C1 C2 1.403(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.396(5) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9500 . ?
C4 C3 1.385(5) 2 ?
C4 H4 0.9500 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.403(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.359(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.408(6) . ?
C8 H8 0.9500 . ?
C10 C11 1.405(6) . ?
C11 C12 1.356(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.390(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.362(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?

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
O3 Cu1 O4 84.95(11) . . ?
O3 Cu1 N3 91.69(13) . . ?
O4 Cu1 N3 155.23(15) . . ?
O3 Cu1 N1 175.51(12) . . ?
O4 Cu1 N1 92.30(13) . . ?
N3 Cu1 N1 92.28(14) . . ?
O3 Cu1 F1 85.55(10) . . ?
O4 Cu1 F1 98.39(13) . . ?
N3 Cu1 F1 105.83(12) . . ?
N1 Cu1 F1 91.35(11) . . ?
O5 V1 O4 107.99(17) . 4_545 ?
O5 V1 F1 108.42(15) . . ?
O4 V1 F1 143.45(15) 4_545 . ?
O5 V1 O2 102.31(15) . . ?
O4 V1 O2 88.64(13) 4_545 . ?
F1 V1 O2 86.70(11) . . ?
O5 V1 O1 99.12(14) . 4_545 ?
O4 V1 O1 88.43(12) 4_545 4_545 ?
F1 V1 O1 82.89(11) . 4_545 ?
O2 V1 O1 158.22(13) . 4_545 ?
O3 P1 O2 112.20(15) . . ?
O3 P1 O1 113.99(16) . . ?
O2 P1 O1 110.53(17) . . ?
O3 P1 C2 105.76(16) . . ?
O2 P1 C2 105.14(17) . . ?
O1 P1 C2 108.66(16) . . ?
V1 F1 Cu1 129.81(12) . . ?
P1 O1 V1 122.72(15) . 4 ?
P1 O2 V1 146.48(18) . . ?
P1 O3 Cu1 123.76(16) . . ?
V1 O4 Cu1 156.36(17) 4 . ?
C9 N1 C5 117.9(3) . . ?
C9 N1 Cu1 124.8(3) . . ?
C5 N1 Cu1 117.0(3) . . ?
C10 N2 C9 132.3(4) . . ?
C10 N2 H2' 117(4) . . ?
C9 N2 H2' 111(4) . . ?
C10 N3 C14 116.9(3) . . ?
C10 N3 Cu1 125.7(3) . . ?
C14 N3 Cu1 117.3(3) . . ?
C2 C1 C2 120.8(5) 2 . ?
C2 C1 H1 119.6 2 . ?
C2 C1 H1 119.6 . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 P1 115.9(3) . . ?
C1 C2 P1 125.1(3) . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C3 121.2(5) . 2 ?
C3 C4 H4 119.4 . . ?
C3 C4 H4 119.4 2 . ?
N1 C5 C6 123.6(4) . . ?
N1 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C5 C6 C7 118.0(4) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
C8 C7 C6 119.5(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.6(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
N1 C9 N2 121.8(3) . . ?
N1 C9 C8 121.2(4) . . ?
N2 C9 C8 117.0(4) . . ?
N3 C10 N2 121.1(4) . . ?
N3 C10 C11 121.8(4) . . ?
N2 C10 C11 117.1(4) . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 119.2(4) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 N3 123.2(4) . . ?
C13 C14 H14 118.4 . . ?
N3 C14 H14 118.4 . . ?

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
O5 V1 F1 Cu1 -66.86(19) . . . . ?
O4 V1 F1 Cu1 118.2(2) 4_545 . . . ?
O2 V1 F1 Cu1 35.02(17) . . . . ?
O1 V1 F1 Cu1 -164.15(17) 4_545 . . . ?
O3 Cu1 F1 V1 -54.89(17) . . . . ?
O4 Cu1 F1 V1 29.33(18) . . . . ?
N3 Cu1 F1 V1 -145.40(17) . . . . ?
N1 Cu1 F1 V1 121.85(18) . . . . ?
O3 P1 O1 V1 -56.6(2) . . . 4 ?
O2 P1 O1 V1 70.9(2) . . . 4 ?
C2 P1 O1 V1 -174.21(18) . . . 4 ?
O3 P1 O2 V1 28.3(4) . . . . ?
O1 P1 O2 V1 -100.1(4) . . . . ?
C2 P1 O2 V1 142.8(3) . . . . ?
O5 V1 O2 P1 88.8(4) . . . . ?
O4 V1 O2 P1 -163.1(4) 4_545 . . . ?
F1 V1 O2 P1 -19.3(4) . . . . ?
O1 V1 O2 P1 -80.7(5) 4_545 . . . ?
O2 P1 O3 Cu1 -57.0(2) . . . . ?
O1 P1 O3 Cu1 69.6(2) . . . . ?
C2 P1 O3 Cu1 -171.09(19) . . . . ?
O4 Cu1 O3 P1 -38.2(2) . . . . ?
N3 Cu1 O3 P1 166.3(2) . . . . ?
N1 Cu1 O3 P1 14.0(18) . . . . ?
F1 Cu1 O3 P1 60.60(19) . . . . ?
O3 Cu1 O4 V1 2.0(6) . . . 4 ?
N3 Cu1 O4 V1 85.1(6) . . . 4 ?
N1 Cu1 O4 V1 -174.4(6) . . . 4 ?
F1 Cu1 O4 V1 -82.7(6) . . . 4 ?
O3 Cu1 N1 C9 138.7(16) . . . . ?
O4 Cu1 N1 C9 -169.3(3) . . . . ?
N3 Cu1 N1 C9 -13.6(3) . . . . ?
F1 Cu1 N1 C9 92.3(3) . . . . ?
O3 Cu1 N1 C5 -34.8(18) . . . . ?
O4 Cu1 N1 C5 17.2(3) . . . . ?
N3 Cu1 N1 C5 172.9(3) . . . . ?
F1 Cu1 N1 C5 -81.2(3) . . . . ?
O3 Cu1 N3 C10 -166.5(3) . . . . ?
O4 Cu1 N3 C10 111.9(4) . . . . ?
N1 Cu1 N3 C10 11.4(3) . . . . ?
F1 Cu1 N3 C10 -80.7(3) . . . . ?
O3 Cu1 N3 C14 15.1(3) . . . . ?
O4 Cu1 N3 C14 -66.5(5) . . . . ?
N1 Cu1 N3 C14 -167.0(3) . . . . ?
F1 Cu1 N3 C14 101.0(3) . . . . ?
C2 C1 C2 C3 1.3(3) 2 . . . ?
C2 C1 C2 P1 178.2(3) 2 . . . ?
O3 P1 C2 C3 74.0(3) . . . . ?
O2 P1 C2 C3 -44.9(3) . . . . ?
O1 P1 C2 C3 -163.2(3) . . . . ?
O3 P1 C2 C1 -102.9(3) . . . . ?
O2 P1 C2 C1 138.2(3) . . . . ?
O1 P1 C2 C1 19.8(3) . . . . ?
C1 C2 C3 C4 -2.6(5) . . . . ?
P1 C2 C3 C4 -179.8(2) . . . . ?
C2 C3 C4 C3 1.3(3) . . . 2 ?
C9 N1 C5 C6 -1.8(6) . . . . ?
Cu1 N1 C5 C6 172.2(4) . . . . ?
N1 C5 C6 C7 -1.8(7) . . . . ?
C5 C6 C7 C8 4.0(7) . . . . ?
C6 C7 C8 C9 -2.5(7) . . . . ?
C5 N1 C9 N2 -178.8(4) . . . . ?
Cu1 N1 C9 N2 7.7(6) . . . . ?
C5 N1 C9 C8 3.3(6) . . . . ?
Cu1 N1 C9 C8 -170.1(3) . . . . ?
C10 N2 C9 N1 7.0(7) . . . . ?
C10 N2 C9 C8 -175.1(4) . . . . ?
C7 C8 C9 N1 -1.2(7) . . . . ?
C7 C8 C9 N2 -179.1(4) . . . . ?
C14 N3 C10 N2 175.3(4) . . . . ?
Cu1 N3 C10 N2 -3.0(6) . . . . ?
C14 N3 C10 C11 -4.4(6) . . . . ?
Cu1 N3 C10 C11 177.3(3) . . . . ?
C9 N2 C10 N3 -9.5(7) . . . . ?
C9 N2 C10 C11 170.2(4) . . . . ?
N3 C10 C11 C12 5.2(6) . . . . ?
N2 C10 C11 C12 -174.5(4) . . . . ?
C10 C11 C12 C13 -1.4(7) . . . . ?
C11 C12 C13 C14 -2.8(7) . . . . ?
C12 C13 C14 N3 3.6(7) . . . . ?
C10 N3 C14 C13 0.0(7) . . . . ?
Cu1 N3 C14 C13 178.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.136

data_6
_database_code_depnum_ccdc_archive 'CCDC 734626'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H15 Cu N2 O9 P2 V'
_chemical_formula_sum            'C18 H15 Cu N2 O9 P2 V'
_chemical_formula_weight         579.74

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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   10.9327(7)
_cell_length_b                   16.1475(10)
_cell_length_c                   11.8455(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.3100(10)
_cell_angle_gamma                90.00
_cell_volume                     2026.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5035
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1164
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_T_max  0.7239
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            21180
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         28.30
_reflns_number_total             5035
_reflns_number_gt                4940
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0168P)²+6.6188P] where P=(Fo²+2Fc²)/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         5035
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0906
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_restrained_S_all      1.268
_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
Cu1 Cu 0.95392(3) 0.70664(2) 0.51571(3) 0.00875(9) Uani 1 1 d . . .
V1 V 0.53901(4) 1.23662(3) 0.53594(4) 0.00970(10) Uani 1 1 d . . .
P1 P 1.01287(7) 0.82346(4) 0.74306(6) 0.00873(14) Uani 1 1 d . . .
P2 P 0.80261(7) 1.16693(4) 0.50545(6) 0.00905(14) Uani 1 1 d . . .
O1 O 0.95094(19) 0.75323(12) 0.66506(18) 0.0127(4) Uani 1 1 d . . .
O2 O 0.9679(2) 0.82068(12) 0.85830(18) 0.0124(4) Uani 1 1 d . . .
O3 O 1.15572(19) 0.82553(13) 0.77210(17) 0.0121(4) Uani 1 1 d . . .
O4 O 0.72747(19) 1.14832(13) 0.37912(18) 0.0127(4) Uani 1 1 d . . .
O5 O 0.90790(19) 1.22695(13) 0.51332(19) 0.0140(4) Uani 1 1 d . . .
O6 O 0.70398(19) 1.19562(13) 0.57089(18) 0.0137(4) Uani 1 1 d . . .
O7 O 0.5027(2) 1.27621(14) 0.40745(19) 0.0196(5) Uani 1 1 d . . .
O8 O 0.4381(2) 1.16370(14) 0.5419(2) 0.0190(5) Uani 1 1 d . . .
O40 O 0.8032(2) 0.78637(14) 0.4071(2) 0.0143(4) Uani 1 1 d . . .
N1 N 0.9694(2) 0.62751(15) 0.3886(2) 0.0105(5) Uani 1 1 d . . .
N2 N 0.8310(2) 0.61941(15) 0.5417(2) 0.0096(4) Uani 1 1 d . . .
C1 C 0.9546(3) 0.92018(17) 0.6760(2) 0.0091(5) Uani 1 1 d . . .
C2 C 1.0355(3) 0.98713(18) 0.6803(2) 0.0111(5) Uani 1 1 d . . .
H2 H 1.1224 0.9814 0.7183 0.013 Uiso 1 1 calc R . .
C3 C 0.9901(3) 1.06292(17) 0.6291(2) 0.0107(5) Uani 1 1 d . . .
H3 H 1.0457 1.1087 0.6335 0.013 Uiso 1 1 calc R . .
C4 C 0.8630(3) 1.07081(17) 0.5718(2) 0.0093(5) Uani 1 1 d . . .
C5 C 0.7816(3) 1.00292(18) 0.5657(2) 0.0116(5) Uani 1 1 d . . .
H5 H 0.6950 1.0080 0.5261 0.014 Uiso 1 1 calc R . .
C6 C 0.8272(3) 0.92829(17) 0.6175(2) 0.0110(5) Uani 1 1 d . . .
H6 H 0.7718 0.8825 0.6133 0.013 Uiso 1 1 calc R . .
C7 C 1.0372(3) 0.63460(19) 0.3102(3) 0.0138(6) Uani 1 1 d . . .
H7 H 1.0824 0.6845 0.3073 0.017 Uiso 1 1 calc R . .
C8 C 1.0442(3) 0.5707(2) 0.2315(3) 0.0173(6) Uani 1 1 d . . .
H8 H 1.0929 0.5781 0.1760 0.021 Uiso 1 1 calc R . .
C9 C 0.9810(3) 0.4979(2) 0.2346(3) 0.0166(6) Uani 1 1 d . . .
H9 H 0.9876 0.4539 0.1833 0.020 Uiso 1 1 calc R . .
C10 C 0.9058(3) 0.48913(18) 0.3152(2) 0.0127(5) Uani 1 1 d . . .
C11 C 0.9030(3) 0.55601(18) 0.3898(2) 0.0106(5) Uani 1 1 d . . .
C12 C 0.8321(3) 0.41682(18) 0.3244(3) 0.0154(6) Uani 1 1 d . . .
H12 H 0.8363 0.3701 0.2768 0.019 Uiso 1 1 calc R . .
C13 C 0.7568(3) 0.41413(19) 0.3995(3) 0.0168(6) Uani 1 1 d . . .
H13 H 0.7074 0.3662 0.4024 0.020 Uiso 1 1 calc R . .
C14 C 0.7507(3) 0.48318(18) 0.4753(3) 0.0128(5) Uani 1 1 d . . .
C15 C 0.8265(3) 0.55262(17) 0.4712(2) 0.0100(5) Uani 1 1 d . . .
C16 C 0.6717(3) 0.48643(19) 0.5533(3) 0.0158(6) Uani 1 1 d . . .
H16 H 0.6178 0.4412 0.5588 0.019 Uiso 1 1 calc R . .
C17 C 0.6736(3) 0.55557(19) 0.6210(3) 0.0152(6) Uani 1 1 d . . .
H17 H 0.6191 0.5592 0.6720 0.018 Uiso 1 1 calc R . .
C18 C 0.7564(3) 0.62097(18) 0.6148(3) 0.0130(5) Uani 1 1 d . . .
H18 H 0.7590 0.6676 0.6642 0.016 Uiso 1 1 calc R . .
H4' H 0.768(5) 1.156(3) 0.327(4) 0.044(14) Uiso 1 1 d . . .
H40B H 0.759(4) 0.751(3) 0.364(4) 0.033(12) Uiso 1 1 d . . .
H40A H 0.764(4) 0.808(3) 0.435(4) 0.021(11) Uiso 1 1 d . . .


_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 1.930(2) . ?
Cu1 O5 1.951(2) 3_776 ?
Cu1 N1 2.014(2) . ?
Cu1 N2 2.022(2) . ?
Cu1 O40 2.232(2) . ?
V1 O7 1.608(2) . ?
V1 O8 1.627(2) . ?
V1 O2 1.861(2) 2_656 ?
V1 O6 1.869(2) . ?
P1 O1 1.513(2) . ?
P1 O3 1.514(2) . ?
P1 O2 1.562(2) . ?
P1 C1 1.796(3) . ?
P2 O5 1.490(2) . ?
P2 O6 1.546(2) . ?
P2 O4 1.548(2) . ?
P2 C4 1.791(3) . ?
O2 V1 1.861(2) 2_646 ?
O4 H4' 0.86(5) . ?
O5 Cu1 1.951(2) 3_776 ?
O40 H40B 0.84(5) . ?
O40 H40A 0.70(4) . ?
N1 C7 1.328(4) . ?
N1 C11 1.366(4) . ?
N2 C18 1.328(4) . ?
N2 C15 1.357(4) . ?
C1 C2 1.390(4) . ?
C1 C6 1.400(4) . ?
C2 C3 1.401(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(4) . ?
C5 C6 1.388(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.405(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.412(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.400(4) . ?
C10 C12 1.438(4) . ?
C11 C15 1.425(4) . ?
C12 C13 1.355(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.443(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.402(4) . ?
C14 C16 1.414(4) . ?
C16 C17 1.371(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.404(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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 O5 97.84(9) . 3_776 ?
O1 Cu1 N1 163.02(9) . . ?
O5 Cu1 N1 90.28(9) 3_776 . ?
O1 Cu1 N2 88.25(9) . . ?
O5 Cu1 N2 169.19(9) 3_776 . ?
N1 Cu1 N2 81.61(10) . . ?
O1 Cu1 O40 97.26(9) . . ?
O5 Cu1 O40 94.28(9) 3_776 . ?
N1 Cu1 O40 96.97(9) . . ?
N2 Cu1 O40 93.79(9) . . ?
O7 V1 O8 108.53(13) . . ?
O7 V1 O2 107.80(11) . 2_656 ?
O8 V1 O2 110.98(10) . 2_656 ?
O7 V1 O6 110.44(11) . . ?
O8 V1 O6 111.20(11) . . ?
O2 V1 O6 107.85(9) 2_656 . ?
O1 P1 O3 115.85(12) . . ?
O1 P1 O2 108.79(12) . . ?
O3 P1 O2 109.40(12) . . ?
O1 P1 C1 108.99(12) . . ?
O3 P1 C1 108.32(12) . . ?
O2 P1 C1 104.94(12) . . ?
O5 P2 O6 113.42(12) . . ?
O5 P2 O4 113.82(12) . . ?
O6 P2 O4 105.87(12) . . ?
O5 P2 C4 109.93(13) . . ?
O6 P2 C4 105.49(12) . . ?
O4 P2 C4 107.82(12) . . ?
P1 O1 Cu1 138.21(13) . . ?
P1 O2 V1 133.09(13) . 2_646 ?
P2 O4 H4' 115(3) . . ?
P2 O5 Cu1 165.08(15) . 3_776 ?
P2 O6 V1 138.54(13) . . ?
Cu1 O40 H40B 101(3) . . ?
Cu1 O40 H40A 118(3) . . ?
H40B O40 H40A 108(4) . . ?
C7 N1 C11 118.1(3) . . ?
C7 N1 Cu1 129.2(2) . . ?
C11 N1 Cu1 112.64(19) . . ?
C18 N2 C15 118.8(2) . . ?
C18 N2 Cu1 128.6(2) . . ?
C15 N2 Cu1 112.59(18) . . ?
C2 C1 C6 119.5(3) . . ?
C2 C1 P1 120.5(2) . . ?
C6 C1 P1 120.1(2) . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 P2 120.6(2) . . ?
C5 C4 P2 119.6(2) . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
N1 C7 C8 122.1(3) . . ?
N1 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.1(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 117.1(3) . . ?
C11 C10 C12 118.6(3) . . ?
C9 C10 C12 124.3(3) . . ?
N1 C11 C10 123.4(3) . . ?
N1 C11 C15 116.2(3) . . ?
C10 C11 C15 120.4(3) . . ?
C13 C12 C10 121.2(3) . . ?
C13 C12 H12 119.4 . . ?
C10 C12 H12 119.4 . . ?
C12 C13 C14 120.9(3) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C16 117.0(3) . . ?
C15 C14 C13 118.5(3) . . ?
C16 C14 C13 124.4(3) . . ?
N2 C15 C14 123.1(3) . . ?
N2 C15 C11 116.6(2) . . ?
C14 C15 C11 120.3(3) . . ?
C17 C16 C14 119.2(3) . . ?
C17 C16 H16 120.4 . . ?
C14 C16 H16 120.4 . . ?
C16 C17 C18 119.9(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N2 C18 C17 121.8(3) . . ?
N2 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?

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
O3 P1 O1 Cu1 -53.3(2) . . . . ?
O2 P1 O1 Cu1 -176.99(17) . . . . ?
C1 P1 O1 Cu1 69.1(2) . . . . ?
O5 Cu1 O1 P1 7.0(2) 3_776 . . . ?
N1 Cu1 O1 P1 124.9(3) . . . . ?
N2 Cu1 O1 P1 178.1(2) . . . . ?
O40 Cu1 O1 P1 -88.3(2) . . . . ?
O1 P1 O2 V1 50.3(2) . . . 2_646 ?
O3 P1 O2 V1 -77.19(19) . . . 2_646 ?
C1 P1 O2 V1 166.77(17) . . . 2_646 ?
O6 P2 O5 Cu1 -150.6(5) . . . 3_776 ?
O4 P2 O5 Cu1 -29.5(6) . . . 3_776 ?
C4 P2 O5 Cu1 91.6(6) . . . 3_776 ?
O5 P2 O6 V1 106.6(2) . . . . ?
O4 P2 O6 V1 -18.9(2) . . . . ?
C4 P2 O6 V1 -133.0(2) . . . . ?
O7 V1 O6 P2 -21.4(2) . . . . ?
O8 V1 O6 P2 99.2(2) . . . . ?
O2 V1 O6 P2 -138.95(19) 2_656 . . . ?
O1 Cu1 N1 C7 -128.4(3) . . . . ?
O5 Cu1 N1 C7 -9.5(3) 3_776 . . . ?
N2 Cu1 N1 C7 177.6(3) . . . . ?
O40 Cu1 N1 C7 84.8(3) . . . . ?
O1 Cu1 N1 C11 48.7(4) . . . . ?
O5 Cu1 N1 C11 167.61(19) 3_776 . . . ?
N2 Cu1 N1 C11 -5.22(18) . . . . ?
O40 Cu1 N1 C11 -98.04(19) . . . . ?
O1 Cu1 N2 C18 19.1(2) . . . . ?
O5 Cu1 N2 C18 143.7(4) 3_776 . . . ?
N1 Cu1 N2 C18 -174.5(3) . . . . ?
O40 Cu1 N2 C18 -78.0(2) . . . . ?
O1 Cu1 N2 C15 -162.29(19) . . . . ?
O5 Cu1 N2 C15 -37.7(6) 3_776 . . . ?
N1 Cu1 N2 C15 4.05(18) . . . . ?
O40 Cu1 N2 C15 100.55(19) . . . . ?
O1 P1 C1 C2 -140.1(2) . . . . ?
O3 P1 C1 C2 -13.2(3) . . . . ?
O2 P1 C1 C2 103.5(2) . . . . ?
O1 P1 C1 C6 39.1(3) . . . . ?
O3 P1 C1 C6 165.9(2) . . . . ?
O2 P1 C1 C6 -77.3(2) . . . . ?
C6 C1 C2 C3 1.5(4) . . . . ?
P1 C1 C2 C3 -179.3(2) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C2 C3 C4 P2 -179.9(2) . . . . ?
O5 P2 C4 C3 5.2(3) . . . . ?
O6 P2 C4 C3 -117.4(2) . . . . ?
O4 P2 C4 C3 129.8(2) . . . . ?
O5 P2 C4 C5 -174.7(2) . . . . ?
O6 P2 C4 C5 62.7(2) . . . . ?
O4 P2 C4 C5 -50.1(3) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
P2 C4 C5 C6 -179.5(2) . . . . ?
C4 C5 C6 C1 -0.1(4) . . . . ?
C2 C1 C6 C5 -0.9(4) . . . . ?
P1 C1 C6 C5 179.9(2) . . . . ?
C11 N1 C7 C8 -1.4(4) . . . . ?
Cu1 N1 C7 C8 175.7(2) . . . . ?
N1 C7 C8 C9 -0.6(5) . . . . ?
C7 C8 C9 C10 2.0(4) . . . . ?
C8 C9 C10 C11 -1.4(4) . . . . ?
C8 C9 C10 C12 178.0(3) . . . . ?
C7 N1 C11 C10 2.0(4) . . . . ?
Cu1 N1 C11 C10 -175.5(2) . . . . ?
C7 N1 C11 C15 -176.9(2) . . . . ?
Cu1 N1 C11 C15 5.6(3) . . . . ?
C9 C10 C11 N1 -0.7(4) . . . . ?
C12 C10 C11 N1 179.9(3) . . . . ?
C9 C10 C11 C15 178.2(3) . . . . ?
C12 C10 C11 C15 -1.2(4) . . . . ?
C11 C10 C12 C13 2.9(4) . . . . ?
C9 C10 C12 C13 -176.5(3) . . . . ?
C10 C12 C13 C14 -1.7(4) . . . . ?
C12 C13 C14 C15 -1.3(4) . . . . ?
C12 C13 C14 C16 177.8(3) . . . . ?
C18 N2 C15 C14 -3.0(4) . . . . ?
Cu1 N2 C15 C14 178.3(2) . . . . ?
C18 N2 C15 C11 176.5(2) . . . . ?
Cu1 N2 C15 C11 -2.3(3) . . . . ?
C16 C14 C15 N2 3.2(4) . . . . ?
C13 C14 C15 N2 -177.6(3) . . . . ?
C16 C14 C15 C11 -176.2(3) . . . . ?
C13 C14 C15 C11 3.0(4) . . . . ?
N1 C11 C15 N2 -2.2(4) . . . . ?
C10 C11 C15 N2 178.8(2) . . . . ?
N1 C11 C15 C14 177.2(2) . . . . ?
C10 C11 C15 C14 -1.7(4) . . . . ?
C15 C14 C16 C17 -0.7(4) . . . . ?
C13 C14 C16 C17 -179.8(3) . . . . ?
C14 C16 C17 C18 -1.9(4) . . . . ?
C15 N2 C18 C17 0.2(4) . . . . ?
Cu1 N2 C18 C17 178.7(2) . . . . ?
C16 C17 C18 N2 2.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.102

data_7a
_database_code_depnum_ccdc_archive 'CCDC 734627'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_sum            'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_weight         561.72

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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   8.2372(6)
_cell_length_b                   16.1717(11)
_cell_length_c                   15.1183(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.7140(10)
_cell_angle_gamma                90.00
_cell_volume                     1972.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5783
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.29

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5382
_exptl_absorpt_correction_T_max  0.8715
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            20519
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         28.29
_reflns_number_total             4879
_reflns_number_gt                4778
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0255P)²+5.5059P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         4879
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_restrained_S_all      1.272
_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 0.52395(4) 0.19944(2) 0.06317(2) 0.00941(9) Uani 1 1 d . . .
V1 V 0.95700(5) 0.23288(3) 0.17306(3) 0.00949(10) Uani 1 1 d . . .
P1 P 1.21388(9) 0.31798(4) 0.06978(5) 0.01019(14) Uani 1 1 d . . .
P2 P 1.52482(9) 0.68186(4) 0.12142(5) 0.00993(14) Uani 1 1 d . . .
O1 O 1.1298(2) 0.30657(12) -0.02875(13) 0.0140(4) Uani 1 1 d . . .
O2 O 1.3513(3) 0.25815(12) 0.10621(14) 0.0149(4) Uani 1 1 d . . .
O3 O 1.0795(3) 0.31350(12) 0.12910(14) 0.0136(4) Uani 1 1 d . . .
O4 O 1.4683(2) 0.72453(12) 0.20244(13) 0.0132(4) Uani 1 1 d . . .
O5 O 1.4623(3) 0.72803(12) 0.03544(13) 0.0141(4) Uani 1 1 d . . .
O6 O 1.7129(2) 0.67132(13) 0.14708(14) 0.0146(4) Uani 1 1 d . . .
H6' H 1.7537 0.6766 0.1008 0.022 Uiso 1 1 calc R . .
O7 O 0.9770(3) 0.14359(13) 0.12983(15) 0.0182(4) Uani 1 1 d . . .
O8 O 0.7612(2) 0.25800(12) 0.14867(13) 0.0134(4) Uani 1 1 d . . .
N1 N 0.6463(3) 0.11013(15) 0.01124(16) 0.0124(4) Uani 1 1 d . . .
N2 N 0.5199(3) 0.11356(14) 0.15762(16) 0.0118(4) Uani 1 1 d . . .
C1 C 1.2953(3) 0.42136(16) 0.08526(18) 0.0109(5) Uani 1 1 d . . .
C2 C 1.4102(4) 0.44177(18) 0.16380(19) 0.0145(5) Uani 1 1 d . . .
H2 H 1.4434 0.4011 0.2092 0.017 Uiso 1 1 calc R . .
C3 C 1.4761(4) 0.52103(17) 0.17606(19) 0.0142(5) Uani 1 1 d . . .
H3 H 1.5525 0.5345 0.2301 0.017 Uiso 1 1 calc R . .
C4 C 1.4302(3) 0.58118(16) 0.10898(18) 0.0104(5) Uani 1 1 d . . .
C5 C 1.3155(4) 0.56111(18) 0.03061(19) 0.0148(5) Uani 1 1 d . . .
H5 H 1.2833 0.6016 -0.0151 0.018 Uiso 1 1 calc R . .
C6 C 1.2482(4) 0.48195(18) 0.01936(19) 0.0150(5) Uani 1 1 d . . .
H6 H 1.1692 0.4690 -0.0339 0.018 Uiso 1 1 calc R . .
C7 C 0.7072(4) 0.1114(2) -0.06347(19) 0.0168(6) Uani 1 1 d . . .
H7 H 0.6934 0.1597 -0.1000 0.020 Uiso 1 1 calc R . .
C8 C 0.7915(4) 0.0435(2) -0.0899(2) 0.0203(6) Uani 1 1 d . . .
H8 H 0.8336 0.0461 -0.1438 0.024 Uiso 1 1 calc R . .
C9 C 0.8132(4) -0.0266(2) -0.0383(2) 0.0206(6) Uani 1 1 d . . .
H9 H 0.8684 -0.0732 -0.0568 0.025 Uiso 1 1 calc R . .
C10 C 0.7528(3) -0.02915(18) 0.0426(2) 0.0169(6) Uani 1 1 d . . .
C11 C 0.6693(3) 0.04164(17) 0.06383(19) 0.0129(5) Uani 1 1 d . . .
C12 C 0.7714(4) -0.09824(18) 0.1034(2) 0.0209(6) Uani 1 1 d . . .
H12 H 0.8279 -0.1463 0.0898 0.025 Uiso 1 1 calc R . .
C13 C 0.7094(4) -0.09584(18) 0.1797(2) 0.0202(6) Uani 1 1 d . . .
H13 H 0.7252 -0.1420 0.2194 0.024 Uiso 1 1 calc R . .
C14 C 0.6205(4) -0.02508(18) 0.2019(2) 0.0165(6) Uani 1 1 d . . .
C15 C 0.6019(3) 0.04331(17) 0.14359(19) 0.0130(5) Uani 1 1 d . . .
C16 C 0.5465(4) -0.01888(19) 0.2779(2) 0.0192(6) Uani 1 1 d . . .
H16 H 0.5551 -0.0633 0.3197 0.023 Uiso 1 1 calc R . .
C17 C 0.4616(4) 0.0519(2) 0.2913(2) 0.0189(6) Uani 1 1 d . . .
H17 H 0.4100 0.0561 0.3418 0.023 Uiso 1 1 calc R . .
C18 C 0.4516(4) 0.11751(19) 0.22999(19) 0.0155(5) Uani 1 1 d . . .
H18 H 0.3943 0.1664 0.2405 0.019 Uiso 1 1 calc R . .


_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 O5 1.9183(19) 3_765 ?
Cu1 O2 1.929(2) 1_455 ?
Cu1 N2 1.997(2) . ?
Cu1 N1 2.010(2) . ?
Cu1 O8 2.316(2) . ?
V1 O7 1.607(2) . ?
V1 O8 1.631(2) . ?
V1 O3 1.853(2) . ?
V1 O4 1.863(2) 2_745 ?
P1 O2 1.506(2) . ?
P1 O1 1.521(2) . ?
P1 O3 1.561(2) . ?
P1 C1 1.799(3) . ?
P2 O5 1.497(2) . ?
P2 O6 1.528(2) . ?
P2 O4 1.557(2) . ?
P2 C4 1.798(3) . ?
O2 Cu1 1.929(2) 1_655 ?
O4 V1 1.863(2) 2_755 ?
O5 Cu1 1.9183(19) 3_765 ?
O6 H6' 0.8400 . ?
N1 C7 1.326(4) . ?
N1 C11 1.354(4) . ?
N2 C18 1.329(4) . ?
N2 C15 1.360(4) . ?
C1 C6 1.395(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.390(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.401(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(4) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.400(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.367(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.412(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.405(4) . ?
C10 C12 1.434(4) . ?
C11 C15 1.427(4) . ?
C12 C13 1.353(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.435(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(4) . ?
C14 C16 1.409(4) . ?
C16 C17 1.377(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.400(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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
O5 Cu1 O2 97.19(9) 3_765 1_455 ?
O5 Cu1 N2 173.27(9) 3_765 . ?
O2 Cu1 N2 88.89(9) 1_455 . ?
O5 Cu1 N1 91.28(9) 3_765 . ?
O2 Cu1 N1 161.39(9) 1_455 . ?
N2 Cu1 N1 82.07(10) . . ?
O5 Cu1 O8 90.42(8) 3_765 . ?
O2 Cu1 O8 101.94(8) 1_455 . ?
N2 Cu1 O8 91.14(8) . . ?
N1 Cu1 O8 94.51(8) . . ?
O7 V1 O8 108.06(11) . . ?
O7 V1 O3 112.23(10) . . ?
O8 V1 O3 109.21(10) . . ?
O7 V1 O4 107.80(10) . 2_745 ?
O8 V1 O4 110.79(9) . 2_745 ?
O3 V1 O4 108.75(9) . 2_745 ?
O2 P1 O1 116.06(12) . . ?
O2 P1 O3 109.16(11) . . ?
O1 P1 O3 108.78(12) . . ?
O2 P1 C1 108.46(12) . . ?
O1 P1 C1 108.89(12) . . ?
O3 P1 C1 104.92(12) . . ?
O5 P2 O6 115.37(12) . . ?
O5 P2 O4 110.91(12) . . ?
O6 P2 O4 107.40(11) . . ?
O5 P2 C4 107.18(12) . . ?
O6 P2 C4 108.73(12) . . ?
O4 P2 C4 106.92(12) . . ?
P1 O2 Cu1 138.04(13) . 1_655 ?
P1 O3 V1 137.72(13) . . ?
P2 O4 V1 137.48(13) . 2_755 ?
P2 O5 Cu1 156.29(14) . 3_765 ?
P2 O6 H6' 109.5 . . ?
V1 O8 Cu1 135.08(11) . . ?
C7 N1 C11 118.8(3) . . ?
C7 N1 Cu1 128.9(2) . . ?
C11 N1 Cu1 112.34(18) . . ?
C18 N2 C15 118.3(2) . . ?
C18 N2 Cu1 128.8(2) . . ?
C15 N2 Cu1 112.87(18) . . ?
C6 C1 C2 118.8(3) . . ?
C6 C1 P1 121.2(2) . . ?
C2 C1 P1 120.0(2) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 P2 120.2(2) . . ?
C3 C4 P2 120.4(2) . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
N1 C7 C8 121.7(3) . . ?
N1 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 116.7(3) . . ?
C11 C10 C12 118.8(3) . . ?
C9 C10 C12 124.5(3) . . ?
N1 C11 C10 123.3(3) . . ?
N1 C11 C15 116.6(2) . . ?
C10 C11 C15 120.0(3) . . ?
C13 C12 C10 120.9(3) . . ?
C13 C12 H12 119.6 . . ?
C10 C12 H12 119.6 . . ?
C12 C13 C14 121.4(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C16 116.5(3) . . ?
C15 C14 C13 118.5(3) . . ?
C16 C14 C13 125.0(3) . . ?
N2 C15 C14 123.7(3) . . ?
N2 C15 C11 116.0(2) . . ?
C14 C15 C11 120.3(3) . . ?
C17 C16 C14 119.7(3) . . ?
C17 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
N2 C18 C17 122.0(3) . . ?
N2 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?

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
O1 P1 O2 Cu1 34.3(2) . . . 1_655 ?
O3 P1 O2 Cu1 157.58(18) . . . 1_655 ?
C1 P1 O2 Cu1 -88.6(2) . . . 1_655 ?
O2 P1 O3 V1 -50.7(2) . . . . ?
O1 P1 O3 V1 76.8(2) . . . . ?
C1 P1 O3 V1 -166.78(19) . . . . ?
O7 V1 O3 P1 -9.1(2) . . . . ?
O8 V1 O3 P1 -128.89(19) . . . . ?
O4 V1 O3 P1 110.1(2) 2_745 . . . ?
O5 P2 O4 V1 -153.12(17) . . . 2_755 ?
O6 P2 O4 V1 -26.2(2) . . . 2_755 ?
C4 P2 O4 V1 90.3(2) . . . 2_755 ?
O6 P2 O5 Cu1 -18.8(4) . . . 3_765 ?
O4 P2 O5 Cu1 103.5(3) . . . 3_765 ?
C4 P2 O5 Cu1 -140.1(3) . . . 3_765 ?
O7 V1 O8 Cu1 -4.25(19) . . . . ?
O3 V1 O8 Cu1 118.10(15) . . . . ?
O4 V1 O8 Cu1 -122.14(14) 2_745 . . . ?
O5 Cu1 O8 V1 -99.05(16) 3_765 . . . ?
O2 Cu1 O8 V1 163.51(15) 1_455 . . . ?
N2 Cu1 O8 V1 74.40(16) . . . . ?
N1 Cu1 O8 V1 -7.73(17) . . . . ?
O5 Cu1 N1 C7 0.7(2) 3_765 . . . ?
O2 Cu1 N1 C7 118.1(3) 1_455 . . . ?
N2 Cu1 N1 C7 179.7(3) . . . . ?
O8 Cu1 N1 C7 -89.8(2) . . . . ?
O5 Cu1 N1 C11 178.97(19) 3_765 . . . ?
O2 Cu1 N1 C11 -63.7(4) 1_455 . . . ?
N2 Cu1 N1 C11 -2.07(18) . . . . ?
O8 Cu1 N1 C11 88.45(19) . . . . ?
O5 Cu1 N2 C18 -169.7(7) 3_765 . . . ?
O2 Cu1 N2 C18 -14.9(2) 1_455 . . . ?
N1 Cu1 N2 C18 -178.6(3) . . . . ?
O8 Cu1 N2 C18 87.0(2) . . . . ?
O5 Cu1 N2 C15 11.4(9) 3_765 . . . ?
O2 Cu1 N2 C15 166.11(19) 1_455 . . . ?
N1 Cu1 N2 C15 2.42(19) . . . . ?
O8 Cu1 N2 C15 -91.97(19) . . . . ?
O2 P1 C1 C6 140.7(2) . . . . ?
O1 P1 C1 C6 13.6(3) . . . . ?
O3 P1 C1 C6 -102.8(2) . . . . ?
O2 P1 C1 C2 -38.2(3) . . . . ?
O1 P1 C1 C2 -165.3(2) . . . . ?
O3 P1 C1 C2 78.3(2) . . . . ?
C6 C1 C2 C3 0.1(4) . . . . ?
P1 C1 C2 C3 179.0(2) . . . . ?
C1 C2 C3 C4 -1.1(4) . . . . ?
C2 C3 C4 C5 1.2(4) . . . . ?
C2 C3 C4 P2 -176.1(2) . . . . ?
O5 P2 C4 C5 -2.7(3) . . . . ?
O6 P2 C4 C5 -128.1(2) . . . . ?
O4 P2 C4 C5 116.3(2) . . . . ?
O5 P2 C4 C3 174.5(2) . . . . ?
O6 P2 C4 C3 49.2(2) . . . . ?
O4 P2 C4 C3 -66.5(2) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
P2 C4 C5 C6 177.0(2) . . . . ?
C4 C5 C6 C1 -0.8(4) . . . . ?
C2 C1 C6 C5 0.9(4) . . . . ?
P1 C1 C6 C5 -178.1(2) . . . . ?
C11 N1 C7 C8 1.2(4) . . . . ?
Cu1 N1 C7 C8 179.4(2) . . . . ?
N1 C7 C8 C9 -0.1(5) . . . . ?
C7 C8 C9 C10 -1.3(4) . . . . ?
C8 C9 C10 C11 1.4(4) . . . . ?
C8 C9 C10 C12 -178.5(3) . . . . ?
C7 N1 C11 C10 -1.0(4) . . . . ?
Cu1 N1 C11 C10 -179.4(2) . . . . ?
C7 N1 C11 C15 179.8(2) . . . . ?
Cu1 N1 C11 C15 1.4(3) . . . . ?
C9 C10 C11 N1 -0.3(4) . . . . ?
C12 C10 C11 N1 179.6(3) . . . . ?
C9 C10 C11 C15 178.8(3) . . . . ?
C12 C10 C11 C15 -1.3(4) . . . . ?
C11 C10 C12 C13 0.2(4) . . . . ?
C9 C10 C12 C13 -179.9(3) . . . . ?
C10 C12 C13 C14 1.2(4) . . . . ?
C12 C13 C14 C15 -1.5(4) . . . . ?
C12 C13 C14 C16 177.3(3) . . . . ?
C18 N2 C15 C14 -0.9(4) . . . . ?
Cu1 N2 C15 C14 178.2(2) . . . . ?
C18 N2 C15 C11 178.6(2) . . . . ?
Cu1 N2 C15 C11 -2.4(3) . . . . ?
C16 C14 C15 N2 0.9(4) . . . . ?
C13 C14 C15 N2 179.9(3) . . . . ?
C16 C14 C15 C11 -178.5(3) . . . . ?
C13 C14 C15 C11 0.4(4) . . . . ?
N1 C11 C15 N2 0.6(4) . . . . ?
C10 C11 C15 N2 -178.5(2) . . . . ?
N1 C11 C15 C14 -179.9(2) . . . . ?
C10 C11 C15 C14 0.9(4) . . . . ?
C15 C14 C16 C17 0.0(4) . . . . ?
C13 C14 C16 C17 -178.8(3) . . . . ?
C14 C16 C17 C18 -1.0(4) . . . . ?
C15 N2 C18 C17 -0.1(4) . . . . ?
Cu1 N2 C18 C17 -179.0(2) . . . . ?
C16 C17 C18 N2 1.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.103

#[Cu(phen)VVO2(HO3PC6H4PO3)] 7b
data_[Cu(phen)VVO2(HO3PC6H4PO3)]7b
_database_code_depnum_ccdc_archive 'CCDC 734628'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_sum            'C18 H13 Cu N2 O8 P2 V'
_chemical_formula_weight         561.72

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'
V V 0.3005 0.5294 '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   C2/c
_symmetry_space_group_name_Hall  -C2yc

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                   11.2896(5)
_cell_length_b                   16.8485(8)
_cell_length_c                   20.5594(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.9090(10)
_cell_angle_gamma                90.00
_cell_volume                     3901.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6443
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            black-green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7164
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            20386
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0289
_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         1.99
_diffrn_reflns_theta_max         28.31
_reflns_number_total             4868
_reflns_number_gt                4816
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0204P)²+62.1992P] where P=(Fo²+2Fc²)/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         4868
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.1449
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_restrained_S_all      1.381
_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 0.69675(5) 0.30664(3) 0.64474(3) 0.00921(14) Uani 1 1 d . . .
V1 V 0.62581(7) 0.28977(5) 0.49007(4) 0.00771(17) Uani 1 1 d . . .
P1 P 0.98688(11) 0.29883(7) 0.64739(6) 0.0081(2) Uani 1 1 d . . .
P2 P 1.15725(11) 0.64992(7) 0.58331(6) 0.0093(2) Uani 1 1 d . . .
O1 O 0.9744(3) 0.2453(2) 0.58867(16) 0.0109(7) Uani 1 1 d . . .
O2 O 0.8819(3) 0.3025(2) 0.68892(16) 0.0112(7) Uani 1 1 d . . .
O3 O 1.0997(3) 0.2685(2) 0.68914(17) 0.0118(7) Uani 1 1 d . . .
O4 O 1.0771(3) 0.6874(2) 0.52777(16) 0.0114(7) Uani 1 1 d . . .
O5 O 1.2861(3) 0.6377(2) 0.56324(16) 0.0112(7) Uani 1 1 d . . .
O6 O 1.1525(3) 0.6963(2) 0.64711(16) 0.0120(7) Uani 1 1 d . . .
O7 O 0.7356(3) 0.2951(2) 0.55315(15) 0.0095(6) Uani 1 1 d . . .
O8 O 0.5270(3) 0.3494(2) 0.51387(17) 0.0136(7) Uani 1 1 d . . .
N1 N 0.6526(4) 0.3252(3) 0.7369(2) 0.0154(9) Uani 1 1 d . . .
N2 N 0.6866(4) 0.4251(3) 0.6401(2) 0.0138(8) Uani 1 1 d . . .
C1 C 1.0222(4) 0.3983(3) 0.6236(2) 0.0092(8) Uani 1 1 d . . .
C2 C 1.0875(5) 0.4131(3) 0.5703(3) 0.0168(10) Uani 1 1 d . . .
H2 H 1.1067 0.3707 0.5424 0.020 Uiso 1 1 calc R . .
C3 C 1.1253(5) 0.4899(3) 0.5574(3) 0.0203(11) Uani 1 1 d . . .
H3 H 1.1692 0.4993 0.5203 0.024 Uiso 1 1 calc R . .
C4 C 1.1001(4) 0.5526(3) 0.5976(2) 0.0126(9) Uani 1 1 d . . .
C5 C 1.0297(5) 0.5387(3) 0.6496(3) 0.0182(11) Uani 1 1 d . . .
H5 H 1.0084 0.5815 0.6765 0.022 Uiso 1 1 calc R . .
C6 C 0.9906(5) 0.4624(3) 0.6620(3) 0.0189(11) Uani 1 1 d . . .
H6 H 0.9416 0.4536 0.6971 0.023 Uiso 1 1 calc R . .
C7 C 0.6340(5) 0.2732(4) 0.7834(3) 0.0204(11) Uani 1 1 d . . .
H7 H 0.6327 0.2182 0.7733 0.024 Uiso 1 1 calc R . .
C8 C 0.6162(5) 0.2973(5) 0.8472(3) 0.0287(14) Uani 1 1 d . . .
H8 H 0.6043 0.2588 0.8799 0.034 Uiso 1 1 calc R . .
C9 C 0.6159(5) 0.3764(5) 0.8624(3) 0.0304(15) Uani 1 1 d . . .
H9 H 0.6023 0.3927 0.9055 0.036 Uiso 1 1 calc R . .
C10 C 0.6355(5) 0.4332(4) 0.8146(3) 0.0236(13) Uani 1 1 d . . .
C11 C 0.6533(4) 0.4038(3) 0.7516(3) 0.0166(10) Uani 1 1 d . . .
C12 C 0.6331(6) 0.5176(4) 0.8234(3) 0.0327(16) Uani 1 1 d . . .
H12 H 0.6200 0.5381 0.8653 0.039 Uiso 1 1 calc R . .
C13 C 0.6486(5) 0.5689(4) 0.7742(3) 0.0313(15) Uani 1 1 d . . .
H13 H 0.6471 0.6244 0.7823 0.038 Uiso 1 1 calc R . .
C14 C 0.6675(5) 0.5407(3) 0.7095(3) 0.0240(12) Uani 1 1 d . . .
C15 C 0.6712(5) 0.4576(3) 0.6995(3) 0.0174(11) Uani 1 1 d . . .
C16 C 0.6765(6) 0.5890(4) 0.6549(4) 0.0318(15) Uani 1 1 d . . .
H16 H 0.6728 0.6451 0.6589 0.038 Uiso 1 1 calc R . .
C17 C 0.6909(6) 0.5548(4) 0.5952(3) 0.0282(13) Uani 1 1 d . . .
H17 H 0.6968 0.5873 0.5578 0.034 Uiso 1 1 calc R . .
C18 C 0.6969(5) 0.4721(3) 0.5895(3) 0.0200(11) Uani 1 1 d . . .
H18 H 0.7086 0.4493 0.5482 0.024 Uiso 1 1 calc R . .
H3' H 1.104(6) 0.279(4) 0.721(4) 0.020(19) Uiso 1 1 d . . .


_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 O6 1.927(3) 3_445 ?
Cu1 O7 1.972(3) . ?
Cu1 N2 2.001(4) . ?
Cu1 N1 2.015(4) . ?
Cu1 O2 2.222(3) . ?
V1 O8 1.603(3) . ?
V1 O7 1.734(3) . ?
V1 O5 1.958(3) 5_766 ?
V1 O4 1.985(3) 3_445 ?
V1 O1 2.000(3) 7_656 ?
V1 O7 2.340(3) 7_656 ?
V1 V1 3.1094(16) 7_656 ?
P1 O1 1.505(3) . ?
P1 O2 1.509(4) . ?
P1 O3 1.572(4) . ?
P1 C1 1.798(5) . ?
P2 O6 1.531(4) . ?
P2 O4 1.543(4) . ?
P2 O5 1.553(4) . ?
P2 C4 1.793(5) . ?
O1 V1 2.000(3) 7_656 ?
O3 H3' 0.69(7) . ?
O4 V1 1.985(3) 3 ?
O5 V1 1.958(3) 5_766 ?
O6 Cu1 1.927(3) 3 ?
O7 V1 2.340(3) 7_656 ?
N1 C7 1.325(7) . ?
N1 C11 1.360(7) . ?
N2 C18 1.320(7) . ?
N2 C15 1.359(6) . ?
C1 C2 1.385(7) . ?
C1 C6 1.399(7) . ?
C2 C3 1.393(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(7) . ?
C5 C6 1.389(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.401(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.400(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.414(7) . ?
C10 C12 1.434(9) . ?
C11 C15 1.427(8) . ?
C12 C13 1.352(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.440(8) . ?
C13 H13 0.9500 . ?
C14 C16 1.397(10) . ?
C14 C15 1.417(8) . ?
C16 C17 1.375(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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
O6 Cu1 O7 90.24(14) 3_445 . ?
O6 Cu1 N2 161.75(17) 3_445 . ?
O7 Cu1 N2 93.93(16) . . ?
O6 Cu1 N1 92.56(17) 3_445 . ?
O7 Cu1 N1 176.37(17) . . ?
N2 Cu1 N1 82.70(19) . . ?
O6 Cu1 O2 101.39(14) 3_445 . ?
O7 Cu1 O2 97.07(13) . . ?
N2 Cu1 O2 95.73(15) . . ?
N1 Cu1 O2 84.65(15) . . ?
O8 V1 O7 102.47(17) . . ?
O8 V1 O5 99.81(17) . 5_766 ?
O7 V1 O5 91.25(15) . 5_766 ?
O8 V1 O4 102.02(17) . 3_445 ?
O7 V1 O4 87.51(15) . 3_445 ?
O5 V1 O4 157.89(15) 5_766 3_445 ?
O8 V1 O1 93.73(16) . 7_656 ?
O7 V1 O1 163.10(16) . 7_656 ?
O5 V1 O1 90.71(14) 5_766 7_656 ?
O4 V1 O1 84.39(14) 3_445 7_656 ?
O8 V1 O7 175.47(15) . 7_656 ?
O7 V1 O7 81.58(14) . 7_656 ?
O5 V1 O7 77.93(13) 5_766 7_656 ?
O4 V1 O7 80.05(13) 3_445 7_656 ?
O1 V1 O7 82.42(13) 7_656 7_656 ?
O8 V1 V1 150.52(13) . 7_656 ?
O7 V1 V1 48.11(11) . 7_656 ?
O5 V1 V1 81.65(11) 5_766 7_656 ?
O4 V1 V1 81.12(11) 3_445 7_656 ?
O1 V1 V1 115.74(11) 7_656 7_656 ?
O7 V1 V1 33.48(8) 7_656 7_656 ?
O1 P1 O2 116.4(2) . . ?
O1 P1 O3 105.7(2) . . ?
O2 P1 O3 110.0(2) . . ?
O1 P1 C1 110.5(2) . . ?
O2 P1 C1 108.2(2) . . ?
O3 P1 C1 105.4(2) . . ?
O6 P2 O4 111.9(2) . . ?
O6 P2 O5 112.5(2) . . ?
O4 P2 O5 111.77(19) . . ?
O6 P2 C4 107.0(2) . . ?
O4 P2 C4 107.2(2) . . ?
O5 P2 C4 106.0(2) . . ?
P1 O1 V1 147.4(2) . 7_656 ?
P1 O2 Cu1 121.55(19) . . ?
P1 O3 H3' 116(6) . . ?
P2 O4 V1 118.7(2) . 3 ?
P2 O5 V1 125.9(2) . 5_766 ?
P2 O6 Cu1 116.5(2) . 3 ?
V1 O7 Cu1 121.69(18) . . ?
V1 O7 V1 98.42(14) . 7_656 ?
Cu1 O7 V1 128.37(16) . 7_656 ?
C7 N1 C11 118.8(5) . . ?
C7 N1 Cu1 129.7(4) . . ?
C11 N1 Cu1 111.2(3) . . ?
C18 N2 C15 119.3(5) . . ?
C18 N2 Cu1 128.9(4) . . ?
C15 N2 Cu1 111.7(4) . . ?
C2 C1 C6 118.6(4) . . ?
C2 C1 P1 121.5(4) . . ?
C6 C1 P1 119.7(4) . . ?
C1 C2 C3 120.3(5) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 121.2(5) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 118.7(5) . . ?
C3 C4 P2 120.7(4) . . ?
C5 C4 P2 120.6(4) . . ?
C6 C5 C4 120.1(5) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
N1 C7 C8 121.7(6) . . ?
N1 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 119.9(6) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 116.3(6) . . ?
C9 C10 C12 125.8(6) . . ?
C11 C10 C12 117.9(6) . . ?
N1 C11 C10 123.1(5) . . ?
N1 C11 C15 116.8(4) . . ?
C10 C11 C15 120.1(5) . . ?
C13 C12 C10 122.4(6) . . ?
C13 C12 H12 118.8 . . ?
C10 C12 H12 118.8 . . ?
C12 C13 C14 121.0(6) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C16 C14 C15 117.0(5) . . ?
C16 C14 C13 125.0(6) . . ?
C15 C14 C13 117.9(6) . . ?
N2 C15 C14 122.4(5) . . ?
N2 C15 C11 116.8(5) . . ?
C14 C15 C11 120.7(5) . . ?
C17 C16 C14 119.6(5) . . ?
C17 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
C16 C17 C18 120.1(6) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N2 C18 C17 121.6(6) . . ?
N2 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 V1 47.2(5) . . . 7_656 ?
O3 P1 O1 V1 169.7(4) . . . 7_656 ?
C1 P1 O1 V1 -76.7(4) . . . 7_656 ?
O1 P1 O2 Cu1 -41.1(3) . . . . ?
O3 P1 O2 Cu1 -161.3(2) . . . . ?
C1 P1 O2 Cu1 84.0(3) . . . . ?
O6 Cu1 O2 P1 95.9(2) 3_445 . . . ?
O7 Cu1 O2 P1 4.2(2) . . . . ?
N2 Cu1 O2 P1 -90.4(2) . . . . ?
N1 Cu1 O2 P1 -172.5(3) . . . . ?
O6 P2 O4 V1 71.3(3) . . . 3 ?
O5 P2 O4 V1 -56.0(3) . . . 3 ?
C4 P2 O4 V1 -171.7(2) . . . 3 ?
O6 P2 O5 V1 -88.8(3) . . . 5_766 ?
O4 P2 O5 V1 38.1(3) . . . 5_766 ?
C4 P2 O5 V1 154.5(2) . . . 5_766 ?
O4 P2 O6 Cu1 -58.0(3) . . . 3 ?
O5 P2 O6 Cu1 68.8(3) . . . 3 ?
C4 P2 O6 Cu1 -175.1(2) . . . 3 ?
O8 V1 O7 Cu1 36.1(2) . . . . ?
O5 V1 O7 Cu1 136.4(2) 5_766 . . . ?
O4 V1 O7 Cu1 -65.7(2) 3_445 . . . ?
O1 V1 O7 Cu1 -127.0(5) 7_656 . . . ?
O7 V1 O7 Cu1 -146.0(3) 7_656 . . . ?
V1 V1 O7 Cu1 -146.0(3) 7_656 . . . ?
O8 V1 O7 V1 -177.93(16) . . . 7_656 ?
O5 V1 O7 V1 -77.60(14) 5_766 . . 7_656 ?
O4 V1 O7 V1 80.30(14) 3_445 . . 7_656 ?
O1 V1 O7 V1 19.0(6) 7_656 . . 7_656 ?
O7 V1 O7 V1 0.0 7_656 . . 7_656 ?
O6 Cu1 O7 V1 75.9(2) 3_445 . . . ?
N2 Cu1 O7 V1 -86.3(2) . . . . ?
N1 Cu1 O7 V1 -64(3) . . . . ?
O2 Cu1 O7 V1 177.4(2) . . . . ?
O6 Cu1 O7 V1 -59.2(2) 3_445 . . 7_656 ?
N2 Cu1 O7 V1 138.6(2) . . . 7_656 ?
N1 Cu1 O7 V1 161(2) . . . 7_656 ?
O2 Cu1 O7 V1 42.4(2) . . . 7_656 ?
O6 Cu1 N1 C7 16.1(5) 3_445 . . . ?
O7 Cu1 N1 C7 156(2) . . . . ?
N2 Cu1 N1 C7 178.4(5) . . . . ?
O2 Cu1 N1 C7 -85.1(5) . . . . ?
O6 Cu1 N1 C11 -169.9(3) 3_445 . . . ?
O7 Cu1 N1 C11 -30(3) . . . . ?
N2 Cu1 N1 C11 -7.6(3) . . . . ?
O2 Cu1 N1 C11 88.9(3) . . . . ?
O6 Cu1 N2 C18 -99.3(7) 3_445 . . . ?
O7 Cu1 N2 C18 3.5(5) . . . . ?
N1 Cu1 N2 C18 -175.2(5) . . . . ?
O2 Cu1 N2 C18 101.0(5) . . . . ?
O6 Cu1 N2 C15 83.2(6) 3_445 . . . ?
O7 Cu1 N2 C15 -174.0(3) . . . . ?
N1 Cu1 N2 C15 7.4(3) . . . . ?
O2 Cu1 N2 C15 -76.5(4) . . . . ?
O1 P1 C1 C2 -31.0(5) . . . . ?
O2 P1 C1 C2 -159.5(4) . . . . ?
O3 P1 C1 C2 82.8(4) . . . . ?
O1 P1 C1 C6 153.5(4) . . . . ?
O2 P1 C1 C6 25.0(5) . . . . ?
O3 P1 C1 C6 -92.7(4) . . . . ?
C6 C1 C2 C3 3.0(8) . . . . ?
P1 C1 C2 C3 -172.6(4) . . . . ?
C1 C2 C3 C4 0.8(9) . . . . ?
C2 C3 C4 C5 -3.8(8) . . . . ?
C2 C3 C4 P2 176.0(4) . . . . ?
O6 P2 C4 C3 -160.1(4) . . . . ?
O4 P2 C4 C3 79.8(5) . . . . ?
O5 P2 C4 C3 -39.7(5) . . . . ?
O6 P2 C4 C5 19.7(5) . . . . ?
O4 P2 C4 C5 -100.4(5) . . . . ?
O5 P2 C4 C5 140.1(4) . . . . ?
C3 C4 C5 C6 2.9(8) . . . . ?
P2 C4 C5 C6 -176.9(4) . . . . ?
C4 C5 C6 C1 0.9(9) . . . . ?
C2 C1 C6 C5 -3.9(8) . . . . ?
P1 C1 C6 C5 171.8(4) . . . . ?
C11 N1 C7 C8 -0.5(8) . . . . ?
Cu1 N1 C7 C8 173.1(4) . . . . ?
N1 C7 C8 C9 1.0(9) . . . . ?
C7 C8 C9 C10 -1.1(9) . . . . ?
C8 C9 C10 C11 0.8(8) . . . . ?
C8 C9 C10 C12 177.5(6) . . . . ?
C7 N1 C11 C10 0.2(8) . . . . ?
Cu1 N1 C11 C10 -174.5(4) . . . . ?
C7 N1 C11 C15 -178.7(5) . . . . ?
Cu1 N1 C11 C15 6.6(6) . . . . ?
C9 C10 C11 N1 -0.4(8) . . . . ?
C12 C10 C11 N1 -177.3(5) . . . . ?
C9 C10 C11 C15 178.5(5) . . . . ?
C12 C10 C11 C15 1.6(8) . . . . ?
C9 C10 C12 C13 -177.5(6) . . . . ?
C11 C10 C12 C13 -0.9(9) . . . . ?
C10 C12 C13 C14 0.6(10) . . . . ?
C12 C13 C14 C16 175.5(6) . . . . ?
C12 C13 C14 C15 -1.1(9) . . . . ?
C18 N2 C15 C14 -1.0(8) . . . . ?
Cu1 N2 C15 C14 176.7(4) . . . . ?
C18 N2 C15 C11 176.3(5) . . . . ?
Cu1 N2 C15 C11 -6.0(6) . . . . ?
C16 C14 C15 N2 2.1(8) . . . . ?
C13 C14 C15 N2 179.0(5) . . . . ?
C16 C14 C15 C11 -175.1(5) . . . . ?
C13 C14 C15 C11 1.8(8) . . . . ?
N1 C11 C15 N2 -0.4(7) . . . . ?
C10 C11 C15 N2 -179.4(5) . . . . ?
N1 C11 C15 C14 176.9(5) . . . . ?
C10 C11 C15 C14 -2.1(8) . . . . ?
C15 C14 C16 C17 -1.4(9) . . . . ?
C13 C14 C16 C17 -178.0(6) . . . . ?
C14 C16 C17 C18 -0.3(10) . . . . ?
C15 N2 C18 C17 -0.7(8) . . . . ?
Cu1 N2 C18 C17 -178.0(4) . . . . ?
C16 C17 C18 N2 1.4(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.147

data_8
_database_code_depnum_ccdc_archive 'CCDC 734629'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H14 Cu N2 O14 P2 V2'
_chemical_formula_sum            'C18 H14 Cu N2 O14 P2 V2'
_chemical_formula_weight         709.67

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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   9.6032(9)
_cell_length_b                   6.1831(6)
_cell_length_c                   19.7804(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.224(2)
_cell_angle_gamma                90.00
_cell_volume                     1167.59(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5926
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      28.31

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             706
_exptl_absorpt_coefficient_mu    1.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5991
_exptl_absorpt_correction_T_max  0.8627
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            11142
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         28.07
_reflns_number_total             2835
_reflns_number_gt                2660
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0438P)²+1.2728P] where P=(Fo²+2Fc²)/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         2835
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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 1.0000 0.0000 0.01510(10) Uani 1 2 d S . .
V1 V 0.18634(3) 0.56065(5) 0.243127(16) 0.01306(10) Uani 1 1 d . . .
P1 P 0.24472(5) 0.85317(8) 0.11210(2) 0.01258(12) Uani 1 1 d . . .
O1 O 0.36600(15) 0.7771(2) 0.07367(7) 0.0172(3) Uani 1 1 d . . .
H1' H 0.4095 0.6770 0.0955 0.026 Uiso 1 1 calc R . .
O2 O 0.18558(15) 0.6649(2) 0.15014(7) 0.0155(3) Uani 1 1 d . . .
O3 O 0.28450(16) 1.0481(2) 0.15754(7) 0.0160(3) Uani 1 1 d . . .
O4 O 0.03660(17) 0.4463(3) 0.23408(8) 0.0244(3) Uani 1 1 d . . .
O5 O 0.31220(16) 0.3699(2) 0.23740(7) 0.0177(3) Uani 1 1 d . . .
O6 O 0.45175(15) 1.2765(2) 0.04065(7) 0.0168(3) Uani 1 1 d . . .
O7 O 0.53046(16) 1.5038(2) 0.12438(8) 0.0198(3) Uani 1 1 d . . .
N1 N 0.65045(18) 0.9948(3) 0.07545(9) 0.0144(3) Uani 1 1 d . . .
C1 C 0.0526(2) 1.1486(3) 0.04993(10) 0.0157(4) Uani 1 1 d . . .
C2 C 0.1096(2) 0.9401(3) 0.04852(10) 0.0133(4) Uani 1 1 d . . .
C3 C 0.0566(2) 0.7936(3) -0.00164(10) 0.0158(4) Uani 1 1 d . . .
C4 C 0.7462(2) 0.8408(3) 0.09092(11) 0.0172(4) Uani 1 1 d . . .
C5 C 0.8451(2) 0.8577(4) 0.14735(12) 0.0211(4) Uani 1 1 d . . .
C6 C 0.8460(2) 1.0418(4) 0.18758(12) 0.0227(4) Uani 1 1 d . . .
C7 C 0.7475(2) 1.2027(4) 0.17118(11) 0.0204(4) Uani 1 1 d . . .
C8 C 0.6502(2) 1.1721(3) 0.11518(10) 0.0158(4) Uani 1 1 d . . .
C9 C 0.5346(2) 1.3283(3) 0.09158(10) 0.0158(4) Uani 1 1 d . . .
H1 H 0.091(3) 1.253(4) 0.0831(13) 0.014(6) Uiso 1 1 d . . .
H3 H 0.091(3) 0.662(5) -0.0016(13) 0.017(6) Uiso 1 1 d . . .
H4 H 0.740(3) 0.725(4) 0.0631(13) 0.019(6) Uiso 1 1 d . . .
H5 H 0.907(3) 0.750(5) 0.1582(14) 0.022(7) Uiso 1 1 d . . .
H6 H 0.912(3) 1.057(5) 0.2285(15) 0.028(7) Uiso 1 1 d . . .
H7 H 0.750(3) 1.323(5) 0.1947(14) 0.026(7) Uiso 1 1 d . . .


_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 N1 1.9617(17) 3_675 ?
Cu1 N1 1.9618(17) . ?
Cu1 O6 1.9661(14) 3_675 ?
Cu1 O6 1.9661(14) . ?
V1 O4 1.5950(16) . ?
V1 O5 1.7011(15) . ?
V1 O2 1.9482(14) . ?
V1 O5 1.9505(15) 2 ?
V1 O3 1.9560(14) 2_545 ?
P1 O3 1.5270(15) . ?
P1 O2 1.5287(15) . ?
P1 O1 1.5320(15) . ?
P1 C2 1.789(2) . ?
O1 H1' 0.8400 . ?
O3 V1 1.9561(14) 2 ?
O5 V1 1.9506(15) 2_545 ?
O6 C9 1.256(2) . ?
O7 C9 1.267(3) . ?
N1 C4 1.336(3) . ?
N1 C8 1.349(3) . ?
C1 C3 1.387(3) 3_575 ?
C1 C2 1.402(3) . ?
C1 H1 0.96(3) . ?
C2 C3 1.398(3) . ?
C3 C1 1.387(3) 3_575 ?
C3 H3 0.88(3) . ?
C4 C5 1.389(3) . ?
C4 H4 0.90(3) . ?
C5 C6 1.388(3) . ?
C5 H5 0.91(3) . ?
C6 C7 1.387(3) . ?
C6 H6 0.98(3) . ?
C7 C8 1.383(3) . ?
C7 H7 0.88(3) . ?
C8 C9 1.507(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
N1 Cu1 N1 180.0 3_675 . ?
N1 Cu1 O6 83.68(6) 3_675 3_675 ?
N1 Cu1 O6 96.32(6) . 3_675 ?
N1 Cu1 O6 96.32(6) 3_675 . ?
N1 Cu1 O6 83.68(6) . . ?
O6 Cu1 O6 180.0 3_675 . ?
O4 V1 O5 108.89(9) . . ?
O4 V1 O2 97.45(7) . . ?
O5 V1 O2 95.53(7) . . ?
O4 V1 O5 116.35(8) . 2 ?
O5 V1 O5 134.65(4) . 2 ?
O2 V1 O5 82.03(6) . 2 ?
O4 V1 O3 97.13(7) . 2_545 ?
O5 V1 O3 90.80(7) . 2_545 ?
O2 V1 O3 161.26(6) . 2_545 ?
O5 V1 O3 80.99(6) 2 2_545 ?
O3 P1 O2 113.20(8) . . ?
O3 P1 O1 112.28(9) . . ?
O2 P1 O1 110.70(8) . . ?
O3 P1 C2 107.02(9) . . ?
O2 P1 C2 107.16(9) . . ?
O1 P1 C2 106.02(9) . . ?
P1 O1 H1' 109.5 . . ?
P1 O2 V1 138.86(9) . . ?
P1 O3 V1 128.47(9) . 2 ?
V1 O5 V1 131.03(9) . 2_545 ?
C9 O6 Cu1 113.12(13) . . ?
C4 N1 C8 119.37(18) . . ?
C4 N1 Cu1 128.15(15) . . ?
C8 N1 Cu1 112.47(13) . . ?
C3 C1 C2 119.40(18) 3_575 . ?
C3 C1 H1 120.1(15) 3_575 . ?
C2 C1 H1 120.5(15) . . ?
C3 C2 C1 119.83(18) . . ?
C3 C2 P1 118.97(15) . . ?
C1 C2 P1 121.15(15) . . ?
C1 C3 C2 120.76(19) 3_575 . ?
C1 C3 H3 119.8(17) 3_575 . ?
C2 C3 H3 119.4(17) . . ?
N1 C4 C5 121.6(2) . . ?
N1 C4 H4 115.1(17) . . ?
C5 C4 H4 123.3(17) . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 H5 120.4(17) . . ?
C4 C5 H5 120.7(17) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 119.2(18) . . ?
C5 C6 H6 121.2(18) . . ?
C8 C7 C6 118.3(2) . . ?
C8 C7 H7 121.3(19) . . ?
C6 C7 H7 120.4(19) . . ?
N1 C8 C7 122.30(19) . . ?
N1 C8 C9 112.85(17) . . ?
C7 C8 C9 124.84(19) . . ?
O6 C9 O7 125.20(19) . . ?
O6 C9 C8 117.81(18) . . ?
O7 C9 C8 116.97(18) . . ?

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
O3 P1 O2 V1 -20.51(17) . . . . ?
O1 P1 O2 V1 106.56(14) . . . . ?
C2 P1 O2 V1 -138.26(13) . . . . ?
O4 V1 O2 P1 149.70(15) . . . . ?
O5 V1 O2 P1 -100.38(14) . . . . ?
O5 V1 O2 P1 34.00(14) 2 . . . ?
O3 V1 O2 P1 8.8(3) 2_545 . . . ?
O2 P1 O3 V1 16.81(15) . . . 2 ?
O1 P1 O3 V1 -109.43(12) . . . 2 ?
C2 P1 O3 V1 134.64(11) . . . 2 ?
O4 V1 O5 V1 -26.68(13) . . . 2_545 ?
O2 V1 O5 V1 -126.51(10) . . . 2_545 ?
O5 V1 O5 V1 149.23(12) 2 . . 2_545 ?
O3 V1 O5 V1 71.14(11) 2_545 . . 2_545 ?
N1 Cu1 O6 C9 -177.80(14) 3_675 . . . ?
N1 Cu1 O6 C9 2.20(14) . . . . ?
O6 Cu1 O6 C9 -13(8) 3_675 . . . ?
N1 Cu1 N1 C4 105(2) 3_675 . . . ?
O6 Cu1 N1 C4 -2.05(18) 3_675 . . . ?
O6 Cu1 N1 C4 177.95(18) . . . . ?
N1 Cu1 N1 C8 -74(2) 3_675 . . . ?
O6 Cu1 N1 C8 178.87(13) 3_675 . . . ?
O6 Cu1 N1 C8 -1.13(13) . . . . ?
C3 C1 C2 C3 0.5(3) 3_575 . . . ?
C3 C1 C2 P1 -176.91(15) 3_575 . . . ?
O3 P1 C2 C3 177.91(15) . . . . ?
O2 P1 C2 C3 -60.38(18) . . . . ?
O1 P1 C2 C3 57.88(18) . . . . ?
O3 P1 C2 C1 -4.70(19) . . . . ?
O2 P1 C2 C1 117.01(17) . . . . ?
O1 P1 C2 C1 -124.73(17) . . . . ?
C1 C2 C3 C1 -0.5(3) . . . 3_575 ?
P1 C2 C3 C1 176.97(16) . . . 3_575 ?
C8 N1 C4 C5 0.5(3) . . . . ?
Cu1 N1 C4 C5 -178.48(15) . . . . ?
N1 C4 C5 C6 -1.5(3) . . . . ?
C4 C5 C6 C7 0.9(3) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C4 N1 C8 C7 1.1(3) . . . . ?
Cu1 N1 C8 C7 -179.72(16) . . . . ?
C4 N1 C8 C9 -179.11(17) . . . . ?
Cu1 N1 C8 C9 0.1(2) . . . . ?
C6 C7 C8 N1 -1.7(3) . . . . ?
C6 C7 C8 C9 178.54(19) . . . . ?
Cu1 O6 C9 O7 176.05(16) . . . . ?
Cu1 O6 C9 C8 -2.8(2) . . . . ?
N1 C8 C9 O6 1.9(3) . . . . ?
C7 C8 C9 O6 -178.36(19) . . . . ?
N1 C8 C9 O7 -177.06(17) . . . . ?
C7 C8 C9 O7 2.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.095

data_9
_database_code_depnum_ccdc_archive 'CCDC 734630'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 CU2 F2 N4 O10 P2 V2'
_chemical_formula_sum            'C26 H20 Cu2 F2 N4 O10 P2 V2'
_chemical_formula_weight         877.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   10.4020(9)
_cell_length_b                   8.8148(7)
_cell_length_c                   15.9060(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.565(2)
_cell_angle_gamma                90.00
_cell_volume                     1433.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    7157
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            dark
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5469
_exptl_absorpt_correction_T_max  0.8382
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            13832
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         28.08
_reflns_number_total             3480
_reflns_number_gt                3403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0208P)²+4.5116P] where P=(Fo²+2Fc²)/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         3480
_refine_ls_number_parameters     257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_restrained_S_all      1.233
_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 0.44193(3) 0.73691(4) 0.15955(2) 0.00925(9) Uani 1 1 d . . .
V1 V 0.34850(4) 1.04210(5) 0.27848(3) 0.01002(11) Uani 1 1 d . . .
P1 P 0.40180(7) 0.71467(8) 0.33853(4) 0.00790(14) Uani 1 1 d . . .
F1 F 0.26878(18) 0.5886(2) 0.15012(11) 0.0203(4) Uani 1 1 d . . .
O1 O 0.25893(18) 0.6750(2) 0.30460(12) 0.0117(4) Uani 1 1 d . . .
O2 O 0.49246(19) 0.6745(2) 0.27628(12) 0.0116(4) Uani 1 1 d . . .
O3 O 0.41009(19) 0.8814(2) 0.36650(12) 0.0101(4) Uani 1 1 d . . .
O4 O 0.4779(2) 1.1449(2) 0.29652(13) 0.0152(4) Uani 1 1 d . . .
O5 O 0.3610(2) 0.9164(2) 0.19819(12) 0.0128(4) Uani 1 1 d . . .
N1 N 0.4149(2) 0.8037(3) 0.03894(15) 0.0110(4) Uani 1 1 d . . .
N2 N 0.5833(2) 0.6161(3) 0.12225(15) 0.0113(5) Uani 1 1 d . . .
C1 C 0.4580(2) 0.5981(3) 0.43069(17) 0.0091(5) Uani 1 1 d . . .
C2 C 0.4777(3) 0.4436(3) 0.41705(17) 0.0106(5) Uani 1 1 d . . .
C3 C 0.4808(3) 0.6538(3) 0.51473(17) 0.0111(5) Uani 1 1 d . . .
C4 C 0.3214(3) 0.8988(3) 0.00179(19) 0.0142(6) Uani 1 1 d . . .
C5 C 0.3104(3) 0.9436(4) -0.08278(19) 0.0158(6) Uani 1 1 d . . .
C6 C 0.4003(3) 0.8890(4) -0.12955(19) 0.0159(6) Uani 1 1 d . . .
C7 C 0.4976(3) 0.7912(4) -0.09165(18) 0.0146(6) Uani 1 1 d . . .
C8 C 0.5022(3) 0.7486(3) -0.00708(18) 0.0108(5) Uani 1 1 d . . .
C9 C 0.6002(3) 0.6449(3) 0.04128(18) 0.0109(5) Uani 1 1 d . . .
C10 C 0.7021(3) 0.5803(3) 0.00830(19) 0.0146(6) Uani 1 1 d . . .
C11 C 0.7874(3) 0.4833(3) 0.0595(2) 0.0165(6) Uani 1 1 d . . .
C12 C 0.7690(3) 0.4522(4) 0.1418(2) 0.0169(6) Uani 1 1 d . . .
C13 C 0.6652(3) 0.5210(3) 0.17110(18) 0.0144(6) Uani 1 1 d . . .
H2 H 0.460(3) 0.403(4) 0.362(2) 0.006(8) Uiso 1 1 d . . .
H3 H 0.472(3) 0.758(4) 0.526(2) 0.011(8) Uiso 1 1 d . . .
H4 H 0.265(4) 0.932(4) 0.035(2) 0.019(9) Uiso 1 1 d . . .
H5 H 0.242(4) 1.007(5) -0.104(3) 0.025(10) Uiso 1 1 d . . .
H6 H 0.394(4) 0.917(4) -0.188(3) 0.022(10) Uiso 1 1 d . . .
H7 H 0.556(4) 0.757(4) -0.119(2) 0.014(9) Uiso 1 1 d . . .
H10 H 0.714(3) 0.603(4) -0.044(2) 0.014(9) Uiso 1 1 d . . .
H11 H 0.858(3) 0.441(4) 0.040(2) 0.007(8) Uiso 1 1 d . . .
H12 H 0.823(3) 0.388(4) 0.176(2) 0.014(9) Uiso 1 1 d . . .
H13 H 0.648(4) 0.505(4) 0.227(2) 0.018(9) Uiso 1 1 d . . .


_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 O2 1.9154(19) . ?
Cu1 O5 1.944(2) . ?
Cu1 N1 1.977(2) . ?
Cu1 N2 1.992(2) . ?
Cu1 F1 2.2085(18) . ?
V1 O4 1.604(2) . ?
V1 O5 1.714(2) . ?
V1 F1 1.8584(17) 2 ?
V1 O1 1.956(2) 2 ?
V1 O3 2.0122(19) . ?
P1 O1 1.526(2) . ?
P1 O2 1.5290(19) . ?
P1 O3 1.533(2) . ?
P1 C1 1.798(3) . ?
F1 V1 1.8584(17) 2_545 ?
O1 V1 1.956(2) 2_545 ?
N1 C4 1.337(4) . ?
N1 C8 1.356(3) . ?
N2 C13 1.338(4) . ?
N2 C9 1.355(4) . ?
C1 C2 1.400(4) . ?
C1 C3 1.403(4) . ?
C2 C3 1.389(4) 3_666 ?
C2 H2 0.93(3) . ?
C3 C2 1.389(4) 3_666 ?
C3 H3 0.94(4) . ?
C4 C5 1.387(4) . ?
C4 H4 0.90(4) . ?
C5 C6 1.384(4) . ?
C5 H5 0.92(4) . ?
C6 C7 1.381(4) . ?
C6 H6 0.95(4) . ?
C7 C8 1.389(4) . ?
C7 H7 0.87(4) . ?
C8 C9 1.476(4) . ?
C9 C10 1.388(4) . ?
C10 C11 1.384(4) . ?
C10 H10 0.89(4) . ?
C11 C12 1.386(4) . ?
C11 H11 0.93(3) . ?
C12 C13 1.390(4) . ?
C12 H12 0.91(4) . ?
C13 H13 0.95(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O5 89.15(8) . . ?
O2 Cu1 N1 172.38(9) . . ?
O5 Cu1 N1 94.11(9) . . ?
O2 Cu1 N2 92.80(9) . . ?
O5 Cu1 N2 156.25(10) . . ?
N1 Cu1 N2 81.46(10) . . ?
O2 Cu1 F1 88.34(8) . . ?
O5 Cu1 F1 96.20(8) . . ?
N1 Cu1 F1 98.13(8) . . ?
N2 Cu1 F1 107.50(9) . . ?
O4 V1 O5 108.83(11) . . ?
O4 V1 F1 112.93(10) . 2 ?
O5 V1 F1 138.23(10) . 2 ?
O4 V1 O1 98.02(10) . 2 ?
O5 V1 O1 89.75(9) . 2 ?
F1 V1 O1 85.60(8) 2 2 ?
O4 V1 O3 97.09(9) . . ?
O5 V1 O3 90.30(9) . . ?
F1 V1 O3 83.74(8) 2 . ?
O1 V1 O3 164.02(8) 2 . ?
O1 P1 O2 113.22(11) . . ?
O1 P1 O3 108.78(11) . . ?
O2 P1 O3 113.67(11) . . ?
O1 P1 C1 107.89(12) . . ?
O2 P1 C1 104.39(12) . . ?
O3 P1 C1 108.58(12) . . ?
V1 F1 Cu1 135.04(9) 2_545 . ?
P1 O1 V1 140.82(12) . 2_545 ?
P1 O2 Cu1 117.96(11) . . ?
P1 O3 V1 118.63(11) . . ?
V1 O5 Cu1 149.12(12) . . ?
C4 N1 C8 119.4(2) . . ?
C4 N1 Cu1 125.31(19) . . ?
C8 N1 Cu1 115.28(19) . . ?
C13 N2 C9 119.3(2) . . ?
C13 N2 Cu1 126.0(2) . . ?
C9 N2 Cu1 114.48(19) . . ?
C2 C1 C3 118.9(2) . . ?
C2 C1 P1 117.7(2) . . ?
C3 C1 P1 123.4(2) . . ?
C3 C2 C1 120.9(3) 3_666 . ?
C3 C2 H2 118(2) 3_666 . ?
C1 C2 H2 121(2) . . ?
C2 C3 C1 120.1(3) 3_666 . ?
C2 C3 H3 118(2) 3_666 . ?
C1 C3 H3 121(2) . . ?
N1 C4 C5 122.1(3) . . ?
N1 C4 H4 116(2) . . ?
C5 C4 H4 122(2) . . ?
C6 C5 C4 118.6(3) . . ?
C6 C5 H5 124(2) . . ?
C4 C5 H5 117(2) . . ?
C7 C6 C5 119.7(3) . . ?
C7 C6 H6 120(2) . . ?
C5 C6 H6 120(2) . . ?
C6 C7 C8 119.0(3) . . ?
C6 C7 H7 122(2) . . ?
C8 C7 H7 119(2) . . ?
N1 C8 C7 121.2(3) . . ?
N1 C8 C9 114.0(2) . . ?
C7 C8 C9 124.8(3) . . ?
N2 C9 C10 121.6(3) . . ?
N2 C9 C8 114.4(2) . . ?
C10 C9 C8 124.0(3) . . ?
C11 C10 C9 118.8(3) . . ?
C11 C10 H10 121(2) . . ?
C9 C10 H10 120(2) . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 121(2) . . ?
C12 C11 H11 119(2) . . ?
C11 C12 C13 118.7(3) . . ?
C11 C12 H12 121(2) . . ?
C13 C12 H12 120(2) . . ?
N2 C13 C12 122.0(3) . . ?
N2 C13 H13 115(2) . . ?
C12 C13 H13 123(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Cu1 F1 V1 40.00(16) . . . 2_545 ?
O5 Cu1 F1 V1 -48.97(16) . . . 2_545 ?
N1 Cu1 F1 V1 -144.04(16) . . . 2_545 ?
N2 Cu1 F1 V1 132.41(15) . . . 2_545 ?
O2 P1 O1 V1 22.1(2) . . . 2_545 ?
O3 P1 O1 V1 149.47(19) . . . 2_545 ?
C1 P1 O1 V1 -92.9(2) . . . 2_545 ?
O1 P1 O2 Cu1 48.48(17) . . . . ?
O3 P1 O2 Cu1 -76.30(15) . . . . ?
C1 P1 O2 Cu1 165.56(13) . . . . ?
O5 Cu1 O2 P1 32.99(14) . . . . ?
N1 Cu1 O2 P1 148.5(6) . . . . ?
N2 Cu1 O2 P1 -170.69(14) . . . . ?
F1 Cu1 O2 P1 -63.25(13) . . . . ?
O1 P1 O3 V1 -60.91(15) . . . . ?
O2 P1 O3 V1 66.22(15) . . . . ?
C1 P1 O3 V1 -178.08(12) . . . . ?
O4 V1 O3 P1 -127.87(14) . . . . ?
O5 V1 O3 P1 -18.85(14) . . . . ?
F1 V1 O3 P1 119.72(13) 2 . . . ?
O1 V1 O3 P1 71.3(3) 2 . . . ?
O4 V1 O5 Cu1 70.9(3) . . . . ?
F1 V1 O5 Cu1 -107.6(2) 2 . . . ?
O1 V1 O5 Cu1 169.3(2) 2 . . . ?
O3 V1 O5 Cu1 -26.7(2) . . . . ?
O2 Cu1 O5 V1 21.0(2) . . . . ?
N1 Cu1 O5 V1 -152.1(2) . . . . ?
N2 Cu1 O5 V1 -74.0(3) . . . . ?
F1 Cu1 O5 V1 109.3(2) . . . . ?
O2 Cu1 N1 C4 -140.7(6) . . . . ?
O5 Cu1 N1 C4 -25.6(2) . . . . ?
N2 Cu1 N1 C4 177.9(3) . . . . ?
F1 Cu1 N1 C4 71.3(2) . . . . ?
O2 Cu1 N1 C8 37.7(8) . . . . ?
O5 Cu1 N1 C8 152.9(2) . . . . ?
N2 Cu1 N1 C8 -3.6(2) . . . . ?
F1 Cu1 N1 C8 -110.2(2) . . . . ?
O2 Cu1 N2 C13 5.4(2) . . . . ?
O5 Cu1 N2 C13 99.6(3) . . . . ?
N1 Cu1 N2 C13 -179.6(3) . . . . ?
F1 Cu1 N2 C13 -83.8(2) . . . . ?
O2 Cu1 N2 C9 -169.7(2) . . . . ?
O5 Cu1 N2 C9 -75.4(3) . . . . ?
N1 Cu1 N2 C9 5.3(2) . . . . ?
F1 Cu1 N2 C9 101.2(2) . . . . ?
O1 P1 C1 C2 72.1(2) . . . . ?
O2 P1 C1 C2 -48.6(2) . . . . ?
O3 P1 C1 C2 -170.2(2) . . . . ?
O1 P1 C1 C3 -107.0(2) . . . . ?
O2 P1 C1 C3 132.3(2) . . . . ?
O3 P1 C1 C3 10.8(3) . . . . ?
C3 C1 C2 C3 0.0(4) . . . 3_666 ?
P1 C1 C2 C3 -179.0(2) . . . 3_666 ?
C2 C1 C3 C2 0.0(4) . . . 3_666 ?
P1 C1 C3 C2 179.0(2) . . . 3_666 ?
C8 N1 C4 C5 0.0(4) . . . . ?
Cu1 N1 C4 C5 178.3(2) . . . . ?
N1 C4 C5 C6 -0.7(5) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C8 0.6(4) . . . . ?
C4 N1 C8 C7 1.1(4) . . . . ?
Cu1 N1 C8 C7 -177.5(2) . . . . ?
C4 N1 C8 C9 -180.0(2) . . . . ?
Cu1 N1 C8 C9 1.5(3) . . . . ?
C6 C7 C8 N1 -1.3(4) . . . . ?
C6 C7 C8 C9 179.8(3) . . . . ?
C13 N2 C9 C10 -1.3(4) . . . . ?
Cu1 N2 C9 C10 174.2(2) . . . . ?
C13 N2 C9 C8 178.6(2) . . . . ?
Cu1 N2 C9 C8 -5.9(3) . . . . ?
N1 C8 C9 N2 2.9(3) . . . . ?
C7 C8 C9 N2 -178.1(3) . . . . ?
N1 C8 C9 C10 -177.1(3) . . . . ?
C7 C8 C9 C10 1.8(4) . . . . ?
N2 C9 C10 C11 0.6(4) . . . . ?
C8 C9 C10 C11 -179.3(3) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
C9 N2 C13 C12 1.1(4) . . . . ?
Cu1 N2 C13 C12 -173.8(2) . . . . ?
C11 C12 C13 N2 -0.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.102

data_10
_database_code_depnum_ccdc_archive 'CCDC 734631'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H32 Cu2 F N6 O18 P4 V3'
_chemical_formula_sum            'C42 H32 Cu2 F N6 O18 P4 V3'
_chemical_formula_weight         1331.52

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'
V V 0.3005 0.5294 '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'
F F 0.0171 0.0103 '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
_symmetry_space_group_name_Hall  -P2ybc

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                   10.3398(7)
_cell_length_b                   25.5265(16)
_cell_length_c                   10.0075(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.7700(10)
_cell_angle_gamma                90.00
_cell_volume                     2315.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6334
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7254
_exptl_absorpt_correction_T_max  0.8472
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            23518
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         28.08
_reflns_number_total             5633
_reflns_number_gt                5484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0263P)²+20.9776P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         5633
_refine_ls_number_parameters     359
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0863
_refine_ls_wR_factor_ref         0.1719
_refine_ls_wR_factor_gt          0.1711
_refine_ls_goodness_of_fit_ref   1.385
_refine_ls_restrained_S_all      1.385
_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 0.55479(7) 0.13429(3) 0.30786(8) 0.01361(17) Uani 1 1 d . . .
V1 V 0.93822(10) 0.15779(4) 0.33783(11) 0.0116(2) Uani 1 1 d . . .
V2 V 1.0000 0.0000 0.5000 0.0278(4) Uani 1 2 d S . .
P1 P 0.85435(16) 0.10437(7) 0.57349(17) 0.0183(3) Uani 1 1 d . . .
P2 P 1.21902(15) 0.12379(5) 1.29924(16) 0.0112(3) Uani 1 1 d . . .
F1 F 1.1109(8) 0.0536(3) 0.5159(8) 0.0190(15) Uani 0.50 1 d P . .
O1 O 0.8700(5) 0.04834(19) 0.5331(5) 0.0237(10) Uani 1 1 d . . .
O2 O 0.9313(5) 0.14417(19) 0.5175(5) 0.0224(10) Uani 1 1 d . . .
O3 O 0.6936(4) 0.11952(18) 0.5165(5) 0.0190(9) Uani 1 1 d . . .
O4 O 1.3593(4) 0.15054(15) 1.3361(4) 0.0141(8) Uani 1 1 d . . .
O5 O 1.2476(4) 0.06672(16) 1.3639(5) 0.0163(8) Uani 1 1 d . . .
H5' H 1.1836 0.0587 1.3892 0.025 Uiso 1 1 calc R . .
O6 O 1.1293(4) 0.15330(16) 1.3620(5) 0.0177(9) Uani 1 1 d . . .
O7 O 0.8885(5) 0.21747(17) 0.2892(5) 0.0226(9) Uani 1 1 d . . .
O8 O 0.8235(6) 0.1215(2) 0.2023(6) 0.0391(14) Uani 1 1 d . . .
O9 O 0.9988(10) 0.0356(4) 0.3478(11) 0.0231(19) Uani 0.50 1 d P . .
O10 O 1.1579(11) 0.0234(4) 0.6443(11) 0.028(2) Uani 0.50 1 d PU . .
N1 N 0.4943(6) 0.0604(2) 0.2285(6) 0.0219(11) Uani 1 1 d . . .
N2 N 0.4481(5) 0.1484(2) 0.0914(5) 0.0159(10) Uani 1 1 d . . .
N3 N 0.5958(5) 0.2115(2) 0.3091(5) 0.0156(10) Uani 1 1 d . . .
C1 C 0.9494(6) 0.1110(2) 0.7776(6) 0.0163(11) Uani 1 1 d . . .
C2 C 0.9883(7) 0.0657(3) 0.8669(7) 0.0220(13) Uani 1 1 d . . .
H2 H 0.9617 0.0322 0.8199 0.026 Uiso 1 1 calc R . .
C3 C 1.0662(7) 0.0697(2) 1.0251(7) 0.0184(12) Uani 1 1 d . . .
H3 H 1.0926 0.0388 1.0854 0.022 Uiso 1 1 calc R . .
C4 C 1.1058(6) 0.1183(2) 1.0960(6) 0.0144(11) Uani 1 1 d . . .
C5 C 1.0637(7) 0.1634(2) 1.0049(7) 0.0181(12) Uani 1 1 d . . .
H5 H 1.0890 0.1969 1.0516 0.022 Uiso 1 1 calc R . .
C6 C 0.9854(7) 0.1596(2) 0.8470(7) 0.0200(12) Uani 1 1 d . . .
H6 H 0.9566 0.1905 0.7865 0.024 Uiso 1 1 calc R . .
C7 C 0.5221(7) 0.0169(3) 0.3137(8) 0.0248(14) Uani 1 1 d . . .
H7 H 0.5856 0.0190 0.4206 0.030 Uiso 1 1 calc R . .
C8 C 0.4604(8) -0.0307(3) 0.2494(9) 0.0327(16) Uani 1 1 d . . .
H8 H 0.4794 -0.0609 0.3117 0.039 Uiso 1 1 calc R . .
C9 C 0.3709(8) -0.0341(3) 0.0940(9) 0.0324(16) Uani 1 1 d . . .
H9 H 0.3282 -0.0666 0.0480 0.039 Uiso 1 1 calc R . .
C10 C 0.3436(7) 0.0106(3) 0.0050(8) 0.0293(15) Uani 1 1 d . . .
H10 H 0.2824 0.0089 -0.1024 0.035 Uiso 1 1 calc R . .
C11 C 0.4067(7) 0.0576(3) 0.0746(8) 0.0231(13) Uani 1 1 d . . .
C12 C 0.3835(6) 0.1085(3) -0.0042(7) 0.0216(13) Uani 1 1 d . . .
C13 C 0.3035(7) 0.1182(3) -0.1604(7) 0.0241(14) Uani 1 1 d . . .
H13 H 0.2598 0.0901 -0.2305 0.029 Uiso 1 1 calc R . .
C14 C 0.2891(7) 0.1692(3) -0.2114(7) 0.0273(15) Uani 1 1 d . . .
H14 H 0.2344 0.1763 -0.3175 0.033 Uiso 1 1 calc R . .
C15 C 0.3539(7) 0.2102(3) -0.1092(7) 0.0258(14) Uani 1 1 d . . .
H15 H 0.3420 0.2454 -0.1436 0.031 Uiso 1 1 calc R . .
C16 C 0.4363(6) 0.1982(3) 0.0445(6) 0.0161(11) Uani 1 1 d . . .
C17 C 0.5230(6) 0.2348(2) 0.1694(6) 0.0161(11) Uani 1 1 d . . .
C18 C 0.5352(7) 0.2878(3) 0.1507(7) 0.0207(13) Uani 1 1 d . . .
H18 H 0.4818 0.3032 0.0525 0.025 Uiso 1 1 calc R . .
C19 C 0.6242(7) 0.3184(3) 0.2738(8) 0.0234(13) Uani 1 1 d . . .
H19 H 0.6343 0.3548 0.2616 0.028 Uiso 1 1 calc R . .
C20 C 0.6997(7) 0.2951(3) 0.4173(7) 0.0211(12) Uani 1 1 d . . .
H20 H 0.7621 0.3152 0.5047 0.025 Uiso 1 1 calc R . .
C21 C 0.6815(6) 0.2417(3) 0.4293(6) 0.0185(12) Uani 1 1 d . . .
H21 H 0.7321 0.2259 0.5271 0.022 Uiso 1 1 calc R . .


_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 O3 1.918(4) . ?
Cu1 N2 1.933(5) . ?
Cu1 N3 2.014(5) . ?
Cu1 N1 2.024(6) . ?
Cu1 O4 2.211(4) 1_454 ?
V1 O8 1.599(5) . ?
V1 O7 1.606(4) . ?
V1 O2 1.866(4) . ?
V1 O6 1.875(4) 1_554 ?
V2 O10 1.685(10) 3_756 ?
V2 O10 1.685(10) . ?
V2 F1 1.743(6) 3_756 ?
V2 F1 1.743(6) . ?
V2 O9 1.769(8) 3_756 ?
V2 O9 1.769(8) . ?
V2 O1 1.967(5) 3_756 ?
V2 O1 1.967(5) . ?
P1 O1 1.516(5) . ?
P1 O3 1.525(4) . ?
P1 O2 1.552(4) . ?
P1 C1 1.799(6) . ?
P2 O4 1.480(4) . ?
P2 O6 1.544(4) . ?
P2 O5 1.563(4) . ?
P2 C4 1.799(6) . ?
O4 Cu1 2.211(4) 1_656 ?
O5 H5' 0.8400 . ?
O6 V1 1.875(4) 1_556 ?
N1 C7 1.345(9) . ?
N1 C11 1.362(8) . ?
N2 C12 1.334(8) . ?
N2 C16 1.340(8) . ?
N3 C21 1.342(8) . ?
N3 C17 1.365(7) . ?
C1 C6 1.382(9) . ?
C1 C2 1.398(8) . ?
C2 C3 1.392(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(8) . ?
C5 C6 1.389(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.381(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.480(9) . ?
C12 C13 1.394(9) . ?
C13 C14 1.380(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.470(8) . ?
C17 C18 1.381(9) . ?
C18 C19 1.372(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.388(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?

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
O3 Cu1 N2 168.79(19) . . ?
O3 Cu1 N3 98.1(2) . . ?
N2 Cu1 N3 80.2(2) . . ?
O3 Cu1 N1 99.9(2) . . ?
N2 Cu1 N1 80.3(2) . . ?
N3 Cu1 N1 159.7(2) . . ?
O3 Cu1 O4 98.57(16) . 1_454 ?
N2 Cu1 O4 92.55(17) . 1_454 ?
N3 Cu1 O4 91.07(17) . 1_454 ?
N1 Cu1 O4 95.52(17) . 1_454 ?
O8 V1 O7 107.1(3) . . ?
O8 V1 O2 110.6(2) . . ?
O7 V1 O2 108.3(2) . . ?
O8 V1 O6 112.3(2) . 1_554 ?
O7 V1 O6 105.1(2) . 1_554 ?
O2 V1 O6 113.00(19) . 1_554 ?
O10 V2 O10 179.999(1) 3_756 . ?
O10 V2 F1 47.1(4) 3_756 3_756 ?
O10 V2 F1 132.9(4) . 3_756 ?
O10 V2 F1 132.9(4) 3_756 . ?
O10 V2 F1 47.1(4) . . ?
F1 V2 F1 179.997(1) 3_756 . ?
O10 V2 O9 99.1(5) 3_756 3_756 ?
O10 V2 O9 80.9(5) . 3_756 ?
F1 V2 O9 53.6(4) 3_756 3_756 ?
F1 V2 O9 126.4(4) . 3_756 ?
O10 V2 O9 80.9(5) 3_756 . ?
O10 V2 O9 99.1(5) . . ?
F1 V2 O9 126.4(4) 3_756 . ?
F1 V2 O9 53.6(4) . . ?
O9 V2 O9 180.000(1) 3_756 . ?
O10 V2 O1 95.3(3) 3_756 3_756 ?
O10 V2 O1 84.7(3) . 3_756 ?
F1 V2 O1 88.0(3) 3_756 3_756 ?
F1 V2 O1 92.0(3) . 3_756 ?
O9 V2 O1 95.8(3) 3_756 3_756 ?
O9 V2 O1 84.2(3) . 3_756 ?
O10 V2 O1 84.7(3) 3_756 . ?
O10 V2 O1 95.3(3) . . ?
F1 V2 O1 92.0(3) 3_756 . ?
F1 V2 O1 88.0(3) . . ?
O9 V2 O1 84.2(3) 3_756 . ?
O9 V2 O1 95.8(3) . . ?
O1 V2 O1 179.998(1) 3_756 . ?
O1 P1 O3 112.1(3) . . ?
O1 P1 O2 112.5(3) . . ?
O3 P1 O2 110.8(2) . . ?
O1 P1 C1 108.8(3) . . ?
O3 P1 C1 107.6(3) . . ?
O2 P1 C1 104.7(3) . . ?
O4 P2 O6 112.5(2) . . ?
O4 P2 O5 111.1(2) . . ?
O6 P2 O5 108.5(2) . . ?
O4 P2 C4 110.1(2) . . ?
O6 P2 C4 107.8(3) . . ?
O5 P2 C4 106.6(3) . . ?
P1 O1 V2 143.7(3) . . ?
P1 O2 V1 137.2(3) . . ?
P1 O3 Cu1 124.5(3) . . ?
P2 O4 Cu1 136.7(2) . 1_656 ?
P2 O5 H5' 109.5 . . ?
P2 O6 V1 141.2(3) . 1_556 ?
C7 N1 C11 119.7(6) . . ?
C7 N1 Cu1 126.1(5) . . ?
C11 N1 Cu1 113.9(5) . . ?
C12 N2 C16 122.8(5) . . ?
C12 N2 Cu1 118.7(4) . . ?
C16 N2 Cu1 118.4(4) . . ?
C21 N3 C17 117.8(5) . . ?
C21 N3 Cu1 127.9(4) . . ?
C17 N3 Cu1 114.2(4) . . ?
C6 C1 C2 119.8(5) . . ?
C6 C1 P1 121.5(4) . . ?
C2 C1 P1 118.7(5) . . ?
C3 C2 C1 119.8(6) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 121.0(5) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 118.6(5) . . ?
C3 C4 P2 121.2(4) . . ?
C5 C4 P2 120.1(5) . . ?
C6 C5 C4 120.7(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C1 C6 C5 120.2(5) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
N1 C7 C8 121.5(7) . . ?
N1 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 119.3(7) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.5(7) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 119.2(7) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
N1 C11 C10 120.8(7) . . ?
N1 C11 C12 113.8(6) . . ?
C10 C11 C12 125.3(6) . . ?
N2 C12 C13 119.5(6) . . ?
N2 C12 C11 113.0(5) . . ?
C13 C12 C11 127.5(6) . . ?
C14 C13 C12 118.7(6) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.7(6) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 118.1(6) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
N2 C16 C15 120.1(6) . . ?
N2 C16 C17 112.9(5) . . ?
C15 C16 C17 126.9(6) . . ?
N3 C17 C18 121.7(6) . . ?
N3 C17 C16 113.8(5) . . ?
C18 C17 C16 124.5(5) . . ?
C19 C18 C17 120.1(6) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 118.8(6) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
C21 C20 C19 118.4(6) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
N3 C21 C20 123.1(5) . . ?
N3 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?

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
O3 P1 O1 V2 156.6(4) . . . . ?
O2 P1 O1 V2 30.9(5) . . . . ?
C1 P1 O1 V2 -84.6(5) . . . . ?
O10 V2 O1 P1 -140.3(6) 3_756 . . . ?
O10 V2 O1 P1 39.7(6) . . . . ?
F1 V2 O1 P1 173.1(5) 3_756 . . . ?
F1 V2 O1 P1 -6.9(5) . . . . ?
O9 V2 O1 P1 120.0(6) 3_756 . . . ?
O9 V2 O1 P1 -60.0(6) . . . . ?
O1 V2 O1 P1 -4.1(10) 3_756 . . . ?
O1 P1 O2 V1 48.0(5) . . . . ?
O3 P1 O2 V1 -78.4(5) . . . . ?
C1 P1 O2 V1 165.9(4) . . . . ?
O8 V1 O2 P1 6.3(5) . . . . ?
O7 V1 O2 P1 123.4(4) . . . . ?
O6 V1 O2 P1 -120.6(4) 1_554 . . . ?
O1 P1 O3 Cu1 -74.9(4) . . . . ?
O2 P1 O3 Cu1 51.6(4) . . . . ?
C1 P1 O3 Cu1 165.5(3) . . . . ?
N2 Cu1 O3 P1 -8.1(13) . . . . ?
N3 Cu1 O3 P1 -88.4(3) . . . . ?
N1 Cu1 O3 P1 82.1(3) . . . . ?
O4 Cu1 O3 P1 179.3(3) 1_454 . . . ?
O6 P2 O4 Cu1 174.7(3) . . . 1_656 ?
O5 P2 O4 Cu1 52.9(4) . . . 1_656 ?
C4 P2 O4 Cu1 -65.0(4) . . . 1_656 ?
O4 P2 O6 V1 162.3(4) . . . 1_556 ?
O5 P2 O6 V1 -74.5(5) . . . 1_556 ?
C4 P2 O6 V1 40.7(5) . . . 1_556 ?
O3 Cu1 N1 C7 13.6(5) . . . . ?
N2 Cu1 N1 C7 -177.8(5) . . . . ?
N3 Cu1 N1 C7 165.5(5) . . . . ?
O4 Cu1 N1 C7 -86.2(5) 1_454 . . . ?
O3 Cu1 N1 C11 -172.6(4) . . . . ?
N2 Cu1 N1 C11 -4.0(4) . . . . ?
N3 Cu1 N1 C11 -20.7(8) . . . . ?
O4 Cu1 N1 C11 87.7(4) 1_454 . . . ?
O3 Cu1 N2 C12 94.6(11) . . . . ?
N3 Cu1 N2 C12 176.7(4) . . . . ?
N1 Cu1 N2 C12 2.5(4) . . . . ?
O4 Cu1 N2 C12 -92.7(4) 1_454 . . . ?
O3 Cu1 N2 C16 -88.5(12) . . . . ?
N3 Cu1 N2 C16 -6.5(4) . . . . ?
N1 Cu1 N2 C16 179.3(4) . . . . ?
O4 Cu1 N2 C16 84.2(4) 1_454 . . . ?
O3 Cu1 N3 C21 -7.6(5) . . . . ?
N2 Cu1 N3 C21 -176.4(5) . . . . ?
N1 Cu1 N3 C21 -159.7(5) . . . . ?
O4 Cu1 N3 C21 91.2(5) 1_454 . . . ?
O3 Cu1 N3 C17 174.1(4) . . . . ?
N2 Cu1 N3 C17 5.3(4) . . . . ?
N1 Cu1 N3 C17 22.0(8) . . . . ?
O4 Cu1 N3 C17 -87.1(4) 1_454 . . . ?
O1 P1 C1 C6 163.7(5) . . . . ?
O3 P1 C1 C6 -74.6(5) . . . . ?
O2 P1 C1 C6 43.3(5) . . . . ?
O1 P1 C1 C2 -15.6(5) . . . . ?
O3 P1 C1 C2 106.0(5) . . . . ?
O2 P1 C1 C2 -136.1(5) . . . . ?
C6 C1 C2 C3 -1.5(9) . . . . ?
P1 C1 C2 C3 177.9(5) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C2 C3 C4 P2 -175.0(5) . . . . ?
O4 P2 C4 C3 117.7(5) . . . . ?
O6 P2 C4 C3 -119.2(5) . . . . ?
O5 P2 C4 C3 -2.9(5) . . . . ?
O4 P2 C4 C5 -58.1(5) . . . . ?
O6 P2 C4 C5 65.0(5) . . . . ?
O5 P2 C4 C5 -178.7(4) . . . . ?
C3 C4 C5 C6 -0.7(9) . . . . ?
P2 C4 C5 C6 175.3(4) . . . . ?
C2 C1 C6 C5 1.8(9) . . . . ?
P1 C1 C6 C5 -177.6(4) . . . . ?
C4 C5 C6 C1 -0.7(9) . . . . ?
C11 N1 C7 C8 -1.8(9) . . . . ?
Cu1 N1 C7 C8 171.8(5) . . . . ?
N1 C7 C8 C9 1.4(11) . . . . ?
C7 C8 C9 C10 -0.4(11) . . . . ?
C8 C9 C10 C11 -0.2(10) . . . . ?
C7 N1 C11 C10 1.1(9) . . . . ?
Cu1 N1 C11 C10 -173.2(5) . . . . ?
C7 N1 C11 C12 178.9(5) . . . . ?
Cu1 N1 C11 C12 4.7(6) . . . . ?
C9 C10 C11 N1 -0.1(9) . . . . ?
C9 C10 C11 C12 -177.7(6) . . . . ?
C16 N2 C12 C13 2.0(8) . . . . ?
Cu1 N2 C12 C13 178.7(4) . . . . ?
C16 N2 C12 C11 -177.4(5) . . . . ?
Cu1 N2 C12 C11 -0.7(6) . . . . ?
N1 C11 C12 N2 -2.7(7) . . . . ?
C10 C11 C12 N2 175.0(6) . . . . ?
N1 C11 C12 C13 178.0(6) . . . . ?
C10 C11 C12 C13 -4.3(10) . . . . ?
N2 C12 C13 C14 -2.2(9) . . . . ?
C11 C12 C13 C14 177.0(6) . . . . ?
C12 C13 C14 C15 0.4(9) . . . . ?
C13 C14 C15 C16 1.7(9) . . . . ?
C12 N2 C16 C15 0.2(8) . . . . ?
Cu1 N2 C16 C15 -176.5(4) . . . . ?
C12 N2 C16 C17 -177.0(5) . . . . ?
Cu1 N2 C16 C17 6.3(6) . . . . ?
C14 C15 C16 N2 -2.0(9) . . . . ?
C14 C15 C16 C17 174.8(6) . . . . ?
C21 N3 C17 C18 -0.5(8) . . . . ?
Cu1 N3 C17 C18 178.0(4) . . . . ?
C21 N3 C17 C16 178.0(5) . . . . ?
Cu1 N3 C17 C16 -3.5(6) . . . . ?
N2 C16 C17 N3 -1.5(7) . . . . ?
C15 C16 C17 N3 -178.5(6) . . . . ?
N2 C16 C17 C18 176.9(5) . . . . ?
C15 C16 C17 C18 -0.1(9) . . . . ?
N3 C17 C18 C19 1.2(9) . . . . ?
C16 C17 C18 C19 -177.1(5) . . . . ?
C17 C18 C19 C20 -0.9(9) . . . . ?
C18 C19 C20 C21 0.0(9) . . . . ?
C17 N3 C21 C20 -0.5(8) . . . . ?
Cu1 N3 C21 C20 -178.7(4) . . . . ?
C19 C20 C21 N3 0.7(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.153

data_11
_database_code_depnum_ccdc_archive 'CCDC 734632'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H22 CU2 F2 N6 O10 P2 V2'
_chemical_formula_sum            'C26 H22 Cu2 F2 N6 O10 P2 V2'
_chemical_formula_weight         907.40

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'
F F 0.0171 0.0103 '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'
V V 0.3005 0.5294 '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)/n
_symmetry_space_group_name_Hall  -P2yn

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                   10.893(2)
_cell_length_b                   8.7599(18)
_cell_length_c                   16.069(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.38(3)
_cell_angle_gamma                90.00
_cell_volume                     1533.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3737
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.09

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5656
_exptl_absorpt_correction_T_max  0.8472
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            14897
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         28.09
_reflns_number_total             3737
_reflns_number_gt                3028
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0586P)²+1.4096P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         3737
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.52340(3) 0.29957(4) 0.16124(2) 0.01458(12) Uani 1 1 d . . .
V1 V 0.82043(5) 0.51195(6) 0.22571(3) 0.01433(14) Uani 1 1 d . . .
P1 P 0.61278(7) 0.33347(9) 0.34012(4) 0.01167(17) Uani 1 1 d . . .
F1 F 0.67956(17) 0.4794(2) 0.15862(11) 0.0223(4) Uani 1 1 d . . .
O1 O 0.50839(19) 0.3488(3) 0.27727(12) 0.0154(4) Uani 1 1 d . . .
O2 O 0.6440(2) 0.1674(2) 0.36250(13) 0.0168(5) Uani 1 1 d . . .
O3 O 0.7276(2) 0.4186(3) 0.31473(13) 0.0208(5) Uani 1 1 d . . .
O4 O 0.9186(2) 0.3835(3) 0.20385(15) 0.0323(6) Uani 1 1 d . . .
O5 O 0.6163(3) 0.1288(4) 0.20257(15) 0.0506(10) Uani 1 1 d . . .
N1 N 0.5482(2) 0.2334(3) 0.04479(15) 0.0139(5) Uani 1 1 d . . .
N2 N 0.3740(2) 0.4210(3) 0.13344(16) 0.0164(5) Uani 1 1 d . . .
N3 N 0.3795(3) 0.3702(3) -0.01136(16) 0.0204(6) Uani 1 1 d . . .
H3' H 0.3442 0.3936 -0.0576 0.025 Uiso 1 1 calc R . .
C1 C 0.5352(3) 0.3479(3) 0.50731(18) 0.0144(6) Uani 1 1 d . . .
H1 H 0.5588 0.2463 0.5123 0.017 Uiso 1 1 calc R . .
C2 C 0.5536(3) 0.4252(3) 0.43224(17) 0.0121(6) Uani 1 1 d . . .
C3 C 0.5182(3) 0.5784(3) 0.42584(18) 0.0147(6) Uani 1 1 d . . .
H3 H 0.5305 0.6310 0.3763 0.018 Uiso 1 1 calc R . .
C4 C 0.6440(3) 0.1373(4) 0.0298(2) 0.0212(7) Uani 1 1 d . . .
H4 H 0.6921 0.1064 0.0747 0.025 Uiso 1 1 calc R . .
C5 C 0.6734(3) 0.0838(4) -0.0477(2) 0.0240(7) Uani 1 1 d . . .
H5 H 0.7404 0.0196 -0.0552 0.029 Uiso 1 1 calc R . .
C6 C 0.5996(3) 0.1284(4) -0.1154(2) 0.0225(7) Uani 1 1 d . . .
H6 H 0.6167 0.0940 -0.1688 0.027 Uiso 1 1 calc R . .
C7 C 0.5027(3) 0.2230(4) -0.1015(2) 0.0202(7) Uani 1 1 d . . .
H7 H 0.4525 0.2530 -0.1456 0.024 Uiso 1 1 calc R . .
C8 C 0.4787(3) 0.2752(3) -0.02048(19) 0.0146(6) Uani 1 1 d . . .
C9 C 0.3258(3) 0.4349(4) 0.05655(19) 0.0161(6) Uani 1 1 d . . .
C10 C 0.2171(3) 0.5180(4) 0.0418(2) 0.0211(7) Uani 1 1 d . . .
H10 H 0.1859 0.5275 -0.0120 0.025 Uiso 1 1 calc R . .
C11 C 0.1582(3) 0.5840(4) 0.1065(2) 0.0257(7) Uani 1 1 d . . .
H11 H 0.0854 0.6373 0.0976 0.031 Uiso 1 1 calc R . .
C12 C 0.2071(3) 0.5716(4) 0.1863(2) 0.0278(8) Uani 1 1 d . . .
H12 H 0.1682 0.6166 0.2314 0.033 Uiso 1 1 calc R . .
C13 C 0.3136(3) 0.4916(4) 0.1967(2) 0.0251(8) Uani 1 1 d . . .
H13 H 0.3469 0.4849 0.2500 0.030 Uiso 1 1 calc R . .


_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 O5 1.922(3) . ?
Cu1 O1 1.922(2) . ?
Cu1 N1 1.979(2) . ?
Cu1 N2 1.993(3) . ?
Cu1 F1 2.3192(19) . ?
V1 O4 1.593(3) . ?
V1 O5 1.686(2) 2_655 ?
V1 F1 1.891(2) . ?
V1 O3 1.938(2) . ?
V1 O2 2.005(2) 2_655 ?
P1 O3 1.514(2) . ?
P1 O1 1.522(2) . ?
P1 O2 1.536(2) . ?
P1 C2 1.807(3) . ?
O2 V1 2.005(2) 2_645 ?
O5 V1 1.685(2) 2_645 ?
N1 C8 1.340(4) . ?
N1 C4 1.364(4) . ?
N2 C9 1.345(4) . ?
N2 C13 1.363(4) . ?
N3 C9 1.365(4) . ?
N3 C8 1.372(4) . ?
N3 H3' 0.8600 . ?
C1 C3 1.384(4) 3_666 ?
C1 C2 1.399(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.400(4) . ?
C3 C1 1.384(4) 3_666 ?
C3 H3 0.9300 . ?
C4 C5 1.371(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.361(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.406(4) . ?
C7 H7 0.9300 . ?
C9 C10 1.409(4) . ?
C10 C11 1.355(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.365(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?

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
O5 Cu1 O1 83.54(10) . . ?
O5 Cu1 N1 91.39(10) . . ?
O1 Cu1 N1 174.92(10) . . ?
O5 Cu1 N2 156.99(14) . . ?
O1 Cu1 N2 91.32(10) . . ?
N1 Cu1 N2 93.47(11) . . ?
O5 Cu1 F1 98.65(13) . . ?
O1 Cu1 F1 86.11(8) . . ?
N1 Cu1 F1 94.42(9) . . ?
N2 Cu1 F1 103.38(9) . . ?
O4 V1 O5 107.94(18) . 2_655 ?
O4 V1 F1 108.12(13) . . ?
O5 V1 F1 143.88(16) 2_655 . ?
O4 V1 O3 102.64(12) . . ?
O5 V1 O3 87.98(11) 2_655 . ?
F1 V1 O3 86.08(9) . . ?
O4 V1 O2 101.00(11) . 2_655 ?
O5 V1 O2 89.46(11) 2_655 2_655 ?
F1 V1 O2 81.92(9) . 2_655 ?
O3 V1 O2 155.85(10) . 2_655 ?
O3 P1 O1 113.10(13) . . ?
O3 P1 O2 110.34(14) . . ?
O1 P1 O2 113.72(13) . . ?
O3 P1 C2 107.54(13) . . ?
O1 P1 C2 103.61(13) . . ?
O2 P1 C2 108.00(13) . . ?
V1 F1 Cu1 133.20(9) . . ?
P1 O1 Cu1 123.77(13) . . ?
P1 O2 V1 121.41(12) . 2_645 ?
P1 O3 V1 147.41(14) . . ?
V1 O5 Cu1 157.08(15) 2_645 . ?
C8 N1 C4 117.3(3) . . ?
C8 N1 Cu1 125.5(2) . . ?
C4 N1 Cu1 117.2(2) . . ?
C9 N2 C13 117.2(3) . . ?
C9 N2 Cu1 124.6(2) . . ?
C13 N2 Cu1 118.2(2) . . ?
C9 N3 C8 132.8(3) . . ?
C9 N3 H3' 113.6 . . ?
C8 N3 H3' 113.6 . . ?
C3 C1 C2 120.4(3) 3_666 . ?
C3 C1 H1 119.8 3_666 . ?
C2 C1 H1 119.8 . . ?
C1 C2 C3 119.1(3) . . ?
C1 C2 P1 123.0(2) . . ?
C3 C2 P1 117.8(2) . . ?
C1 C3 C2 120.5(3) 3_666 . ?
C1 C3 H3 119.8 3_666 . ?
C2 C3 H3 119.8 . . ?
N1 C4 C5 123.8(3) . . ?
N1 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C4 C5 C6 118.2(3) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C7 C6 C5 118.9(3) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 119.9(3) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
N1 C8 N3 121.5(3) . . ?
N1 C8 C7 121.9(3) . . ?
N3 C8 C7 116.6(3) . . ?
N2 C9 N3 122.0(3) . . ?
N2 C9 C10 121.6(3) . . ?
N3 C9 C10 116.4(3) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 118.3(3) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
N2 C13 C12 123.7(3) . . ?
N2 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?

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
O4 V1 F1 Cu1 73.60(17) . . . . ?
O5 V1 F1 Cu1 -109.6(2) 2_655 . . . ?
O3 V1 F1 Cu1 -28.42(15) . . . . ?
O2 V1 F1 Cu1 172.59(15) 2_655 . . . ?
O5 Cu1 F1 V1 -32.75(16) . . . . ?
O1 Cu1 F1 V1 50.11(15) . . . . ?
N1 Cu1 F1 V1 -124.83(15) . . . . ?
N2 Cu1 F1 V1 140.54(15) . . . . ?
O3 P1 O1 Cu1 54.4(2) . . . . ?
O2 P1 O1 Cu1 -72.45(18) . . . . ?
C2 P1 O1 Cu1 170.56(15) . . . . ?
O5 Cu1 O1 P1 40.81(19) . . . . ?
N1 Cu1 O1 P1 37.8(12) . . . . ?
N2 Cu1 O1 P1 -161.69(17) . . . . ?
F1 Cu1 O1 P1 -58.36(16) . . . . ?
O3 P1 O2 V1 -75.43(17) . . . 2_645 ?
O1 P1 O2 V1 52.88(18) . . . 2_645 ?
C2 P1 O2 V1 167.28(14) . . . 2_645 ?
O1 P1 O3 V1 -19.7(3) . . . . ?
O2 P1 O3 V1 108.9(3) . . . . ?
C2 P1 O3 V1 -133.5(3) . . . . ?
O4 V1 O3 P1 -99.2(3) . . . . ?
O5 V1 O3 P1 152.9(3) 2_655 . . . ?
F1 V1 O3 P1 8.5(3) . . . . ?
O2 V1 O3 P1 68.7(4) 2_655 . . . ?
O1 Cu1 O5 V1 3.5(6) . . . 2_645 ?
N1 Cu1 O5 V1 -176.8(6) . . . 2_645 ?
N2 Cu1 O5 V1 -74.6(8) . . . 2_645 ?
F1 Cu1 O5 V1 88.5(7) . . . 2_645 ?
O5 Cu1 N1 C8 159.4(3) . . . . ?
O1 Cu1 N1 C8 162.4(10) . . . . ?
N2 Cu1 N1 C8 1.9(3) . . . . ?
F1 Cu1 N1 C8 -101.8(3) . . . . ?
O5 Cu1 N1 C4 -20.6(3) . . . . ?
O1 Cu1 N1 C4 -17.6(13) . . . . ?
N2 Cu1 N1 C4 -178.1(2) . . . . ?
F1 Cu1 N1 C4 78.2(2) . . . . ?
O5 Cu1 N2 C9 -102.0(3) . . . . ?
O1 Cu1 N2 C9 -178.5(3) . . . . ?
N1 Cu1 N2 C9 -0.2(3) . . . . ?
F1 Cu1 N2 C9 95.2(3) . . . . ?
O5 Cu1 N2 C13 75.9(4) . . . . ?
O1 Cu1 N2 C13 -0.6(3) . . . . ?
N1 Cu1 N2 C13 177.7(3) . . . . ?
F1 Cu1 N2 C13 -86.9(3) . . . . ?
C3 C1 C2 C3 0.4(5) 3_666 . . . ?
C3 C1 C2 P1 -175.6(2) 3_666 . . . ?
O3 P1 C2 C1 -122.6(3) . . . . ?
O1 P1 C2 C1 117.4(3) . . . . ?
O2 P1 C2 C1 -3.5(3) . . . . ?
O3 P1 C2 C3 61.4(3) . . . . ?
O1 P1 C2 C3 -58.6(3) . . . . ?
O2 P1 C2 C3 -179.5(2) . . . . ?
C1 C2 C3 C1 -0.4(5) . . . 3_666 ?
P1 C2 C3 C1 175.8(2) . . . 3_666 ?
C8 N1 C4 C5 0.9(5) . . . . ?
Cu1 N1 C4 C5 -179.1(3) . . . . ?
N1 C4 C5 C6 -1.0(6) . . . . ?
C4 C5 C6 C7 0.2(5) . . . . ?
C5 C6 C7 C8 0.5(5) . . . . ?
C4 N1 C8 N3 179.3(3) . . . . ?
Cu1 N1 C8 N3 -0.7(4) . . . . ?
C4 N1 C8 C7 -0.1(5) . . . . ?
Cu1 N1 C8 C7 179.9(2) . . . . ?
C9 N3 C8 N1 -3.4(6) . . . . ?
C9 N3 C8 C7 176.0(3) . . . . ?
C6 C7 C8 N1 -0.6(5) . . . . ?
C6 C7 C8 N3 180.0(3) . . . . ?
C13 N2 C9 N3 179.3(3) . . . . ?
Cu1 N2 C9 N3 -2.7(4) . . . . ?
C13 N2 C9 C10 -0.4(5) . . . . ?
Cu1 N2 C9 C10 177.5(2) . . . . ?
C8 N3 C9 N2 5.3(6) . . . . ?
C8 N3 C9 C10 -175.0(3) . . . . ?
N2 C9 C10 C11 -0.9(5) . . . . ?
N3 C9 C10 C11 179.3(3) . . . . ?
C9 C10 C11 C12 1.3(5) . . . . ?
C10 C11 C12 C13 -0.4(6) . . . . ?
C9 N2 C13 C12 1.5(5) . . . . ?
Cu1 N2 C13 C12 -176.6(3) . . . . ?
C11 C12 C13 N2 -1.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.09
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.123

#[Cu(bipy)VVO2{(HO3P)3C6H3}] ?1.5 H2O 12
data_[Cu(bipy)VVO2{(HO3P)3C6H3}]?1.5H2O12
_database_code_depnum_ccdc_archive 'CCDC 734633'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H17 Cu N2 O12.50 P3 V'
_chemical_formula_weight         644.71

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'
V V 0.3005 0.5294 '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  -P1

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

_cell_length_a                   10.2667(11)
_cell_length_b                   10.3840(11)
_cell_length_c                   10.6223(11)
_cell_angle_alpha                99.967(2)
_cell_angle_beta                 92.781(2)
_cell_angle_gamma                101.734(2)
_cell_volume                     1087.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3268
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7845
_exptl_absorpt_correction_T_max  0.8484
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            10999
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         28.32
_reflns_number_total             5342
_reflns_number_gt                4984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0436P)²+4.0566P] where P=(Fo²+2Fc²)/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         5342
_refine_ls_number_parameters     347
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1374
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_restrained_S_all      1.251
_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 0.65663(5) 0.13965(5) 0.55420(5) 0.00826(13) Uani 1 1 d . . .
V1 V 0.81294(7) 0.29873(7) 0.86988(7) 0.00941(16) Uani 1 1 d . . .
P1 P 0.42205(10) 0.61703(11) 0.27748(10) 0.0086(2) Uani 1 1 d . . .
P2 P 0.81667(10) 0.36991(10) 0.41977(10) 0.0087(2) Uani 1 1 d . . .
P3 P 0.87138(10) 0.61975(11) 0.00365(10) 0.0086(2) Uani 1 1 d . . .
O1 O 0.4549(3) 0.7375(3) 0.3863(3) 0.0109(6) Uani 1 1 d . . .
O2 O 0.3361(3) 0.4933(3) 0.3213(3) 0.0160(7) Uani 1 1 d . . .
O3 O 0.3611(3) 0.6449(3) 0.1547(3) 0.0125(6) Uani 1 1 d . . .
O4 O 0.8522(3) 0.4681(3) 0.5466(3) 0.0115(6) Uani 1 1 d . . .
O5 O 0.7206(3) 0.2415(3) 0.4246(3) 0.0106(6) Uani 1 1 d . . .
O6 O 0.9483(3) 0.3381(3) 0.3655(3) 0.0122(6) Uani 1 1 d . . .
O7 O 0.8847(3) 0.4962(3) -0.0890(3) 0.0105(6) Uani 1 1 d . . .
O8 O 0.7929(4) 0.7053(4) -0.0661(4) 0.0164(7) Uani 1 1 d . . .
O9 O 1.0022(3) 0.7070(3) 0.0651(3) 0.0125(6) Uani 1 1 d . . .
O10 O 0.8207(3) 0.2318(3) 0.7207(3) 0.0145(6) Uani 1 1 d . . .
O11 O 0.7468(3) 0.1827(3) 0.9465(3) 0.0182(7) Uani 1 1 d . . .
O90 O 0.8713(8) 0.9721(6) 0.9963(10) 0.080(3) Uani 0.75 1 d P . .
O91A O 0.0873(14) 0.8910(14) 0.8592(13) 0.048(4) Uani 0.364(13) 1 d P A 1
O91B O -0.0458(14) 0.8567(14) 0.8108(13) 0.054(5) Uani 0.386(13) 1 d P A 2
N1 N 0.5793(4) 0.0082(4) 0.6625(3) 0.0112(7) Uani 1 1 d . . .
N2 N 0.7476(4) -0.0060(3) 0.4877(4) 0.0116(7) Uani 1 1 d . . .
C1 C 0.5738(4) 0.5636(4) 0.2439(4) 0.0093(8) Uani 1 1 d . . .
C2 C 0.6241(4) 0.4890(4) 0.3246(4) 0.0103(8) Uani 1 1 d . . .
H2 H 0.5741 0.4619 0.3921 0.012 Uiso 1 1 calc R . .
C3 C 0.7477(4) 0.4536(4) 0.3069(4) 0.0094(8) Uani 1 1 d . . .
C4 C 0.8197(4) 0.4933(4) 0.2075(4) 0.0091(8) Uani 1 1 d . . .
H4 H 0.9031 0.4691 0.1943 0.011 Uiso 1 1 calc R . .
C5 C 0.7699(4) 0.5688(4) 0.1266(4) 0.0110(8) Uani 1 1 d . . .
C6 C 0.6470(4) 0.6026(4) 0.1449(4) 0.0093(8) Uani 1 1 d . . .
H6 H 0.6127 0.6527 0.0893 0.011 Uiso 1 1 calc R . .
C7 C 0.4905(5) 0.0257(4) 0.7494(4) 0.0161(9) Uani 1 1 d . . .
H7 H 0.4490 0.1000 0.7533 0.019 Uiso 1 1 calc R . .
C8 C 0.4578(5) -0.0620(5) 0.8336(4) 0.0196(10) Uani 1 1 d . . .
H8 H 0.3943 -0.0483 0.8940 0.024 Uiso 1 1 calc R . .
C9 C 0.5188(5) -0.1691(5) 0.8280(5) 0.0207(10) Uani 1 1 d . . .
H9 H 0.4986 -0.2296 0.8855 0.025 Uiso 1 1 calc R . .
C10 C 0.6097(5) -0.1880(5) 0.7381(5) 0.0191(10) Uani 1 1 d . . .
H10 H 0.6521 -0.2618 0.7329 0.023 Uiso 1 1 calc R . .
C11 C 0.6380(4) -0.0971(4) 0.6552(4) 0.0143(9) Uani 1 1 d . . .
C12 C 0.7326(4) -0.1060(4) 0.5554(4) 0.0151(9) Uani 1 1 d . . .
C13 C 0.8023(5) -0.2086(5) 0.5289(5) 0.0199(10) Uani 1 1 d . . .
H13 H 0.7920 -0.2782 0.5774 0.024 Uiso 1 1 calc R . .
C14 C 0.8861(5) -0.2076(5) 0.4314(5) 0.0212(10) Uani 1 1 d . . .
H14 H 0.9353 -0.2759 0.4135 0.025 Uiso 1 1 calc R . .
C15 C 0.8985(5) -0.1075(5) 0.3597(5) 0.0198(10) Uani 1 1 d . . .
H15 H 0.9534 -0.1073 0.2903 0.024 Uiso 1 1 calc R . .
C16 C 0.8284(5) -0.0072(5) 0.3922(5) 0.0178(9) Uani 1 1 d . . .
H16 H 0.8380 0.0634 0.3449 0.021 Uiso 1 1 calc R . .
H2' H 0.274(7) 0.509(6) 0.361(6) 0.031(17) Uiso 1 1 d . . .
H6' H 1.005(6) 0.386(6) 0.385(6) 0.015(16) Uiso 1 1 d . . .
H8' H 0.816(11) 0.761(10) -0.052(11) 0.09(4) Uiso 1 1 d . . .


_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 1.929(3) 2_666 ?
Cu1 O5 1.938(3) . ?
Cu1 N2 1.982(4) . ?
Cu1 N1 2.001(4) . ?
Cu1 O10 2.313(3) . ?
V1 O11 1.624(3) . ?
V1 O10 1.629(3) . ?
V1 O7 1.996(3) 1_556 ?
V1 O9 2.004(3) 2_766 ?
V1 O3 2.009(3) 2_666 ?
P1 O3 1.517(3) . ?
P1 O1 1.519(3) . ?
P1 O2 1.560(3) . ?
P1 C1 1.788(4) . ?
P2 O5 1.499(3) . ?
P2 O4 1.521(3) . ?
P2 O6 1.569(3) . ?
P2 C3 1.796(4) . ?
P3 O9 1.506(3) . ?
P3 O7 1.510(3) . ?
P3 O8 1.565(3) . ?
P3 C5 1.794(4) . ?
P3 H8' 1.85(10) . ?
O1 Cu1 1.929(3) 2_666 ?
O2 H2' 0.81(7) . ?
O3 V1 2.009(3) 2_666 ?
O6 H6' 0.68(6) . ?
O7 V1 1.996(3) 1_554 ?
O8 H8' 0.57(10) . ?
O9 V1 2.004(3) 2_766 ?
N1 C7 1.345(6) . ?
N1 C11 1.345(6) . ?
N2 C16 1.341(6) . ?
N2 C12 1.350(6) . ?
C1 C6 1.391(6) . ?
C1 C2 1.397(6) . ?
C2 C3 1.404(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(6) . ?
C4 C5 1.403(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.476(7) . ?
C12 C13 1.397(6) . ?
C13 C14 1.378(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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 O5 91.62(13) 2_666 . ?
O1 Cu1 N2 171.93(14) 2_666 . ?
O5 Cu1 N2 92.36(14) . . ?
O1 Cu1 N1 93.47(14) 2_666 . ?
O5 Cu1 N1 170.07(14) . . ?
N2 Cu1 N1 81.59(15) . . ?
O1 Cu1 O10 93.25(12) 2_666 . ?
O5 Cu1 O10 100.90(12) . . ?
N2 Cu1 O10 92.89(13) . . ?
N1 Cu1 O10 87.33(13) . . ?
O11 V1 O10 109.21(17) . . ?
O11 V1 O7 136.85(15) . 1_556 ?
O10 V1 O7 113.94(14) . 1_556 ?
O11 V1 O9 91.73(14) . 2_766 ?
O10 V1 O9 97.44(14) . 2_766 ?
O7 V1 O9 82.97(12) 1_556 2_766 ?
O11 V1 O3 92.38(15) . 2_666 ?
O10 V1 O3 97.11(14) . 2_666 ?
O7 V1 O3 82.51(12) 1_556 2_666 ?
O9 V1 O3 162.64(13) 2_766 2_666 ?
O3 P1 O1 113.99(17) . . ?
O3 P1 O2 112.20(19) . . ?
O1 P1 O2 111.18(18) . . ?
O3 P1 C1 108.29(18) . . ?
O1 P1 C1 107.86(18) . . ?
O2 P1 C1 102.54(18) . . ?
O5 P2 O4 115.52(17) . . ?
O5 P2 O6 109.45(18) . . ?
O4 P2 O6 108.96(18) . . ?
O5 P2 C3 109.08(18) . . ?
O4 P2 C3 107.67(18) . . ?
O6 P2 C3 105.71(19) . . ?
O9 P3 O7 114.35(17) . . ?
O9 P3 O8 109.0(2) . . ?
O7 P3 O8 109.85(19) . . ?
O9 P3 C5 109.15(19) . . ?
O7 P3 C5 108.60(18) . . ?
O8 P3 C5 105.5(2) . . ?
O9 P3 H8' 93(3) . . ?
O7 P3 H8' 122(3) . . ?
O8 P3 H8' 17(3) . . ?
C5 P3 H8' 109(3) . . ?
P1 O1 Cu1 128.08(18) . 2_666 ?
P1 O2 H2' 114(5) . . ?
P1 O3 V1 126.91(18) . 2_666 ?
P2 O5 Cu1 137.23(19) . . ?
P2 O6 H6' 115(5) . . ?
P3 O7 V1 141.13(18) . 1_554 ?
P3 O8 H8' 111(10) . . ?
P3 O9 V1 142.88(19) . 2_766 ?
V1 O10 Cu1 131.85(17) . . ?
C7 N1 C11 119.7(4) . . ?
C7 N1 Cu1 126.0(3) . . ?
C11 N1 Cu1 113.6(3) . . ?
C16 N2 C12 119.3(4) . . ?
C16 N2 Cu1 126.3(3) . . ?
C12 N2 Cu1 114.1(3) . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 P1 121.3(3) . . ?
C2 C1 P1 119.0(3) . . ?
C1 C2 C3 120.6(4) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 P2 120.9(3) . . ?
C2 C3 P2 119.7(3) . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 P3 122.7(3) . . ?
C4 C5 P3 117.5(3) . . ?
C5 C6 C1 120.5(4) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
N1 C7 C8 121.7(4) . . ?
N1 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 118.9(5) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C8 C9 C10 119.6(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 119.0(4) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
N1 C11 C10 121.0(4) . . ?
N1 C11 C12 114.6(4) . . ?
C10 C11 C12 124.4(4) . . ?
N2 C12 C13 120.8(4) . . ?
N2 C12 C11 114.7(4) . . ?
C13 C12 C11 124.4(4) . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 120.0(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 118.0(5) . . ?
C14 C15 H15 121.0 . . ?
C16 C15 H15 121.0 . . ?
N2 C16 C15 122.6(4) . . ?
N2 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?

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
O3 P1 O1 Cu1 47.3(3) . . . 2_666 ?
O2 P1 O1 Cu1 -80.7(3) . . . 2_666 ?
C1 P1 O1 Cu1 167.6(2) . . . 2_666 ?
O1 P1 O3 V1 -62.4(3) . . . 2_666 ?
O2 P1 O3 V1 65.1(3) . . . 2_666 ?
C1 P1 O3 V1 177.6(2) . . . 2_666 ?
O4 P2 O5 Cu1 -19.2(3) . . . . ?
O6 P2 O5 Cu1 104.2(3) . . . . ?
C3 P2 O5 Cu1 -140.6(3) . . . . ?
O1 Cu1 O5 P2 75.7(3) 2_666 . . . ?
N2 Cu1 O5 P2 -111.4(3) . . . . ?
N1 Cu1 O5 P2 -163.6(7) . . . . ?
O10 Cu1 O5 P2 -18.0(3) . . . . ?
O9 P3 O7 V1 130.7(3) . . . 1_554 ?
O8 P3 O7 V1 -106.4(3) . . . 1_554 ?
C5 P3 O7 V1 8.6(3) . . . 1_554 ?
O7 P3 O9 V1 -34.1(4) . . . 2_766 ?
O8 P3 O9 V1 -157.4(3) . . . 2_766 ?
C5 P3 O9 V1 87.8(3) . . . 2_766 ?
O11 V1 O10 Cu1 69.8(3) . . . . ?
O7 V1 O10 Cu1 -110.1(2) 1_556 . . . ?
O9 V1 O10 Cu1 164.3(2) 2_766 . . . ?
O3 V1 O10 Cu1 -25.2(2) 2_666 . . . ?
O1 Cu1 O10 V1 33.7(2) 2_666 . . . ?
O5 Cu1 O10 V1 126.0(2) . . . . ?
N2 Cu1 O10 V1 -141.1(2) . . . . ?
N1 Cu1 O10 V1 -59.6(2) . . . . ?
O1 Cu1 N1 C7 -5.3(4) 2_666 . . . ?
O5 Cu1 N1 C7 -125.9(7) . . . . ?
N2 Cu1 N1 C7 -178.9(4) . . . . ?
O10 Cu1 N1 C7 87.8(4) . . . . ?
O1 Cu1 N1 C11 -176.4(3) 2_666 . . . ?
O5 Cu1 N1 C11 63.0(9) . . . . ?
N2 Cu1 N1 C11 10.1(3) . . . . ?
O10 Cu1 N1 C11 -83.3(3) . . . . ?
O1 Cu1 N2 C16 123.9(9) 2_666 . . . ?
O5 Cu1 N2 C16 4.4(4) . . . . ?
N1 Cu1 N2 C16 176.5(4) . . . . ?
O10 Cu1 N2 C16 -96.7(4) . . . . ?
O1 Cu1 N2 C12 -62.1(11) 2_666 . . . ?
O5 Cu1 N2 C12 178.4(3) . . . . ?
N1 Cu1 N2 C12 -9.5(3) . . . . ?
O10 Cu1 N2 C12 77.3(3) . . . . ?
O3 P1 C1 C6 26.5(4) . . . . ?
O1 P1 C1 C6 -97.3(4) . . . . ?
O2 P1 C1 C6 145.3(3) . . . . ?
O3 P1 C1 C2 -157.9(3) . . . . ?
O1 P1 C1 C2 78.3(4) . . . . ?
O2 P1 C1 C2 -39.1(4) . . . . ?
C6 C1 C2 C3 0.3(6) . . . . ?
P1 C1 C2 C3 -175.4(3) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C1 C2 C3 P2 174.8(3) . . . . ?
O5 P2 C3 C4 -126.2(3) . . . . ?
O4 P2 C3 C4 107.7(3) . . . . ?
O6 P2 C3 C4 -8.6(4) . . . . ?
O5 P2 C3 C2 58.8(4) . . . . ?
O4 P2 C3 C2 -67.3(4) . . . . ?
O6 P2 C3 C2 176.4(3) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
P2 C3 C4 C5 -174.5(3) . . . . ?
C3 C4 C5 C6 -0.8(6) . . . . ?
C3 C4 C5 P3 178.3(3) . . . . ?
O9 P3 C5 C6 118.1(4) . . . . ?
O7 P3 C5 C6 -116.6(4) . . . . ?
O8 P3 C5 C6 1.1(4) . . . . ?
O9 P3 C5 C4 -61.0(4) . . . . ?
O7 P3 C5 C4 64.3(4) . . . . ?
O8 P3 C5 C4 -178.0(3) . . . . ?
C4 C5 C6 C1 0.9(6) . . . . ?
P3 C5 C6 C1 -178.2(3) . . . . ?
C2 C1 C6 C5 -0.6(6) . . . . ?
P1 C1 C6 C5 175.0(3) . . . . ?
C11 N1 C7 C8 0.5(6) . . . . ?
Cu1 N1 C7 C8 -170.1(3) . . . . ?
N1 C7 C8 C9 0.4(7) . . . . ?
C7 C8 C9 C10 -0.8(7) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C7 N1 C11 C10 -1.0(6) . . . . ?
Cu1 N1 C11 C10 170.7(3) . . . . ?
C7 N1 C11 C12 179.5(4) . . . . ?
Cu1 N1 C11 C12 -8.8(5) . . . . ?
C9 C10 C11 N1 0.5(7) . . . . ?
C9 C10 C11 C12 -180.0(4) . . . . ?
C16 N2 C12 C13 1.3(6) . . . . ?
Cu1 N2 C12 C13 -173.1(3) . . . . ?
C16 N2 C12 C11 -178.1(4) . . . . ?
Cu1 N2 C12 C11 7.5(5) . . . . ?
N1 C11 C12 N2 1.0(5) . . . . ?
C10 C11 C12 N2 -178.6(4) . . . . ?
N1 C11 C12 C13 -178.4(4) . . . . ?
C10 C11 C12 C13 2.1(7) . . . . ?
N2 C12 C13 C14 -0.6(7) . . . . ?
C11 C12 C13 C14 178.7(4) . . . . ?
C12 C13 C14 C15 -1.2(7) . . . . ?
C13 C14 C15 C16 2.3(7) . . . . ?
C12 N2 C16 C15 -0.2(7) . . . . ?
Cu1 N2 C16 C15 173.5(3) . . . . ?
C14 C15 C16 N2 -1.6(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.147

#[{Cu(bipy)}2VV3O7{(O3P)2C6H3(PO3H}] 13
data_[{Cu(bipy)}2VV3O7{(O3P)2C6H3(PO3H}]13
_database_code_depnum_ccdc_archive 'CCDC 734634'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 Cu2 N4 O16 P3 V3'
_chemical_formula_sum            'C26 H20 Cu2 N4 O16 P3 V3'
_chemical_formula_weight         1017.27

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'
V V 0.3005 0.5294 '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   Pbca
_symmetry_space_group_name_Hall  -P2ac2ab

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

_cell_length_a                   8.8764(6)
_cell_length_b                   17.0724(11)
_cell_length_c                   43.440(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6583.0(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3563
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      22.84

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4032
_exptl_absorpt_coefficient_mu    2.321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7222
_exptl_absorpt_correction_T_max  0.8361
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            40634
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         23.01
_reflns_number_total             4592
_reflns_number_gt                3913
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0370P)²+57.4397P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         4592
_refine_ls_number_parameters     487
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0622
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_restrained_S_all      1.275
_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 0.44053(10) 0.43920(5) 0.17182(2) 0.0108(2) Uani 1 1 d . . .
Cu2 Cu 0.09561(10) 0.44349(5) 0.05176(2) 0.0118(2) Uani 1 1 d . . .
V1 V 0.56058(16) 0.23836(8) 0.18390(3) 0.0187(4) Uani 1 1 d . . .
V2 V 0.49620(14) 0.38004(7) 0.09895(3) 0.0069(3) Uani 1 1 d . . .
V3 V 0.00873(14) 0.51344(7) 0.11956(3) 0.0072(3) Uani 1 1 d . . .
P1 P 0.6432(2) 0.53666(11) 0.12602(5) 0.0096(5) Uani 1 1 d . . .
P2 P 0.1075(2) 0.69833(11) 0.11948(5) 0.0105(5) Uani 1 1 d . . .
P3 P 0.6357(2) 0.85569(11) 0.09425(5) 0.0081(4) Uani 1 1 d . . .
O1 O 0.5981(5) 0.4828(3) 0.09932(12) 0.0110(12) Uani 1 1 d U . .
O2 O 0.5988(6) 0.5053(3) 0.15706(12) 0.0142(12) Uani 1 1 d . . .
O3 O 0.8091(6) 0.5580(3) 0.12379(13) 0.0165(13) Uani 1 1 d U . .
O4 O 0.0703(6) 0.7037(3) 0.15352(13) 0.0216(14) Uani 1 1 d . . .
O5 O 0.0558(6) 0.6213(3) 0.10634(12) 0.0137(12) Uani 1 1 d . . .
O6 O 0.0467(5) 0.7656(3) 0.10129(13) 0.0142(12) Uani 1 1 d U . .
O7 O 0.5714(6) 0.8795(3) 0.06338(12) 0.0137(12) Uani 1 1 d . . .
O8 O 0.6010(6) 0.9139(3) 0.11991(12) 0.0115(12) Uani 1 1 d . . .
O9 O 0.8024(6) 0.8377(3) 0.09146(12) 0.0115(12) Uani 1 1 d . . .
O10 O 0.7303(6) 0.1848(3) 0.18645(14) 0.0200(14) Uani 1 1 d . . .
O11 O 0.4660(8) 0.2293(4) 0.21577(14) 0.0368(17) Uani 1 1 d . . .
O12 O 0.5975(6) 0.3322(3) 0.17879(14) 0.0254(15) Uani 1 1 d . . .
O13 O 0.3921(6) 0.4024(3) 0.13000(11) 0.0109(12) Uani 1 1 d . . .
O14 O 0.3966(6) 0.3928(3) 0.06859(12) 0.0140(12) Uani 1 1 d . . .
O15 O 0.1276(6) 0.4801(3) 0.09226(12) 0.0129(12) Uani 1 1 d . . .
O16 O 0.0965(6) 0.5089(3) 0.15138(13) 0.0163(13) Uani 1 1 d . . .
N1 N 0.4564(8) 0.4814(4) 0.21429(16) 0.0194(17) Uani 1 1 d . . .
N2 N 0.2692(7) 0.3829(4) 0.19098(15) 0.0149(15) Uani 1 1 d . . .
N3 N 0.2345(7) 0.5202(4) 0.03246(14) 0.0135(15) Uani 1 1 d . . .
N4 N 0.0905(7) 0.4019(4) 0.00919(15) 0.0160(16) Uani 1 1 d . . .
C1 C 0.5461(8) 0.6282(4) 0.11996(17) 0.0083(16) Uani 1 1 d . . .
C2 C 0.3903(9) 0.6311(5) 0.12259(18) 0.0152(18) Uani 1 1 d . . .
H2 H 0.3374 0.5856 0.1290 0.018 Uiso 1 1 calc R . .
C3 C 0.3107(8) 0.6981(4) 0.11622(16) 0.0038(15) Uani 1 1 d U . .
C4 C 0.3873(8) 0.7646(4) 0.10637(17) 0.0105(17) Uani 1 1 d U . .
H4 H 0.3324 0.8100 0.1006 0.013 Uiso 1 1 calc R . .
C5 C 0.5438(8) 0.7650(4) 0.10497(17) 0.0083(17) Uani 1 1 d . . .
C6 C 0.6226(9) 0.6973(4) 0.11197(17) 0.0113(17) Uani 1 1 d . . .
H6 H 0.7296 0.6976 0.1114 0.014 Uiso 1 1 calc R . .
C7 C 0.5472(9) 0.5402(5) 0.2237(2) 0.021(2) Uani 1 1 d . . .
H7 H 0.6076 0.5668 0.2090 0.025 Uiso 1 1 calc R . .
C8 C 0.5544(11) 0.5625(6) 0.2540(2) 0.037(3) Uani 1 1 d . . .
H8 H 0.6165 0.6052 0.2600 0.044 Uiso 1 1 calc R . .
C9 C 0.4721(12) 0.5232(6) 0.2756(2) 0.038(3) Uani 1 1 d . . .
H9 H 0.4776 0.5379 0.2966 0.045 Uiso 1 1 calc R . .
C10 C 0.3806(12) 0.4617(6) 0.2666(2) 0.035(3) Uani 1 1 d . . .
H10 H 0.3242 0.4328 0.2814 0.042 Uiso 1 1 calc R . .
C11 C 0.3738(10) 0.4433(6) 0.2355(2) 0.026(2) Uani 1 1 d . . .
C12 C 0.2694(9) 0.3843(5) 0.22205(18) 0.0164(19) Uani 1 1 d . . .
C13 C 0.1721(11) 0.3364(5) 0.2380(2) 0.028(2) Uani 1 1 d . . .
H13 H 0.1731 0.3364 0.2599 0.033 Uiso 1 1 calc R . .
C14 C 0.0743(11) 0.2891(6) 0.2225(2) 0.034(3) Uani 1 1 d . . .
H14 H 0.0087 0.2552 0.2335 0.040 Uiso 1 1 calc R . .
C15 C 0.0711(11) 0.2908(5) 0.1908(2) 0.027(2) Uani 1 1 d . . .
H15 H 0.0015 0.2595 0.1796 0.033 Uiso 1 1 calc R . .
C16 C 0.1705(9) 0.3385(5) 0.1759(2) 0.021(2) Uani 1 1 d . . .
H16 H 0.1692 0.3401 0.1540 0.025 Uiso 1 1 calc R . .
C17 C 0.3021(9) 0.5783(5) 0.0473(2) 0.019(2) Uani 1 1 d . . .
H17 H 0.2824 0.5859 0.0686 0.023 Uiso 1 1 calc R . .
C18 C 0.4000(10) 0.6278(5) 0.0324(2) 0.027(2) Uani 1 1 d . . .
H18 H 0.4482 0.6689 0.0433 0.032 Uiso 1 1 calc R . .
C19 C 0.4279(10) 0.6171(5) 0.0015(2) 0.028(2) Uani 1 1 d . . .
H19 H 0.4959 0.6509 -0.0089 0.033 Uiso 1 1 calc R . .
C20 C 0.3572(10) 0.5575(6) -0.0143(2) 0.028(2) Uani 1 1 d . . .
H20 H 0.3738 0.5499 -0.0357 0.034 Uiso 1 1 calc R . .
C21 C 0.2616(9) 0.5093(5) 0.00196(19) 0.0165(19) Uani 1 1 d . . .
C22 C 0.1814(9) 0.4398(5) -0.0111(2) 0.0183(19) Uani 1 1 d . . .
C23 C 0.1995(10) 0.4136(6) -0.04100(19) 0.026(2) Uani 1 1 d . . .
H23 H 0.2634 0.4407 -0.0549 0.031 Uiso 1 1 calc R . .
C24 C 0.1234(10) 0.3477(6) -0.0500(2) 0.026(2) Uani 1 1 d . . .
H24 H 0.1384 0.3269 -0.0701 0.031 Uiso 1 1 calc R . .
C25 C 0.0259(10) 0.3120(6) -0.0302(2) 0.027(2) Uani 1 1 d . . .
H25 H -0.0321 0.2683 -0.0368 0.032 Uiso 1 1 calc R . .
C26 C 0.0126(10) 0.3398(5) -0.0009(2) 0.023(2) Uani 1 1 d . . .
H26 H -0.0543 0.3142 0.0129 0.028 Uiso 1 1 calc R . .


_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 O2 1.912(5) . ?
Cu1 O13 1.970(5) . ?
Cu1 N2 1.982(6) . ?
Cu1 N1 1.986(7) . ?
Cu1 O12 2.317(6) . ?
Cu2 O15 1.888(5) . ?
Cu2 O7 1.909(5) 8_655 ?
Cu2 N4 1.982(6) . ?
Cu2 N3 1.985(6) . ?
V1 O11 1.627(7) . ?
V1 O12 1.651(6) . ?
V1 O10 1.766(5) . ?
V1 O4 1.855(6) 8_655 ?
V2 O14 1.603(5) . ?
V2 O13 1.679(5) . ?
V2 O9 1.956(5) 8_755 ?
V2 O1 1.974(5) . ?
V2 O6 1.993(5) 8_655 ?
V3 O16 1.588(6) . ?
V3 O15 1.686(5) . ?
V3 O3 1.937(5) 1_455 ?
V3 O8 1.959(5) 8_655 ?
V3 O5 1.974(5) . ?
P1 O2 1.504(6) . ?
P1 O3 1.520(6) . ?
P1 O1 1.533(6) . ?
P1 C1 1.804(8) . ?
P2 O6 1.495(6) . ?
P2 O5 1.505(6) . ?
P2 O4 1.518(6) . ?
P2 C3 1.809(7) . ?
P3 O7 1.513(6) . ?
P3 O9 1.516(5) . ?
P3 O8 1.525(5) . ?
P3 C5 1.811(7) . ?
O3 V3 1.937(5) 1_655 ?
O4 V1 1.855(6) 8_665 ?
O6 V2 1.993(5) 8_665 ?
O7 Cu2 1.909(5) 8_665 ?
O8 V3 1.959(5) 8_665 ?
O9 V2 1.956(5) 8_765 ?
N1 C11 1.344(11) . ?
N1 C7 1.352(11) . ?
N2 C16 1.331(11) . ?
N2 C12 1.350(10) . ?
N3 C17 1.326(10) . ?
N3 C21 1.359(10) . ?
N4 C26 1.339(11) . ?
N4 C22 1.359(10) . ?
C1 C2 1.389(11) . ?
C1 C6 1.404(11) . ?
C2 C3 1.372(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(10) . ?
C4 C5 1.390(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.372(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.364(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.488(13) . ?
C12 C13 1.376(12) . ?
C13 C14 1.364(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.374(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(12) . ?
C20 H20 0.9500 . ?
C21 C22 1.496(12) . ?
C22 C23 1.382(12) . ?
C23 C24 1.371(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.364(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.365(12) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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
O2 Cu1 O13 92.3(2) . . ?
O2 Cu1 N2 172.0(3) . . ?
O13 Cu1 N2 93.7(2) . . ?
O2 Cu1 N1 92.6(3) . . ?
O13 Cu1 N1 171.2(2) . . ?
N2 Cu1 N1 80.8(3) . . ?
O2 Cu1 O12 93.8(2) . . ?
O13 Cu1 O12 90.0(2) . . ?
N2 Cu1 O12 91.4(2) . . ?
N1 Cu1 O12 97.0(2) . . ?
O15 Cu2 O7 93.4(2) . 8_655 ?
O15 Cu2 N4 172.5(3) . . ?
O7 Cu2 N4 91.4(3) 8_655 . ?
O15 Cu2 N3 94.7(2) . . ?
O7 Cu2 N3 166.3(2) 8_655 . ?
N4 Cu2 N3 81.7(3) . . ?
O11 V1 O12 108.0(3) . . ?
O11 V1 O10 109.7(3) . . ?
O12 V1 O10 110.0(3) . . ?
O11 V1 O4 104.6(3) . 8_655 ?
O12 V1 O4 109.8(3) . 8_655 ?
O10 V1 O4 114.5(3) . 8_655 ?
O14 V2 O13 109.1(3) . . ?
O14 V2 O9 114.7(2) . 8_755 ?
O13 V2 O9 136.1(2) . 8_755 ?
O14 V2 O1 98.0(2) . . ?
O13 V2 O1 92.5(2) . . ?
O9 V2 O1 84.9(2) 8_755 . ?
O14 V2 O6 94.0(2) . 8_655 ?
O13 V2 O6 94.4(2) . 8_655 ?
O9 V2 O6 79.7(2) 8_755 8_655 ?
O1 V2 O6 163.4(2) . 8_655 ?
O16 V3 O15 106.8(3) . . ?
O16 V3 O3 112.7(3) . 1_455 ?
O15 V3 O3 140.5(3) . 1_455 ?
O16 V3 O8 101.3(2) . 8_655 ?
O15 V3 O8 91.3(2) . 8_655 ?
O3 V3 O8 83.4(2) 1_455 8_655 ?
O16 V3 O5 101.2(2) . . ?
O15 V3 O5 88.8(2) . . ?
O3 V3 O5 81.6(2) 1_455 . ?
O8 V3 O5 156.5(2) 8_655 . ?
O2 P1 O3 113.3(3) . . ?
O2 P1 O1 113.4(3) . . ?
O3 P1 O1 110.4(3) . . ?
O2 P1 C1 108.3(3) . . ?
O3 P1 C1 104.2(3) . . ?
O1 P1 C1 106.5(3) . . ?
O6 P2 O5 111.1(3) . . ?
O6 P2 O4 112.9(3) . . ?
O5 P2 O4 110.9(3) . . ?
O6 P2 C3 108.7(3) . . ?
O5 P2 C3 105.8(3) . . ?
O4 P2 C3 107.1(3) . . ?
O7 P3 O9 110.6(3) . . ?
O7 P3 O8 113.4(3) . . ?
O9 P3 O8 112.8(3) . . ?
O7 P3 C5 106.7(3) . . ?
O9 P3 C5 106.7(3) . . ?
O8 P3 C5 106.2(3) . . ?
P1 O1 V2 131.2(3) . . ?
P1 O2 Cu1 134.7(3) . . ?
P1 O3 V3 143.0(3) . 1_655 ?
P2 O4 V1 148.1(4) . 8_665 ?
P2 O5 V3 140.3(3) . . ?
P2 O6 V2 148.1(4) . 8_665 ?
P3 O7 Cu2 132.9(3) . 8_665 ?
P3 O8 V3 131.3(3) . 8_665 ?
P3 O9 V2 143.5(3) . 8_765 ?
V1 O12 Cu1 131.5(3) . . ?
V2 O13 Cu1 133.9(3) . . ?
V3 O15 Cu2 132.3(3) . . ?
C11 N1 C7 118.5(8) . . ?
C11 N1 Cu1 115.0(6) . . ?
C7 N1 Cu1 126.4(6) . . ?
C16 N2 C12 120.2(7) . . ?
C16 N2 Cu1 125.0(6) . . ?
C12 N2 Cu1 114.2(5) . . ?
C17 N3 C21 119.8(7) . . ?
C17 N3 Cu2 124.7(5) . . ?
C21 N3 Cu2 115.5(5) . . ?
C26 N4 C22 118.1(7) . . ?
C26 N4 Cu2 126.9(6) . . ?
C22 N4 Cu2 115.0(5) . . ?
C2 C1 C6 118.2(7) . . ?
C2 C1 P1 119.6(6) . . ?
C6 C1 P1 122.2(6) . . ?
C3 C2 C1 121.7(7) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 119.4(7) . . ?
C2 C3 P2 120.0(6) . . ?
C4 C3 P2 120.6(5) . . ?
C5 C4 C3 120.4(7) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 119.4(7) . . ?
C6 C5 P3 122.9(6) . . ?
C4 C5 P3 117.7(6) . . ?
C5 C6 C1 120.7(7) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
N1 C7 C8 121.7(9) . . ?
N1 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 119.8(10) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.8(10) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 118.0(10) . . ?
C9 C10 H10 121.0 . . ?
C11 C10 H10 121.0 . . ?
N1 C11 C10 122.3(9) . . ?
N1 C11 C12 113.5(7) . . ?
C10 C11 C12 124.1(9) . . ?
N2 C12 C13 119.5(8) . . ?
N2 C12 C11 113.9(7) . . ?
C13 C12 C11 126.5(8) . . ?
C14 C13 C12 120.2(9) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.6(9) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 118.3(9) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
N2 C16 C15 122.1(8) . . ?
N2 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
N3 C17 C18 121.1(8) . . ?
N3 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 119.5(9) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C18 C19 C20 120.1(8) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 117.7(9) . . ?
C21 C20 H20 121.1 . . ?
C19 C20 H20 121.1 . . ?
N3 C21 C20 121.8(8) . . ?
N3 C21 C22 113.3(7) . . ?
C20 C21 C22 124.9(8) . . ?
N4 C22 C23 121.7(8) . . ?
N4 C22 C21 114.4(7) . . ?
C23 C22 C21 123.9(8) . . ?
C24 C23 C22 118.5(8) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C25 C24 C23 119.9(8) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 119.2(9) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
N4 C26 C25 122.4(9) . . ?
N4 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?

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
O2 P1 O1 V2 -1.2(5) . . . . ?
O3 P1 O1 V2 127.2(4) . . . . ?
C1 P1 O1 V2 -120.2(4) . . . . ?
O14 V2 O1 P1 142.8(4) . . . . ?
O13 V2 O1 P1 33.2(4) . . . . ?
O9 V2 O1 P1 -102.9(4) 8_755 . . . ?
O6 V2 O1 P1 -81.3(9) 8_655 . . . ?
O3 P1 O2 Cu1 -155.9(4) . . . . ?
O1 P1 O2 Cu1 -29.0(6) . . . . ?
C1 P1 O2 Cu1 89.0(5) . . . . ?
O13 Cu1 O2 P1 15.6(5) . . . . ?
N2 Cu1 O2 P1 -123.2(17) . . . . ?
N1 Cu1 O2 P1 -157.0(5) . . . . ?
O12 Cu1 O2 P1 105.8(5) . . . . ?
O2 P1 O3 V3 76.3(7) . . . 1_655 ?
O1 P1 O3 V3 -52.1(7) . . . 1_655 ?
C1 P1 O3 V3 -166.2(6) . . . 1_655 ?
O6 P2 O4 V1 29.1(8) . . . 8_665 ?
O5 P2 O4 V1 -96.4(7) . . . 8_665 ?
C3 P2 O4 V1 148.7(7) . . . 8_665 ?
O6 P2 O5 V3 -150.2(5) . . . . ?
O4 P2 O5 V3 -23.7(6) . . . . ?
C3 P2 O5 V3 92.0(5) . . . . ?
O16 V3 O5 P2 -20.5(6) . . . . ?
O15 V3 O5 P2 -127.3(5) . . . . ?
O3 V3 O5 P2 91.1(5) 1_455 . . . ?
O8 V3 O5 P2 142.2(5) 8_655 . . . ?
O5 P2 O6 V2 163.6(6) . . . 8_665 ?
O4 P2 O6 V2 38.3(7) . . . 8_665 ?
C3 P2 O6 V2 -80.4(7) . . . 8_665 ?
O9 P3 O7 Cu2 -153.4(4) . . . 8_665 ?
O8 P3 O7 Cu2 -25.6(5) . . . 8_665 ?
C5 P3 O7 Cu2 91.0(5) . . . 8_665 ?
O7 P3 O8 V3 -0.9(5) . . . 8_665 ?
O9 P3 O8 V3 125.8(4) . . . 8_665 ?
C5 P3 O8 V3 -117.8(4) . . . 8_665 ?
O7 P3 O9 V2 101.4(6) . . . 8_765 ?
O8 P3 O9 V2 -26.7(7) . . . 8_765 ?
C5 P3 O9 V2 -142.9(5) . . . 8_765 ?
O11 V1 O12 Cu1 -62.4(5) . . . . ?
O10 V1 O12 Cu1 177.8(4) . . . . ?
O4 V1 O12 Cu1 51.0(5) 8_655 . . . ?
O2 Cu1 O12 V1 -164.4(4) . . . . ?
O13 Cu1 O12 V1 -72.1(5) . . . . ?
N2 Cu1 O12 V1 21.6(5) . . . . ?
N1 Cu1 O12 V1 102.5(5) . . . . ?
O14 V2 O13 Cu1 -153.5(4) . . . . ?
O9 V2 O13 Cu1 31.1(6) 8_755 . . . ?
O1 V2 O13 Cu1 -54.2(4) . . . . ?
O6 V2 O13 Cu1 110.7(4) 8_655 . . . ?
O2 Cu1 O13 V2 38.1(4) . . . . ?
N2 Cu1 O13 V2 -147.2(4) . . . . ?
N1 Cu1 O13 V2 161.5(15) . . . . ?
O12 Cu1 O13 V2 -55.8(4) . . . . ?
O16 V3 O15 Cu2 162.1(4) . . . . ?
O3 V3 O15 Cu2 -21.3(6) 1_455 . . . ?
O8 V3 O15 Cu2 59.9(4) 8_655 . . . ?
O5 V3 O15 Cu2 -96.5(4) . . . . ?
O7 Cu2 O15 V3 -45.4(4) 8_655 . . . ?
N4 Cu2 O15 V3 -175.2(17) . . . . ?
N3 Cu2 O15 V3 123.6(4) . . . . ?
O2 Cu1 N1 C11 -171.8(6) . . . . ?
O13 Cu1 N1 C11 64.8(19) . . . . ?
N2 Cu1 N1 C11 12.7(6) . . . . ?
O12 Cu1 N1 C11 -77.6(6) . . . . ?
O2 Cu1 N1 C7 4.1(7) . . . . ?
O13 Cu1 N1 C7 -119.3(16) . . . . ?
N2 Cu1 N1 C7 -171.4(7) . . . . ?
O12 Cu1 N1 C7 98.3(6) . . . . ?
O2 Cu1 N2 C16 139.1(16) . . . . ?
O13 Cu1 N2 C16 0.3(7) . . . . ?
N1 Cu1 N2 C16 173.4(7) . . . . ?
O12 Cu1 N2 C16 -89.8(7) . . . . ?
O2 Cu1 N2 C12 -49(2) . . . . ?
O13 Cu1 N2 C12 172.1(5) . . . . ?
N1 Cu1 N2 C12 -14.9(5) . . . . ?
O12 Cu1 N2 C12 81.9(6) . . . . ?
O15 Cu2 N3 C17 -6.1(7) . . . . ?
O7 Cu2 N3 C17 120.1(11) 8_655 . . . ?
N4 Cu2 N3 C17 -179.5(7) . . . . ?
O15 Cu2 N3 C21 172.5(5) . . . . ?
O7 Cu2 N3 C21 -61.3(13) 8_655 . . . ?
N4 Cu2 N3 C21 -0.9(5) . . . . ?
O15 Cu2 N4 C26 117.9(19) . . . . ?
O7 Cu2 N4 C26 -12.1(7) 8_655 . . . ?
N3 Cu2 N4 C26 179.8(7) . . . . ?
O15 Cu2 N4 C22 -59(2) . . . . ?
O7 Cu2 N4 C22 170.7(6) 8_655 . . . ?
N3 Cu2 N4 C22 2.6(6) . . . . ?
O2 P1 C1 C2 -54.7(7) . . . . ?
O3 P1 C1 C2 -175.6(6) . . . . ?
O1 P1 C1 C2 67.6(7) . . . . ?
O2 P1 C1 C6 126.7(6) . . . . ?
O3 P1 C1 C6 5.7(7) . . . . ?
O1 P1 C1 C6 -111.0(6) . . . . ?
C6 C1 C2 C3 3.1(12) . . . . ?
P1 C1 C2 C3 -175.6(6) . . . . ?
C1 C2 C3 C4 1.1(12) . . . . ?
C1 C2 C3 P2 179.1(6) . . . . ?
O6 P2 C3 C2 -160.3(6) . . . . ?
O5 P2 C3 C2 -40.9(7) . . . . ?
O4 P2 C3 C2 77.4(7) . . . . ?
O6 P2 C3 C4 17.7(7) . . . . ?
O5 P2 C3 C4 137.1(6) . . . . ?
O4 P2 C3 C4 -104.6(6) . . . . ?
C2 C3 C4 C5 -4.3(11) . . . . ?
P2 C3 C4 C5 177.7(6) . . . . ?
C3 C4 C5 C6 3.3(11) . . . . ?
C3 C4 C5 P3 -176.2(5) . . . . ?
O7 P3 C5 C6 124.3(6) . . . . ?
O9 P3 C5 C6 6.0(7) . . . . ?
O8 P3 C5 C6 -114.5(6) . . . . ?
O7 P3 C5 C4 -56.3(7) . . . . ?
O9 P3 C5 C4 -174.5(6) . . . . ?
O8 P3 C5 C4 65.0(7) . . . . ?
C4 C5 C6 C1 1.0(11) . . . . ?
P3 C5 C6 C1 -179.6(6) . . . . ?
C2 C1 C6 C5 -4.1(11) . . . . ?
P1 C1 C6 C5 174.6(6) . . . . ?
C11 N1 C7 C8 -1.2(12) . . . . ?
Cu1 N1 C7 C8 -177.0(6) . . . . ?
N1 C7 C8 C9 2.1(13) . . . . ?
C7 C8 C9 C10 -0.8(14) . . . . ?
C8 C9 C10 C11 -1.4(14) . . . . ?
C7 N1 C11 C10 -1.1(12) . . . . ?
Cu1 N1 C11 C10 175.1(7) . . . . ?
C7 N1 C11 C12 175.3(7) . . . . ?
Cu1 N1 C11 C12 -8.4(9) . . . . ?
C9 C10 C11 N1 2.4(13) . . . . ?
C9 C10 C11 C12 -173.7(8) . . . . ?
C16 N2 C12 C13 3.3(12) . . . . ?
Cu1 N2 C12 C13 -168.8(6) . . . . ?
C16 N2 C12 C11 -173.3(7) . . . . ?
Cu1 N2 C12 C11 14.5(8) . . . . ?
N1 C11 C12 N2 -4.0(10) . . . . ?
C10 C11 C12 N2 172.4(8) . . . . ?
N1 C11 C12 C13 179.6(8) . . . . ?
C10 C11 C12 C13 -4.0(14) . . . . ?
N2 C12 C13 C14 -1.3(13) . . . . ?
C11 C12 C13 C14 174.9(8) . . . . ?
C12 C13 C14 C15 -1.4(14) . . . . ?
C13 C14 C15 C16 2.0(14) . . . . ?
C12 N2 C16 C15 -2.7(12) . . . . ?
Cu1 N2 C16 C15 168.5(6) . . . . ?
C14 C15 C16 N2 0.0(13) . . . . ?
C21 N3 C17 C18 -0.3(12) . . . . ?
Cu2 N3 C17 C18 178.2(6) . . . . ?
N3 C17 C18 C19 0.4(13) . . . . ?
C17 C18 C19 C20 0.3(14) . . . . ?
C18 C19 C20 C21 -1.1(13) . . . . ?
C17 N3 C21 C20 -0.5(12) . . . . ?
Cu2 N3 C21 C20 -179.2(6) . . . . ?
C17 N3 C21 C22 177.9(7) . . . . ?
Cu2 N3 C21 C22 -0.7(8) . . . . ?
C19 C20 C21 N3 1.2(13) . . . . ?
C19 C20 C21 C22 -177.1(8) . . . . ?
C26 N4 C22 C23 -3.0(12) . . . . ?
Cu2 N4 C22 C23 174.5(6) . . . . ?
C26 N4 C22 C21 178.9(7) . . . . ?
Cu2 N4 C22 C21 -3.6(9) . . . . ?
N3 C21 C22 N4 2.9(10) . . . . ?
C20 C21 C22 N4 -178.8(8) . . . . ?
N3 C21 C22 C23 -175.3(8) . . . . ?
C20 C21 C22 C23 3.1(13) . . . . ?
N4 C22 C23 C24 0.0(12) . . . . ?
C21 C22 C23 C24 178.0(8) . . . . ?
C22 C23 C24 C25 3.6(13) . . . . ?
C23 C24 C25 C26 -4.1(14) . . . . ?
C22 N4 C26 C25 2.5(13) . . . . ?
Cu2 N4 C26 C25 -174.7(7) . . . . ?
C24 C25 C26 N4 1.0(14) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.141

data_14
_database_code_depnum_ccdc_archive 'CCDC 734635'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H11 Cu1 N2 O15.50 P3 V3, (O0.50)'
_chemical_formula_sum            'C18 H14 Cu N2 O16 P3 V3'
_chemical_formula_weight         823.58

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'
V V 0.3005 0.5294 '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
_symmetry_space_group_name_Hall  -P2ybc

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                   16.244(2)
_cell_length_b                   7.2007(9)
_cell_length_c                   22.401(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.056(2)
_cell_angle_gamma                90.00
_cell_volume                     2541.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    6221
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.25

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1628
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5622
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            18971
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4469
_reflns_number_gt                4330
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0054P)²+36.9760P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         4469
_refine_ls_number_parameters     406
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0781
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_restrained_S_all      1.340
_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 0.69291(5) 1.17342(12) 0.65694(4) 0.0086(2) Uani 1 1 d . . .
V1A V 1.1238(11) 0.340(4) 0.4791(6) 0.012(3) Uani 0.38(5) 1 d P . 1
V1B V 1.0977(12) 0.3861(11) 0.4855(2) 0.009(2) Uani 0.62(5) 1 d PU . 2
V2 V 1.19296(8) 0.66316(18) 0.59572(5) 0.0099(3) Uani 1 1 d . . .
V3 V 0.71796(8) 0.68210(17) 0.67280(6) 0.0089(3) Uani 1 1 d . . .
P1 P 1.15294(11) 0.9005(3) 0.87137(8) 0.0076(4) Uani 1 1 d . . .
P2 P 0.80553(11) 0.9596(3) 0.77494(8) 0.0067(4) Uani 1 1 d . . .
P3 P 1.02243(12) 0.8762(3) 0.62095(9) 0.0104(4) Uani 1 1 d . . .
O1 O 1.1245(3) 0.9176(7) 0.9308(2) 0.0110(11) Uani 1 1 d . . .
O2 O 1.2061(3) 0.7301(7) 0.8712(2) 0.0094(10) Uani 1 1 d . . .
O3 O 1.2006(3) 1.0803(8) 0.8615(3) 0.0160(12) Uani 1 1 d . . .
O4 O 0.8145(3) 0.9747(7) 0.8436(2) 0.0118(11) Uani 1 1 d . . .
O5 O 0.7609(3) 0.7717(7) 0.7529(2) 0.0092(10) Uani 1 1 d . . .
O6 O 0.7595(3) 1.1220(7) 0.7399(2) 0.0100(10) Uani 1 1 d . . .
O7 O 1.1137(3) 0.8163(8) 0.6269(2) 0.0191(12) Uani 1 1 d . . .
O8 O 0.9592(4) 0.7330(8) 0.5899(3) 0.0260(14) Uani 1 1 d . . .
O9 O 1.0037(4) 1.0668(8) 0.5885(3) 0.0236(13) Uani 1 1 d . . .
O10 O 1.1070(5) 0.1871(9) 0.5289(3) 0.0409(18) Uani 1 1 d . . .
O11A O 1.1943(12) 0.203(3) 0.4602(11) 0.089(7) Uani 0.50 1 d P . .
O11B O 1.0000 0.5000 0.5000 0.061(4) Uani 1 2 d S . .
O12 O 1.1956(3) 0.5000(7) 0.5428(2) 0.0157(12) Uani 1 1 d . . .
O13 O 1.2865(3) 0.7372(8) 0.6215(2) 0.0194(12) Uani 1 1 d . . .
O14 O 0.6453(3) 0.5290(8) 0.6721(2) 0.0184(12) Uani 1 1 d . . .
O15 O 0.6771(3) 0.8563(7) 0.6296(2) 0.0161(12) Uani 1 1 d . . .
O40 O 1.1578(4) 0.8384(8) 0.5216(2) 0.0209(13) Uani 1 1 d . . .
N1 N 0.6168(4) 1.2220(8) 0.5733(3) 0.0076(12) Uani 1 1 d . . .
N2 N 0.5815(4) 1.1451(8) 0.6810(3) 0.0086(12) Uani 1 1 d U . .
C1 C 1.0614(4) 0.9014(10) 0.8072(3) 0.0091(14) Uani 1 1 d . . .
C2 C 1.0750(4) 0.8946(10) 0.7485(3) 0.0101(15) Uani 1 1 d . . .
H2 H 1.1310 0.8850 0.7431 0.012 Uiso 1 1 calc R . .
C3 C 1.0056(5) 0.9020(10) 0.6970(3) 0.0093(15) Uani 1 1 d . . .
C4 C 0.9249(4) 0.9247(9) 0.7052(3) 0.0075(14) Uani 1 1 d . . .
H4 H 0.8781 0.9337 0.6704 0.009 Uiso 1 1 calc R . .
C5 C 0.9115(4) 0.9343(10) 0.7641(3) 0.0076(14) Uani 1 1 d U . .
C6 C 0.9800(4) 0.9183(9) 0.8146(3) 0.0065(14) Uani 1 1 d U . .
H6 H 0.9706 0.9189 0.8548 0.008 Uiso 1 1 calc R . .
C7 C 0.6366(5) 1.2594(11) 0.5209(4) 0.0151(16) Uani 1 1 d . . .
H7 H 0.6947 1.2694 0.5204 0.018 Uiso 1 1 calc R . .
C8 C 0.5746(5) 1.2847(11) 0.4659(4) 0.0169(17) Uani 1 1 d . . .
H8 H 0.5908 1.3094 0.4287 0.020 Uiso 1 1 calc R . .
C9 C 0.4912(5) 1.2737(12) 0.4661(4) 0.0209(18) Uani 1 1 d . . .
H9 H 0.4487 1.2935 0.4291 0.025 Uiso 1 1 calc R . .
C10 C 0.4681(5) 1.2337(11) 0.5203(4) 0.0149(16) Uani 1 1 d . . .
C11 C 0.5325(4) 1.2112(9) 0.5742(3) 0.0072(14) Uani 1 1 d U . .
C12 C 0.3815(5) 1.2177(12) 0.5270(4) 0.0224(19) Uani 1 1 d . . .
H12 H 0.3360 1.2323 0.4916 0.027 Uiso 1 1 calc R . .
C13 C 0.3637(5) 1.1832(13) 0.5814(4) 0.0211(19) Uani 1 1 d . . .
H13 H 0.3061 1.1775 0.5837 0.025 Uiso 1 1 calc R . .
C14 C 0.4299(5) 1.1545(11) 0.6364(4) 0.0173(17) Uani 1 1 d . . .
C15 C 0.5144(5) 1.1686(10) 0.6313(4) 0.0141(16) Uani 1 1 d . . .
C16 C 0.4170(5) 1.1119(11) 0.6949(4) 0.0164(17) Uani 1 1 d . . .
H16 H 0.3611 1.0977 0.7002 0.020 Uiso 1 1 calc R . .
C17 C 0.4854(5) 1.0911(11) 0.7438(4) 0.0157(16) Uani 1 1 d U . .
H17 H 0.4772 1.0648 0.7835 0.019 Uiso 1 1 calc R . .
C18 C 0.5676(5) 1.1088(10) 0.7354(3) 0.0120(15) Uani 1 1 d . . .
H18 H 0.6146 1.0941 0.7698 0.014 Uiso 1 1 calc R . .


_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 O2 1.938(5) 2_756 ?
Cu1 O6 1.945(5) . ?
Cu1 N1 2.009(6) . ?
Cu1 N2 2.020(6) . ?
Cu1 O15 2.362(5) . ?
V1A O10 1.638(11) . ?
V1A O11A 1.64(4) . ?
V1A O8 1.862(10) 3_766 ?
V1A O12 1.978(17) . ?
V1A O1 2.054(17) 4_575 ?
V1A O11B 2.46(3) . ?
V1B O10 1.717(8) . ?
V1B O11B 1.88(2) . ?
V1B O8 1.920(7) 3_766 ?
V1B O12 1.963(10) . ?
V1B O1 1.988(8) 4_575 ?
V2 O13 1.582(6) . ?
V2 O12 1.677(5) . ?
V2 O4 1.946(5) 2_746 ?
V2 O7 1.949(5) . ?
V2 O40 2.054(5) . ?
V3 O14 1.613(5) . ?
V3 O15 1.624(6) . ?
V3 O3 1.836(5) 2_746 ?
V3 O5 1.875(5) . ?
P1 O2 1.501(5) . ?
P1 O1 1.515(5) . ?
P1 O3 1.552(6) . ?
P1 C1 1.799(7) . ?
P2 O6 1.503(5) . ?
P2 O4 1.513(5) . ?
P2 O5 1.557(5) . ?
P2 C5 1.805(7) . ?
P3 O8 1.502(6) . ?
P3 O7 1.519(6) . ?
P3 O9 1.549(6) . ?
P3 C3 1.799(7) . ?
O1 V1B 1.988(8) 4_576 ?
O1 V1A 2.054(18) 4_576 ?
O2 Cu1 1.938(5) 2_746 ?
O3 V3 1.836(5) 2_756 ?
O4 V2 1.946(5) 2_756 ?
O8 V1A 1.862(10) 3_766 ?
O8 V1B 1.920(7) 3_766 ?
O11B V1B 1.88(2) 3_766 ?
O11B V1A 2.46(3) 3_766 ?
N1 C7 1.320(10) . ?
N1 C11 1.375(9) . ?
N2 C18 1.319(9) . ?
N2 C15 1.365(10) . ?
C1 C6 1.378(10) . ?
C1 C2 1.388(10) . ?
C2 C3 1.403(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(10) . ?
C4 C5 1.390(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.401(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.358(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(10) . ?
C10 C12 1.455(11) . ?
C11 C15 1.414(11) . ?
C12 C13 1.344(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.440(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.409(11) . ?
C14 C16 1.410(11) . ?
C16 C17 1.367(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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
O2 Cu1 O6 91.8(2) 2_756 . ?
O2 Cu1 N1 92.2(2) 2_756 . ?
O6 Cu1 N1 175.9(2) . . ?
O2 Cu1 N2 172.6(2) 2_756 . ?
O6 Cu1 N2 93.0(2) . . ?
N1 Cu1 N2 82.9(2) . . ?
O2 Cu1 O15 99.6(2) 2_756 . ?
O6 Cu1 O15 93.7(2) . . ?
N1 Cu1 O15 85.6(2) . . ?
N2 Cu1 O15 85.6(2) . . ?
O10 V1A O11A 90.7(17) . . ?
O10 V1A O8 99.6(6) . 3_766 ?
O11A V1A O8 91.5(15) . 3_766 ?
O10 V1A O12 93.8(6) . . ?
O11A V1A O12 102.0(10) . . ?
O8 V1A O12 160.8(17) 3_766 . ?
O10 V1A O1 162(2) . 4_575 ?
O11A V1A O1 106.3(12) . 4_575 ?
O8 V1A O1 84.2(4) 3_766 4_575 ?
O12 V1A O1 79.0(8) . 4_575 ?
O10 V1A O11B 84.6(10) . . ?
O11A V1A O11B 169.6(10) . . ?
O8 V1A O11B 80.2(8) 3_766 . ?
O12 V1A O11B 87.5(13) . . ?
O1 V1A O11B 79.2(11) 4_575 . ?
O10 V1B O11B 103.2(8) . . ?
O10 V1B O8 94.7(4) . 3_766 ?
O11B V1B O8 95.7(7) . 3_766 ?
O10 V1B O12 91.9(5) . . ?
O11B V1B O12 106.8(6) . . ?
O8 V1B O12 154.4(12) 3_766 . ?
O10 V1B O1 160.1(14) . 4_575 ?
O11B V1B O1 96.7(6) . 4_575 ?
O8 V1B O1 84.6(3) 3_766 4_575 ?
O12 V1B O1 80.9(4) . 4_575 ?
O13 V2 O12 107.9(3) . . ?
O13 V2 O4 101.4(3) . 2_746 ?
O12 V2 O4 91.3(2) . 2_746 ?
O13 V2 O7 109.8(3) . . ?
O12 V2 O7 141.5(3) . . ?
O4 V2 O7 89.1(2) 2_746 . ?
O13 V2 O40 98.2(3) . . ?
O12 V2 O40 84.8(2) . . ?
O4 V2 O40 160.3(2) 2_746 . ?
O7 V2 O40 82.2(2) . . ?
O14 V3 O15 109.3(3) . . ?
O14 V3 O3 108.9(3) . 2_746 ?
O15 V3 O3 106.9(3) . 2_746 ?
O14 V3 O5 110.2(3) . . ?
O15 V3 O5 107.9(2) . . ?
O3 V3 O5 113.5(2) 2_746 . ?
O2 P1 O1 111.6(3) . . ?
O2 P1 O3 112.0(3) . . ?
O1 P1 O3 109.0(3) . . ?
O2 P1 C1 111.4(3) . . ?
O1 P1 C1 109.4(3) . . ?
O3 P1 C1 103.1(3) . . ?
O6 P2 O4 112.9(3) . . ?
O6 P2 O5 112.1(3) . . ?
O4 P2 O5 107.9(3) . . ?
O6 P2 C5 112.2(3) . . ?
O4 P2 C5 106.5(3) . . ?
O5 P2 C5 104.8(3) . . ?
O8 P3 O7 112.9(4) . . ?
O8 P3 O9 110.9(4) . . ?
O7 P3 O9 111.7(3) . . ?
O8 P3 C3 105.4(3) . . ?
O7 P3 C3 108.4(3) . . ?
O9 P3 C3 107.2(3) . . ?
P1 O1 V1B 139.4(6) . 4_576 ?
P1 O1 V1A 125.0(10) . 4_576 ?
V1B O1 V1A 16.5(3) 4_576 4_576 ?
P1 O2 Cu1 135.0(3) . 2_746 ?
P1 O3 V3 145.9(4) . 2_756 ?
P2 O4 V2 138.9(3) . 2_756 ?
P2 O5 V3 129.7(3) . . ?
P2 O6 Cu1 137.6(3) . . ?
P3 O7 V2 147.7(4) . . ?
P3 O8 V1A 148.7(6) . 3_766 ?
P3 O8 V1B 147.5(5) . 3_766 ?
V1A O8 V1B 17.6(5) 3_766 3_766 ?
V1A O10 V1B 19.8(5) . . ?
V1B O11B V1B 179.996(1) 3_766 . ?
V1B O11B V1A 2.4(5) 3_766 3_766 ?
V1B O11B V1A 177.6(5) . 3_766 ?
V1B O11B V1A 177.6(5) 3_766 . ?
V1B O11B V1A 2.4(5) . . ?
V1A O11B V1A 179.998(5) 3_766 . ?
V2 O12 V1B 126.8(7) . . ?
V2 O12 V1A 143.7(10) . . ?
V1B O12 V1A 17.0(4) . . ?
V3 O15 Cu1 126.1(3) . . ?
C7 N1 C11 118.9(6) . . ?
C7 N1 Cu1 129.6(5) . . ?
C11 N1 Cu1 111.5(4) . . ?
C18 N2 C15 119.7(6) . . ?
C18 N2 Cu1 129.2(5) . . ?
C15 N2 Cu1 111.1(5) . . ?
C6 C1 C2 119.6(7) . . ?
C6 C1 P1 122.4(5) . . ?
C2 C1 P1 117.8(5) . . ?
C1 C2 C3 119.8(6) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 119.7(7) . . ?
C4 C3 P3 120.5(5) . . ?
C2 C3 P3 119.8(6) . . ?
C3 C4 C5 120.4(7) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.4(6) . . ?
C6 C5 P2 120.1(5) . . ?
C4 C5 P2 120.5(5) . . ?
C1 C6 C5 120.9(7) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N1 C7 C8 122.1(7) . . ?
N1 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 119.6(7) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.8(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 118.4(7) . . ?
C9 C10 C12 125.5(7) . . ?
C11 C10 C12 116.1(7) . . ?
N1 C11 C10 121.2(6) . . ?
N1 C11 C15 116.8(6) . . ?
C10 C11 C15 122.0(7) . . ?
C13 C12 C10 122.4(7) . . ?
C13 C12 H12 118.8 . . ?
C10 C12 H12 118.8 . . ?
C12 C13 C14 121.5(7) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C16 117.3(7) . . ?
C15 C14 C13 117.4(7) . . ?
C16 C14 C13 125.3(7) . . ?
N2 C15 C14 121.7(7) . . ?
N2 C15 C11 117.6(7) . . ?
C14 C15 C11 120.6(7) . . ?
C17 C16 C14 119.5(7) . . ?
C17 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
C16 C17 C18 119.9(7) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
N2 C18 C17 121.8(7) . . ?
N2 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?

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
O2 P1 O1 V1B 148.5(8) . . . 4_576 ?
O3 P1 O1 V1B 24.3(9) . . . 4_576 ?
C1 P1 O1 V1B -87.8(9) . . . 4_576 ?
O2 P1 O1 V1A 137.5(4) . . . 4_576 ?
O3 P1 O1 V1A 13.3(5) . . . 4_576 ?
C1 P1 O1 V1A -98.8(5) . . . 4_576 ?
O1 P1 O2 Cu1 -140.1(4) . . . 2_746 ?
O3 P1 O2 Cu1 -17.6(5) . . . 2_746 ?
C1 P1 O2 Cu1 97.3(5) . . . 2_746 ?
O2 P1 O3 V3 28.1(7) . . . 2_756 ?
O1 P1 O3 V3 152.1(6) . . . 2_756 ?
C1 P1 O3 V3 -91.7(6) . . . 2_756 ?
O6 P2 O4 V2 -17.5(6) . . . 2_756 ?
O5 P2 O4 V2 -141.9(4) . . . 2_756 ?
C5 P2 O4 V2 106.0(5) . . . 2_756 ?
O6 P2 O5 V3 46.0(5) . . . . ?
O4 P2 O5 V3 170.9(3) . . . . ?
C5 P2 O5 V3 -75.9(4) . . . . ?
O14 V3 O5 P2 -156.0(4) . . . . ?
O15 V3 O5 P2 -36.7(5) . . . . ?
O3 V3 O5 P2 81.6(4) 2_746 . . . ?
O4 P2 O6 Cu1 -155.3(4) . . . . ?
O5 P2 O6 Cu1 -33.2(5) . . . . ?
C5 P2 O6 Cu1 84.4(5) . . . . ?
O2 Cu1 O6 P2 -86.4(5) 2_756 . . . ?
N1 Cu1 O6 P2 93(3) . . . . ?
N2 Cu1 O6 P2 99.2(5) . . . . ?
O15 Cu1 O6 P2 13.4(5) . . . . ?
O8 P3 O7 V2 25.0(8) . . . . ?
O9 P3 O7 V2 -100.7(7) . . . . ?
C3 P3 O7 V2 141.4(6) . . . . ?
O13 V2 O7 P3 163.2(6) . . . . ?
O12 V2 O7 P3 -4.0(9) . . . . ?
O4 V2 O7 P3 -95.0(7) 2_746 . . . ?
O40 V2 O7 P3 67.3(7) . . . . ?
O7 P3 O8 V1A -109(2) . . . 3_766 ?
O9 P3 O8 V1A 17(2) . . . 3_766 ?
C3 P3 O8 V1A 133(2) . . . 3_766 ?
O7 P3 O8 V1B -75.2(14) . . . 3_766 ?
O9 P3 O8 V1B 51.0(14) . . . 3_766 ?
C3 P3 O8 V1B 166.7(13) . . . 3_766 ?
O11A V1A O10 V1B -178(2) . . . . ?
O8 V1A O10 V1B -86.3(9) 3_766 . . . ?
O12 V1A O10 V1B 80(3) . . . . ?
O1 V1A O10 V1B 15.1(18) 4_575 . . . ?
O11B V1A O10 V1B -7.2(13) . . . . ?
O11B V1B O10 V1A 170.3(18) . . . . ?
O8 V1B O10 V1A 73.3(11) 3_766 . . . ?
O12 V1B O10 V1A -82(2) . . . . ?
O1 V1B O10 V1A -13.7(18) 4_575 . . . ?
O10 V1B O11B V1B -151(5) . . . 3_766 ?
O8 V1B O11B V1B -54(5) 3_766 . . 3_766 ?
O12 V1B O11B V1B 113(5) . . . 3_766 ?
O1 V1B O11B V1B 31(5) 4_575 . . 3_766 ?
O10 V1B O11B V1A 117(6) . . . 3_766 ?
O8 V1B O11B V1A -147(6) 3_766 . . 3_766 ?
O12 V1B O11B V1A 20(6) . . . 3_766 ?
O1 V1B O11B V1A -62(6) 4_575 . . 3_766 ?
O10 V1B O11B V1A -63(6) . . . . ?
O8 V1B O11B V1A 33(6) 3_766 . . . ?
O12 V1B O11B V1A -160(6) . . . . ?
O1 V1B O11B V1A 118(6) 4_575 . . . ?
O10 V1A O11B V1B -67(6) . . . 3_766 ?
O11A V1A O11B V1B -3(9) . . . 3_766 ?
O8 V1A O11B V1B 34(6) 3_766 . . 3_766 ?
O12 V1A O11B V1B -161(6) . . . 3_766 ?
O1 V1A O11B V1B 120(6) 4_575 . . 3_766 ?
O10 V1A O11B V1B 113(6) . . . . ?
O11A V1A O11B V1B 177(100) . . . . ?
O8 V1A O11B V1B -146(6) 3_766 . . . ?
O12 V1A O11B V1B 19(6) . . . . ?
O1 V1A O11B V1B -60(6) 4_575 . . . ?
O10 V1A O11B V1A -138(14) . . . 3_766 ?
O11A V1A O11B V1A -75(14) . . . 3_766 ?
O8 V1A O11B V1A -37(13) 3_766 . . 3_766 ?
O12 V1A O11B V1A 128(13) . . . 3_766 ?
O1 V1A O11B V1A 49(13) 4_575 . . 3_766 ?
O13 V2 O12 V1B -169.5(4) . . . . ?
O4 V2 O12 V1B 88.1(4) 2_746 . . . ?
O7 V2 O12 V1B -2.1(6) . . . . ?
O40 V2 O12 V1B -72.5(4) . . . . ?
O13 V2 O12 V1A -172.0(7) . . . . ?
O4 V2 O12 V1A 85.6(8) 2_746 . . . ?
O7 V2 O12 V1A -4.6(10) . . . . ?
O40 V2 O12 V1A -75.0(8) . . . . ?
O10 V1B O12 V2 -102.9(8) . . . . ?
O11B V1B O12 V2 1.5(5) . . . . ?
O8 V1B O12 V2 152.1(13) 3_766 . . . ?
O1 V1B O12 V2 95.8(7) 4_575 . . . ?
O10 V1B O12 V1A 72.0(9) . . . . ?
O11B V1B O12 V1A 176.4(14) . . . . ?
O8 V1B O12 V1A -33(2) 3_766 . . . ?
O1 V1B O12 V1A -89.3(16) 4_575 . . . ?
O10 V1A O12 V2 -80.2(17) . . . . ?
O11A V1A O12 V2 -171.8(11) . . . . ?
O8 V1A O12 V2 54(4) 3_766 . . . ?
O1 V1A O12 V2 83.7(7) 4_575 . . . ?
O11B V1A O12 V2 4.2(8) . . . . ?
O10 V1A O12 V1B -87.1(10) . . . . ?
O11A V1A O12 V1B -178.6(18) . . . . ?
O8 V1A O12 V1B 47(5) 3_766 . . . ?
O1 V1A O12 V1B 76.8(18) 4_575 . . . ?
O11B V1A O12 V1B -2.7(10) . . . . ?
O14 V3 O15 Cu1 131.1(3) . . . . ?
O3 V3 O15 Cu1 -111.2(3) 2_746 . . . ?
O5 V3 O15 Cu1 11.3(4) . . . . ?
O2 Cu1 O15 V3 90.2(4) 2_756 . . . ?
O6 Cu1 O15 V3 -2.3(4) . . . . ?
N1 Cu1 O15 V3 -178.3(4) . . . . ?
N2 Cu1 O15 V3 -95.0(4) . . . . ?
O2 Cu1 N1 C7 5.7(7) 2_756 . . . ?
O6 Cu1 N1 C7 -173(3) . . . . ?
N2 Cu1 N1 C7 -179.8(7) . . . . ?
O15 Cu1 N1 C7 -93.7(7) . . . . ?
O2 Cu1 N1 C11 -174.8(5) 2_756 . . . ?
O6 Cu1 N1 C11 6(4) . . . . ?
N2 Cu1 N1 C11 -0.4(5) . . . . ?
O15 Cu1 N1 C11 85.8(5) . . . . ?
O2 Cu1 N2 C18 -129.9(17) 2_756 . . . ?
O6 Cu1 N2 C18 1.3(6) . . . . ?
N1 Cu1 N2 C18 -179.2(6) . . . . ?
O15 Cu1 N2 C18 94.7(6) . . . . ?
O2 Cu1 N2 C15 50(2) 2_756 . . . ?
O6 Cu1 N2 C15 -178.6(5) . . . . ?
N1 Cu1 N2 C15 1.0(5) . . . . ?
O15 Cu1 N2 C15 -85.1(5) . . . . ?
O2 P1 C1 C6 124.7(6) . . . . ?
O1 P1 C1 C6 0.8(7) . . . . ?
O3 P1 C1 C6 -115.1(6) . . . . ?
O2 P1 C1 C2 -58.8(6) . . . . ?
O1 P1 C1 C2 177.4(5) . . . . ?
O3 P1 C1 C2 61.4(6) . . . . ?
C6 C1 C2 C3 -1.0(10) . . . . ?
P1 C1 C2 C3 -177.6(5) . . . . ?
C1 C2 C3 C4 3.0(10) . . . . ?
C1 C2 C3 P3 -175.4(5) . . . . ?
O8 P3 C3 C4 -47.8(7) . . . . ?
O7 P3 C3 C4 -169.0(6) . . . . ?
O9 P3 C3 C4 70.4(6) . . . . ?
O8 P3 C3 C2 130.6(6) . . . . ?
O7 P3 C3 C2 9.5(7) . . . . ?
O9 P3 C3 C2 -111.2(6) . . . . ?
C2 C3 C4 C5 -2.0(10) . . . . ?
P3 C3 C4 C5 176.4(5) . . . . ?
C3 C4 C5 C6 -1.0(10) . . . . ?
C3 C4 C5 P2 -178.8(5) . . . . ?
O6 P2 C5 C6 128.8(6) . . . . ?
O4 P2 C5 C6 4.8(7) . . . . ?
O5 P2 C5 C6 -109.4(6) . . . . ?
O6 P2 C5 C4 -53.4(7) . . . . ?
O4 P2 C5 C4 -177.3(6) . . . . ?
O5 P2 C5 C4 68.5(6) . . . . ?
C2 C1 C6 C5 -2.0(11) . . . . ?
P1 C1 C6 C5 174.4(5) . . . . ?
C4 C5 C6 C1 3.0(10) . . . . ?
P2 C5 C6 C1 -179.1(5) . . . . ?
C11 N1 C7 C8 -1.3(11) . . . . ?
Cu1 N1 C7 C8 178.2(6) . . . . ?
N1 C7 C8 C9 1.0(12) . . . . ?
C7 C8 C9 C10 -1.4(12) . . . . ?
C8 C9 C10 C11 2.0(12) . . . . ?
C8 C9 C10 C12 -180.0(8) . . . . ?
C7 N1 C11 C10 1.9(10) . . . . ?
Cu1 N1 C11 C10 -177.7(5) . . . . ?
C7 N1 C11 C15 179.3(7) . . . . ?
Cu1 N1 C11 C15 -0.3(8) . . . . ?
C9 C10 C11 N1 -2.2(11) . . . . ?
C12 C10 C11 N1 179.5(7) . . . . ?
C9 C10 C11 C15 -179.5(7) . . . . ?
C12 C10 C11 C15 2.3(11) . . . . ?
C9 C10 C12 C13 -178.2(9) . . . . ?
C11 C10 C12 C13 -0.1(12) . . . . ?
C10 C12 C13 C14 -1.8(14) . . . . ?
C12 C13 C14 C15 1.5(13) . . . . ?
C12 C13 C14 C16 -177.9(8) . . . . ?
C18 N2 C15 C14 -0.2(11) . . . . ?
Cu1 N2 C15 C14 179.7(6) . . . . ?
C18 N2 C15 C11 178.7(6) . . . . ?
Cu1 N2 C15 C11 -1.4(8) . . . . ?
C16 C14 C15 N2 -1.0(11) . . . . ?
C13 C14 C15 N2 179.5(7) . . . . ?
C16 C14 C15 C11 -179.9(7) . . . . ?
C13 C14 C15 C11 0.6(11) . . . . ?
N1 C11 C15 N2 1.2(10) . . . . ?
C10 C11 C15 N2 178.5(7) . . . . ?
N1 C11 C15 C14 -179.9(7) . . . . ?
C10 C11 C15 C14 -2.6(11) . . . . ?
C15 C14 C16 C17 1.7(11) . . . . ?
C13 C14 C16 C17 -178.9(8) . . . . ?
C14 C16 C17 C18 -1.2(12) . . . . ?
C15 N2 C18 C17 0.8(11) . . . . ?
Cu1 N2 C18 C17 -179.1(5) . . . . ?
C16 C17 C18 N2 -0.1(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.159

data_15
_database_code_depnum_ccdc_archive 'CCDC 734636'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Cu N2 O10 P2, O'
_chemical_formula_sum            'C18 H18 Cu N2 O11 P2'
_chemical_formula_weight         563.82

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  -P1

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

_cell_length_a                   6.4769(7)
_cell_length_b                   8.4915(9)
_cell_length_c                   18.798(2)
_cell_angle_alpha                92.437(2)
_cell_angle_beta                 98.233(2)
_cell_angle_gamma                92.697(2)
_cell_volume                     1020.78(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5380
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             574
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_T_max  0.7816
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            10151
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         28.07
_reflns_number_total             4921
_reflns_number_gt                4592
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0510P)²+1.7726P] where P=(Fo²+2Fc²)/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         4921
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1071
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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 1.0000 0.01339(11) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.5000 0.5000 0.01544(11) Uani 1 2 d S . .
P1 P 0.71288(10) 0.03863(7) 0.83109(3) 0.01434(14) Uani 1 1 d . . .
P2 P 0.76016(10) 0.58931(7) 0.68682(3) 0.01392(14) Uani 1 1 d . . .
N1 N 0.5328(3) 0.2104(2) 1.05011(11) 0.0126(4) Uani 1 1 d . . .
N2 N 0.4709(3) 0.7108(2) 0.46228(11) 0.0155(4) Uani 1 1 d . . .
O1 O 0.4970(3) 0.0091(2) 0.79200(10) 0.0204(4) Uani 1 1 d . . .
O2 O 0.7075(3) 0.1133(2) 0.90719(10) 0.0167(4) Uani 1 1 d . . .
O3 O 0.8398(3) -0.1133(2) 0.84096(10) 0.0182(4) Uani 1 1 d . . .
O4 O 0.7589(3) 0.5925(2) 0.60409(10) 0.0178(4) Uani 1 1 d . . .
O5 O 0.8869(3) 0.7296(2) 0.72478(10) 0.0177(4) Uani 1 1 d . . .
O6 O 0.5331(3) 0.5708(2) 0.70125(11) 0.0213(4) Uani 1 1 d . . .
O7 O 0.2260(3) 0.0728(2) 0.95999(9) 0.0158(3) Uani 1 1 d . . .
O8 O 0.0149(3) 0.2694(2) 0.97345(10) 0.0179(4) Uani 1 1 d . . .
O9 O 0.2484(3) 0.5535(2) 0.54376(10) 0.0170(4) Uani 1 1 d . . .
O10 O 0.0150(3) 0.7410(2) 0.54250(10) 0.0197(4) Uani 1 1 d . . .
O90 O 0.2998(3) 0.7882(2) 0.70711(11) 0.0209(4) Uani 1 1 d . . .
C1 C 0.8719(4) 0.4103(3) 0.71641(13) 0.0140(4) Uani 1 1 d . . .
C2 C 0.7655(4) 0.3069(3) 0.75600(13) 0.0152(5) Uani 1 1 d . . .
H2 H 0.6278 0.3276 0.7642 0.018 Uiso 1 1 calc R . .
C3 C 0.8590(4) 0.1730(3) 0.78381(13) 0.0146(5) Uani 1 1 d . . .
C4 C 1.0624(4) 0.1464(3) 0.77313(14) 0.0169(5) Uani 1 1 d . . .
H4 H 1.1301 0.0587 0.7936 0.020 Uiso 1 1 calc R . .
C5 C 1.1675(4) 0.2475(3) 0.73263(14) 0.0183(5) Uani 1 1 d . . .
H5 H 1.3056 0.2267 0.7248 0.022 Uiso 1 1 calc R . .
C6 C 1.0735(4) 0.3787(3) 0.70341(14) 0.0170(5) Uani 1 1 d . . .
H6 H 1.1454 0.4460 0.6749 0.020 Uiso 1 1 calc R . .
C7 C 0.7013(4) 0.2757(3) 1.09228(13) 0.0166(5) Uani 1 1 d . . .
H7 H 0.8222 0.2165 1.1023 0.020 Uiso 1 1 calc R . .
C8 C 0.7027(4) 0.4294(3) 1.12192(14) 0.0194(5) Uani 1 1 d . . .
H8 H 0.8241 0.4752 1.1513 0.023 Uiso 1 1 calc R . .
C9 C 0.5258(4) 0.5141(3) 1.10803(14) 0.0188(5) Uani 1 1 d . . .
H9 H 0.5247 0.6189 1.1277 0.023 Uiso 1 1 calc R . .
C10 C 0.3485(4) 0.4448(3) 1.06500(13) 0.0163(5) Uani 1 1 d . . .
H10 H 0.2242 0.5001 1.0555 0.020 Uiso 1 1 calc R . .
C11 C 0.3601(4) 0.2930(3) 1.03667(13) 0.0134(4) Uani 1 1 d . . .
C12 C 0.1856(4) 0.2058(3) 0.98654(13) 0.0146(4) Uani 1 1 d . . .
C13 C 0.5951(4) 0.7856(3) 0.42231(14) 0.0177(5) Uani 1 1 d . . .
H13 H 0.7229 0.7417 0.4147 0.021 Uiso 1 1 calc R . .
C14 C 0.5405(5) 0.9272(3) 0.39147(14) 0.0210(5) Uani 1 1 d . . .
H14 H 0.6319 0.9809 0.3642 0.025 Uiso 1 1 calc R . .
C15 C 0.3523(5) 0.9881(3) 0.40104(15) 0.0231(6) Uani 1 1 d . . .
H15 H 0.3103 1.0820 0.3787 0.028 Uiso 1 1 calc R . .
C16 C 0.2247(4) 0.9115(3) 0.44350(14) 0.0195(5) Uani 1 1 d . . .
H16 H 0.0955 0.9525 0.4514 0.023 Uiso 1 1 calc R . .
C17 C 0.2910(4) 0.7735(3) 0.47395(13) 0.0155(5) Uani 1 1 d . . .
C18 C 0.1739(4) 0.6820(3) 0.52371(13) 0.0158(5) Uani 1 1 d . . .
H2' H 0.803(7) 0.154(5) 0.926(2) 0.048(13) Uiso 1 1 d . . .
H4' H 0.864(9) 0.631(7) 0.587(3) 0.085(19) Uiso 1 1 d . . .


_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 1.9644(17) 2_657 ?
Cu1 O7 1.9644(17) . ?
Cu1 N1 1.972(2) 2_657 ?
Cu1 N1 1.972(2) . ?
Cu2 N2 1.960(2) 2_666 ?
Cu2 N2 1.960(2) . ?
Cu2 O9 1.9901(18) 2_666 ?
Cu2 O9 1.9901(18) . ?
P1 O1 1.488(2) . ?
P1 O2 1.5456(19) . ?
P1 O3 1.5656(18) . ?
P1 C3 1.792(3) . ?
P2 O5 1.5066(19) . ?
P2 O6 1.5356(19) . ?
P2 O4 1.5555(19) . ?
P2 C1 1.790(2) . ?
N1 C7 1.336(3) . ?
N1 C11 1.347(3) . ?
N2 C13 1.335(3) . ?
N2 C17 1.346(3) . ?
O2 H2' 0.73(5) . ?
O4 H4' 0.85(6) . ?
O7 C12 1.269(3) . ?
O8 C12 1.250(3) . ?
O9 C18 1.265(3) . ?
O10 C18 1.254(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.399(3) . ?
C2 C3 1.399(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(3) . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.397(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.506(3) . ?
C13 C14 1.395(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.504(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 O7 179.998(1) 2_657 . ?
O7 Cu1 N1 83.23(8) 2_657 2_657 ?
O7 Cu1 N1 96.77(8) . 2_657 ?
O7 Cu1 N1 96.77(8) 2_657 . ?
O7 Cu1 N1 83.23(8) . . ?
N1 Cu1 N1 180.00(14) 2_657 . ?
N2 Cu2 N2 179.998(1) 2_666 . ?
N2 Cu2 O9 82.86(8) 2_666 2_666 ?
N2 Cu2 O9 97.14(8) . 2_666 ?
N2 Cu2 O9 97.14(8) 2_666 . ?
N2 Cu2 O9 82.86(8) . . ?
O9 Cu2 O9 180.000(1) 2_666 . ?
O1 P1 O2 110.42(11) . . ?
O1 P1 O3 114.11(11) . . ?
O2 P1 O3 106.87(10) . . ?
O1 P1 C3 110.23(11) . . ?
O2 P1 C3 107.88(11) . . ?
O3 P1 C3 107.08(11) . . ?
O5 P2 O6 115.69(11) . . ?
O5 P2 O4 110.57(11) . . ?
O6 P2 O4 108.30(11) . . ?
O5 P2 C1 110.02(11) . . ?
O6 P2 C1 103.99(11) . . ?
O4 P2 C1 107.85(11) . . ?
C7 N1 C11 119.7(2) . . ?
C7 N1 Cu1 127.89(17) . . ?
C11 N1 Cu1 112.41(16) . . ?
C13 N2 C17 119.6(2) . . ?
C13 N2 Cu2 127.55(18) . . ?
C17 N2 Cu2 112.44(17) . . ?
P1 O2 H2' 118(4) . . ?
P2 O4 H4' 121(4) . . ?
C12 O7 Cu1 113.92(16) . . ?
C18 O9 Cu2 113.51(16) . . ?
C2 C1 C6 119.6(2) . . ?
C2 C1 P2 120.81(19) . . ?
C6 C1 P2 119.47(19) . . ?
C1 C2 C3 120.9(2) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 118.9(2) . . ?
C4 C3 P1 121.59(19) . . ?
C2 C3 P1 119.47(19) . . ?
C3 C4 C5 120.3(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C1 C6 H6 120.4 . . ?
N1 C7 C8 121.1(2) . . ?
N1 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 119.3(2) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.7(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 117.7(2) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
N1 C11 C10 122.6(2) . . ?
N1 C11 C12 113.5(2) . . ?
C10 C11 C12 123.9(2) . . ?
O8 C12 O7 125.1(2) . . ?
O8 C12 C11 118.4(2) . . ?
O7 C12 C11 116.5(2) . . ?
N2 C13 C14 121.2(2) . . ?
N2 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 119.2(2) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.6(2) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 118.1(2) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
N2 C17 C16 122.2(2) . . ?
N2 C17 C18 113.8(2) . . ?
C16 C17 C18 124.0(2) . . ?
O10 C18 O9 126.1(2) . . ?
O10 C18 C17 117.5(2) . . ?
O9 C18 C17 116.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Cu1 N1 C7 4.5(2) 2_657 . . . ?
O7 Cu1 N1 C7 -175.5(2) . . . . ?
N1 Cu1 N1 C7 161(6) 2_657 . . . ?
O7 Cu1 N1 C11 -176.91(16) 2_657 . . . ?
O7 Cu1 N1 C11 3.09(16) . . . . ?
N1 Cu1 N1 C11 -21(6) 2_657 . . . ?
N2 Cu2 N2 C13 -55(3) 2_666 . . . ?
O9 Cu2 N2 C13 -2.0(2) 2_666 . . . ?
O9 Cu2 N2 C13 178.0(2) . . . . ?
N2 Cu2 N2 C17 118(3) 2_666 . . . ?
O9 Cu2 N2 C17 170.89(17) 2_666 . . . ?
O9 Cu2 N2 C17 -9.11(17) . . . . ?
O7 Cu1 O7 C12 -119(6) 2_657 . . . ?
N1 Cu1 O7 C12 174.35(17) 2_657 . . . ?
N1 Cu1 O7 C12 -5.65(17) . . . . ?
N2 Cu2 O9 C18 -173.65(17) 2_666 . . . ?
N2 Cu2 O9 C18 6.34(17) . . . . ?
O9 Cu2 O9 C18 -21(15) 2_666 . . . ?
O5 P2 C1 C2 113.2(2) . . . . ?
O6 P2 C1 C2 -11.3(2) . . . . ?
O4 P2 C1 C2 -126.1(2) . . . . ?
O5 P2 C1 C6 -62.9(2) . . . . ?
O6 P2 C1 C6 172.6(2) . . . . ?
O4 P2 C1 C6 57.8(2) . . . . ?
C6 C1 C2 C3 1.0(4) . . . . ?
P2 C1 C2 C3 -175.14(19) . . . . ?
C1 C2 C3 C4 1.7(4) . . . . ?
C1 C2 C3 P1 -177.36(19) . . . . ?
O1 P1 C3 C4 -135.3(2) . . . . ?
O2 P1 C3 C4 104.1(2) . . . . ?
O3 P1 C3 C4 -10.7(2) . . . . ?
O1 P1 C3 C2 43.8(2) . . . . ?
O2 P1 C3 C2 -76.9(2) . . . . ?
O3 P1 C3 C2 168.42(19) . . . . ?
C2 C3 C4 C5 -2.9(4) . . . . ?
P1 C3 C4 C5 176.1(2) . . . . ?
C3 C4 C5 C6 1.4(4) . . . . ?
C4 C5 C6 C1 1.3(4) . . . . ?
C2 C1 C6 C5 -2.5(4) . . . . ?
P2 C1 C6 C5 173.7(2) . . . . ?
C11 N1 C7 C8 -1.0(4) . . . . ?
Cu1 N1 C7 C8 177.50(18) . . . . ?
N1 C7 C8 C9 0.9(4) . . . . ?
C7 C8 C9 C10 0.3(4) . . . . ?
C8 C9 C10 C11 -1.2(4) . . . . ?
C7 N1 C11 C10 0.0(4) . . . . ?
Cu1 N1 C11 C10 -178.76(19) . . . . ?
C7 N1 C11 C12 178.3(2) . . . . ?
Cu1 N1 C11 C12 -0.5(2) . . . . ?
C9 C10 C11 N1 1.1(4) . . . . ?
C9 C10 C11 C12 -177.0(2) . . . . ?
Cu1 O7 C12 O8 -174.1(2) . . . . ?
Cu1 O7 C12 C11 6.9(3) . . . . ?
N1 C11 C12 O8 176.6(2) . . . . ?
C10 C11 C12 O8 -5.1(4) . . . . ?
N1 C11 C12 O7 -4.3(3) . . . . ?
C10 C11 C12 O7 173.9(2) . . . . ?
C17 N2 C13 C14 -0.8(4) . . . . ?
Cu2 N2 C13 C14 171.64(19) . . . . ?
N2 C13 C14 C15 -1.7(4) . . . . ?
C13 C14 C15 C16 2.7(4) . . . . ?
C14 C15 C16 C17 -1.1(4) . . . . ?
C13 N2 C17 C16 2.5(4) . . . . ?
Cu2 N2 C17 C16 -171.0(2) . . . . ?
C13 N2 C17 C18 -176.3(2) . . . . ?
Cu2 N2 C17 C18 10.2(3) . . . . ?
C15 C16 C17 N2 -1.5(4) . . . . ?
C15 C16 C17 C18 177.1(2) . . . . ?
Cu2 O9 C18 O10 179.0(2) . . . . ?
Cu2 O9 C18 C17 -2.5(3) . . . . ?
N2 C17 C18 O10 173.5(2) . . . . ?
C16 C17 C18 O10 -5.3(4) . . . . ?
N2 C17 C18 O9 -5.2(3) . . . . ?
C16 C17 C18 O9 176.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.103

data_16
_database_code_depnum_ccdc_archive 'CCDC 734637'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H16 Cu N2 O10 P2'
_chemical_formula_sum            'C18 H16 Cu N2 O10 P2'
_chemical_formula_weight         545.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  -P2ybc

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                   10.3525(5)
_cell_length_b                   6.4579(3)
_cell_length_c                   15.6396(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0850(10)
_cell_angle_gamma                90.00
_cell_volume                     993.94(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4698
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             554
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7776
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            9781
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.07
_reflns_number_total             2414
_reflns_number_gt                2386
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0240P)²+3.3132P] where P=(Fo²+2Fc²)/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         2414
_refine_ls_number_parameters     159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_restrained_S_all      1.339
_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
O2 O 0.7912(2) 0.7183(4) -0.09070(15) 0.0143(5) Uani 1 1 d . . .
Cu1 Cu 1.0000 0.5000 0.0000 0.01382(15) Uani 1 2 d S . .
P1 P 0.63871(8) 0.67203(13) -0.14186(5) 0.01253(18) Uani 1 1 d . . .
O1 O 0.6486(2) 0.4953(4) -0.20635(16) 0.0188(5) Uani 1 1 d . . .
O3 O 0.5643(2) 0.8618(4) -0.18443(16) 0.0207(5) Uani 1 1 d . . .
O4 O 0.9135(2) 0.2307(4) -0.03078(15) 0.0157(5) Uani 1 1 d . . .
O5 O 0.7994(2) -0.0043(4) 0.02236(16) 0.0187(5) Uani 1 1 d . . .
N1 N 0.9183(3) 0.4932(4) 0.09775(17) 0.0136(5) Uani 1 1 d . . .
C1 C 0.5415(3) 0.7051(5) 0.0027(2) 0.0155(6) Uani 1 1 d . . .
H1 H 0.5701 0.8453 0.0044 0.019 Uiso 1 1 calc R . .
C2 C 0.5620(3) 0.5697(5) -0.0622(2) 0.0119(6) Uani 1 1 d . . .
C3 C 0.5205(3) 0.3652(5) -0.0646(2) 0.0152(6) Uani 1 1 d . . .
H3 H 0.5343 0.2732 -0.1083 0.018 Uiso 1 1 calc R . .
C4 C 0.9212(3) 0.6377(5) 0.1591(2) 0.0159(6) Uani 1 1 d . . .
H4 H 0.9691 0.7630 0.1588 0.019 Uiso 1 1 calc R . .
C5 C 0.8559(3) 0.6097(6) 0.2234(2) 0.0188(7) Uani 1 1 d . . .
H5 H 0.8582 0.7150 0.2663 0.023 Uiso 1 1 calc R . .
C6 C 0.7874(3) 0.4260(6) 0.2242(2) 0.0187(7) Uani 1 1 d . . .
H6 H 0.7431 0.4034 0.2683 0.022 Uiso 1 1 calc R . .
C7 C 0.7838(3) 0.2751(5) 0.1605(2) 0.0164(6) Uani 1 1 d . . .
H7 H 0.7371 0.1481 0.1597 0.020 Uiso 1 1 calc R . .
C8 C 0.8505(3) 0.3155(5) 0.0979(2) 0.0141(6) Uani 1 1 d . . .
C9 C 0.8543(3) 0.1682(5) 0.0242(2) 0.0143(6) Uani 1 1 d . . .
H2' H 0.802(6) 0.808(9) -0.056(4) 0.055(18) Uiso 1 1 d . . .
H1' H 0.562(7) 0.454(10) -0.248(5) 0.08(2) Uiso 1 1 d . . .


_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
O2 P1 1.561(2) . ?
O2 Cu1 2.602(2) . ?
O2 H2' 0.78(6) . ?
Cu1 O4 1.947(2) 3_765 ?
Cu1 O4 1.947(2) . ?
Cu1 N1 1.964(3) . ?
Cu1 N1 1.964(3) 3_765 ?
P1 O3 1.490(2) . ?
P1 O1 1.547(2) . ?
P1 C2 1.798(3) . ?
O1 H1' 0.97(7) . ?
O4 C9 1.267(4) . ?
O5 C9 1.247(4) . ?
N1 C4 1.332(4) . ?
N1 C8 1.346(4) . ?
C1 C3 1.393(4) 3_665 ?
C1 C2 1.405(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(4) . ?
C3 C1 1.393(4) 3_665 ?
C3 H3 0.9500 . ?
C4 C5 1.387(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.504(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 O2 Cu1 135.43(13) . . ?
P1 O2 H2' 114(4) . . ?
Cu1 O2 H2' 96(4) . . ?
O4 Cu1 O4 180.0 3_765 . ?
O4 Cu1 N1 95.95(10) 3_765 . ?
O4 Cu1 N1 84.05(10) . . ?
O4 Cu1 N1 84.05(10) 3_765 3_765 ?
O4 Cu1 N1 95.95(10) . 3_765 ?
N1 Cu1 N1 180.0 . 3_765 ?
O4 Cu1 O2 83.77(9) 3_765 . ?
O4 Cu1 O2 96.23(9) . . ?
N1 Cu1 O2 87.18(9) . . ?
N1 Cu1 O2 92.82(9) 3_765 . ?
O3 P1 O1 116.42(14) . . ?
O3 P1 O2 111.81(14) . . ?
O1 P1 O2 102.40(13) . . ?
O3 P1 C2 109.49(14) . . ?
O1 P1 C2 108.25(14) . . ?
O2 P1 C2 108.01(13) . . ?
P1 O1 H1' 114(4) . . ?
C9 O4 Cu1 113.5(2) . . ?
C4 N1 C8 119.4(3) . . ?
C4 N1 Cu1 128.8(2) . . ?
C8 N1 Cu1 111.8(2) . . ?
C3 C1 C2 120.3(3) 3_665 . ?
C3 C1 H1 119.9 3_665 . ?
C2 C1 H1 119.9 . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 P1 122.2(2) . . ?
C1 C2 P1 118.0(2) . . ?
C2 C3 C1 119.9(3) . 3_665 ?
C2 C3 H3 120.0 . . ?
C1 C3 H3 120.0 3_665 . ?
N1 C4 C5 121.6(3) . . ?
N1 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 119.7(3) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C8 117.9(3) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
N1 C8 C7 122.4(3) . . ?
N1 C8 C9 113.6(3) . . ?
C7 C8 C9 124.0(3) . . ?
O5 C9 O4 125.6(3) . . ?
O5 C9 C8 117.6(3) . . ?
O4 C9 C8 116.8(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
P1 O2 Cu1 O4 -171.32(19) . . . 3_765 ?
P1 O2 Cu1 O4 8.68(19) . . . . ?
P1 O2 Cu1 N1 -75.01(19) . . . . ?
P1 O2 Cu1 N1 104.99(19) . . . 3_765 ?
Cu1 O2 P1 O3 -178.72(16) . . . . ?
Cu1 O2 P1 O1 -53.4(2) . . . . ?
Cu1 O2 P1 C2 60.8(2) . . . . ?
O4 Cu1 O4 C9 91(11) 3_765 . . . ?
N1 Cu1 O4 C9 -3.8(2) . . . . ?
N1 Cu1 O4 C9 176.2(2) 3_765 . . . ?
O2 Cu1 O4 C9 -90.3(2) . . . . ?
O4 Cu1 N1 C4 2.8(3) 3_765 . . . ?
O4 Cu1 N1 C4 -177.2(3) . . . . ?
N1 Cu1 N1 C4 118(5) 3_765 . . . ?
O2 Cu1 N1 C4 -80.6(3) . . . . ?
O4 Cu1 N1 C8 -178.2(2) 3_765 . . . ?
O4 Cu1 N1 C8 1.8(2) . . . . ?
N1 Cu1 N1 C8 -63(5) 3_765 . . . ?
O2 Cu1 N1 C8 98.4(2) . . . . ?
C3 C1 C2 C3 -0.1(5) 3_665 . . . ?
C3 C1 C2 P1 178.5(2) 3_665 . . . ?
O3 P1 C2 C3 127.1(3) . . . . ?
O1 P1 C2 C3 -0.8(3) . . . . ?
O2 P1 C2 C3 -110.9(3) . . . . ?
O3 P1 C2 C1 -51.4(3) . . . . ?
O1 P1 C2 C1 -179.3(2) . . . . ?
O2 P1 C2 C1 70.5(3) . . . . ?
C1 C2 C3 C1 0.1(5) . . . 3_665 ?
P1 C2 C3 C1 -178.4(2) . . . 3_665 ?
C8 N1 C4 C5 0.1(5) . . . . ?
Cu1 N1 C4 C5 179.0(2) . . . . ?
N1 C4 C5 C6 0.7(5) . . . . ?
C4 C5 C6 C7 -0.8(5) . . . . ?
C5 C6 C7 C8 0.2(5) . . . . ?
C4 N1 C8 C7 -0.7(5) . . . . ?
Cu1 N1 C8 C7 -179.8(2) . . . . ?
C4 N1 C8 C9 179.2(3) . . . . ?
Cu1 N1 C8 C9 0.1(3) . . . . ?
C6 C7 C8 N1 0.5(5) . . . . ?
C6 C7 C8 C9 -179.3(3) . . . . ?
Cu1 O4 C9 O5 -175.1(3) . . . . ?
Cu1 O4 C9 C8 4.8(3) . . . . ?
N1 C8 C9 O5 176.6(3) . . . . ?
C7 C8 C9 O5 -3.6(5) . . . . ?
N1 C8 C9 O4 -3.3(4) . . . . ?
C7 C8 C9 O4 176.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.106

data_17
_database_code_depnum_ccdc_archive 'CCDC 734638'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H34 Cu2 N4 O20 P6'
_chemical_formula_sum            'C32 H34 Cu2 N4 O20 P6'
_chemical_formula_weight         1107.53

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  -P1

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

_cell_length_a                   10.114(2)
_cell_length_b                   10.753(2)
_cell_length_c                   11.130(2)
_cell_angle_alpha                114.17(3)
_cell_angle_beta                 105.57(3)
_cell_angle_gamma                104.01(3)
_cell_volume                     974.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    4759
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             562
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_T_max  0.8702
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            9826
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         28.30
_reflns_number_total             4759
_reflns_number_gt                4482
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0402P)²+1.3065P] where P=(Fo²+2Fc²)/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         4759
_refine_ls_number_parameters     313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_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 0.32964(3) 1.03078(3) 0.63871(3) 0.00992(8) Uani 1 1 d . . .
P1 P 0.37230(6) 0.79014(6) 0.38268(6) 0.00936(12) Uani 1 1 d . . .
P2 P -0.12859(6) 0.25476(6) 0.10277(6) 0.01208(12) Uani 1 1 d . . .
P3 P 0.43751(6) 0.25250(6) 0.20176(6) 0.01130(12) Uani 1 1 d . . .
O1 O 0.37265(17) 0.85962(17) 0.53234(17) 0.0117(3) Uani 1 1 d . . .
O2 O 0.26335(19) 0.83265(19) 0.2932(2) 0.0143(3) Uani 1 1 d . . .
O3 O 0.52366(17) 0.82871(17) 0.37879(18) 0.0131(3) Uani 1 1 d . . .
O4 O -0.1666(2) 0.3360(2) 0.2314(2) 0.0222(4) Uani 1 1 d . . .
O5 O -0.21487(19) 0.2580(2) -0.02796(18) 0.0190(4) Uani 1 1 d . . .
O6 O -0.1418(2) 0.0998(2) 0.0752(2) 0.0280(5) Uani 1 1 d . . .
O7 O 0.59514(18) 0.35312(19) 0.2492(2) 0.0195(4) Uani 1 1 d . . .
O8 O 0.36576(18) 0.12553(18) 0.04510(18) 0.0158(3) Uani 1 1 d . . .
O9 O 0.4181(2) 0.1897(2) 0.3041(2) 0.0195(4) Uani 1 1 d . . .
O40 O 0.4765(2) 1.0623(2) 0.8415(2) 0.0176(4) Uani 1 1 d . . .
N1 N 0.2640(2) 1.1895(2) 0.7395(2) 0.0136(4) Uani 1 1 d . . .
N2 N 0.1275(2) 0.9021(2) 0.6064(2) 0.0123(4) Uani 1 1 d . . .
C1 C 0.2897(2) 0.5900(2) 0.2997(2) 0.0105(4) Uani 1 1 d . . .
C2 C 0.1346(2) 0.5116(2) 0.2412(2) 0.0114(4) Uani 1 1 d . . .
H2 H 0.0729 0.5634 0.2474 0.014 Uiso 1 1 calc R . .
C3 C 0.0707(2) 0.3560(2) 0.1732(2) 0.0114(4) Uani 1 1 d . . .
C4 C 0.1647(2) 0.2790(2) 0.1611(2) 0.0119(4) Uani 1 1 d . . .
H4 H 0.1232 0.1757 0.1132 0.014 Uiso 1 1 calc R . .
C5 C 0.3201(2) 0.3557(2) 0.2203(2) 0.0110(4) Uani 1 1 d . . .
C6 C 0.3813(2) 0.5105(2) 0.2912(2) 0.0117(4) Uani 1 1 d . . .
H6 H 0.4847 0.5621 0.3337 0.014 Uiso 1 1 calc R . .
C7 C 0.3472(3) 1.3364(3) 0.8132(3) 0.0173(5) Uani 1 1 d . . .
H7 H 0.4393 1.3698 0.8099 0.021 Uiso 1 1 calc R . .
C8 C 0.3015(3) 1.4400(3) 0.8938(3) 0.0187(5) Uani 1 1 d . . .
H8 H 0.3601 1.5413 0.9409 0.022 Uiso 1 1 calc R . .
C9 C 0.1673(3) 1.3902(3) 0.9029(3) 0.0190(5) Uani 1 1 d . . .
H9 H 0.1354 1.4575 0.9584 0.023 Uiso 1 1 calc R . .
C10 C 0.0809(3) 1.2389(3) 0.8286(3) 0.0185(5) Uani 1 1 d . . .
H10 H -0.0094 1.2034 0.8342 0.022 Uiso 1 1 calc R . .
C11 C 0.1307(3) 1.1407(3) 0.7453(2) 0.0138(4) Uani 1 1 d . . .
C12 C 0.0474(2) 0.9779(3) 0.6596(2) 0.0135(4) Uani 1 1 d . . .
C13 C -0.0997(3) 0.9056(3) 0.6338(3) 0.0183(5) Uani 1 1 d . . .
H13 H -0.1532 0.9594 0.6696 0.022 Uiso 1 1 calc R . .
C14 C -0.1650(3) 0.7514(3) 0.5534(3) 0.0212(5) Uani 1 1 d . . .
H14 H -0.2639 0.7005 0.5333 0.025 Uiso 1 1 calc R . .
C15 C -0.0823(3) 0.6733(3) 0.5031(3) 0.0198(5) Uani 1 1 d . . .
H15 H -0.1239 0.5699 0.4508 0.024 Uiso 1 1 calc R . .
C16 C 0.0644(3) 0.7534(3) 0.5327(3) 0.0161(4) Uani 1 1 d . . .
H16 H 0.1206 0.7015 0.5001 0.019 Uiso 1 1 calc R . .
H2' H 0.250(4) 0.802(4) 0.219(4) 0.030(10) Uiso 1 1 d . . .
H4' H -0.241(5) 0.324(5) 0.218(5) 0.049(13) Uiso 1 1 d . . .
H6' H -0.227(5) 0.018(5) 0.027(5) 0.068(14) Uiso 1 1 d . . .
H9' H 0.480(4) 0.165(4) 0.338(4) 0.034(10) Uiso 1 1 d . . .
H40A H 0.448(4) 1.080(4) 0.899(4) 0.026(9) Uiso 1 1 d . . .
H40B H 0.550(5) 1.110(4) 0.868(4) 0.032(11) Uiso 1 1 d . . .


_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 O3 1.9578(17) 2_676 ?
Cu1 O1 1.9643(17) . ?
Cu1 N1 1.998(2) . ?
Cu1 N2 2.013(2) . ?
Cu1 O40 2.178(2) . ?
P1 O3 1.5033(16) . ?
P1 O1 1.5195(17) . ?
P1 O2 1.5627(18) . ?
P1 C1 1.808(2) . ?
P2 O5 1.5013(19) . ?
P2 O6 1.5296(19) . ?
P2 O4 1.548(2) . ?
P2 C3 1.803(2) . ?
P3 O7 1.4954(19) . ?
P3 O8 1.524(2) . ?
P3 O9 1.5736(19) . ?
P3 C5 1.807(2) . ?
O2 H2' 0.71(4) . ?
O3 Cu1 1.9578(17) 2_676 ?
O4 H4' 0.70(4) . ?
O6 H6' 0.89(5) . ?
O9 H9' 0.81(4) . ?
O40 H40A 0.74(4) . ?
O40 H40B 0.69(4) . ?
N1 C7 1.342(3) . ?
N1 C11 1.352(3) . ?
N2 C16 1.337(3) . ?
N2 C12 1.361(3) . ?
C1 C2 1.398(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.402(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.402(3) . ?
C4 C5 1.399(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.383(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.381(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.474(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.388(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.392(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?

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
O3 Cu1 O1 94.82(7) 2_676 . ?
O3 Cu1 N1 90.51(8) 2_676 . ?
O1 Cu1 N1 173.95(7) . . ?
O3 Cu1 N2 158.28(8) 2_676 . ?
O1 Cu1 N2 93.35(8) . . ?
N1 Cu1 N2 80.66(9) . . ?
O3 Cu1 O40 97.81(9) 2_676 . ?
O1 Cu1 O40 89.34(8) . . ?
N1 Cu1 O40 92.79(8) . . ?
N2 Cu1 O40 102.37(9) . . ?
O3 P1 O1 115.63(10) . . ?
O3 P1 O2 113.56(10) . . ?
O1 P1 O2 105.52(10) . . ?
O3 P1 C1 106.28(10) . . ?
O1 P1 C1 108.48(10) . . ?
O2 P1 C1 107.01(11) . . ?
O5 P2 O6 114.66(12) . . ?
O5 P2 O4 111.31(11) . . ?
O6 P2 O4 111.41(13) . . ?
O5 P2 C3 112.59(11) . . ?
O6 P2 C3 102.76(11) . . ?
O4 P2 C3 103.23(11) . . ?
O7 P3 O8 113.82(11) . . ?
O7 P3 O9 113.79(11) . . ?
O8 P3 O9 109.99(10) . . ?
O7 P3 C5 110.61(10) . . ?
O8 P3 C5 107.30(10) . . ?
O9 P3 C5 100.31(10) . . ?
P1 O1 Cu1 132.04(10) . . ?
P1 O2 H2' 116(3) . . ?
P1 O3 Cu1 143.13(10) . 2_676 ?
P2 O4 H4' 118(4) . . ?
P2 O6 H6' 126(3) . . ?
P3 O9 H9' 120(3) . . ?
Cu1 O40 H40A 115(3) . . ?
Cu1 O40 H40B 114(3) . . ?
H40A O40 H40B 112(4) . . ?
C7 N1 C11 118.7(2) . . ?
C7 N1 Cu1 125.49(16) . . ?
C11 N1 Cu1 115.38(16) . . ?
C16 N2 C12 118.8(2) . . ?
C16 N2 Cu1 126.33(16) . . ?
C12 N2 Cu1 114.78(16) . . ?
C2 C1 C6 118.8(2) . . ?
C2 C1 P1 121.24(17) . . ?
C6 C1 P1 119.94(17) . . ?
C1 C2 C3 121.1(2) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 118.8(2) . . ?
C4 C3 P2 119.93(17) . . ?
C2 C3 P2 121.23(17) . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C6 C5 C4 119.2(2) . . ?
C6 C5 P3 121.29(17) . . ?
C4 C5 P3 119.56(17) . . ?
C5 C6 C1 121.2(2) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
N1 C7 C8 122.6(2) . . ?
N1 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C9 C8 C7 118.7(2) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C10 119.3(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C10 C11 119.2(2) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
N1 C11 C10 121.4(2) . . ?
N1 C11 C12 114.5(2) . . ?
C10 C11 C12 124.1(2) . . ?
N2 C12 C13 122.0(2) . . ?
N2 C12 C11 114.1(2) . . ?
C13 C12 C11 124.0(2) . . ?
C14 C13 C12 118.5(2) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 118.5(2) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
N2 C16 C15 122.4(2) . . ?
N2 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?

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
O3 P1 O1 Cu1 101.58(14) . . . . ?
O2 P1 O1 Cu1 -24.82(15) . . . . ?
C1 P1 O1 Cu1 -139.20(13) . . . . ?
O3 Cu1 O1 P1 -55.05(14) 2_676 . . . ?
N1 Cu1 O1 P1 96.4(7) . . . . ?
N2 Cu1 O1 P1 104.82(14) . . . . ?
O40 Cu1 O1 P1 -152.83(14) . . . . ?
O1 P1 O3 Cu1 -92.30(19) . . . 2_676 ?
O2 P1 O3 Cu1 29.9(2) . . . 2_676 ?
C1 P1 O3 Cu1 147.28(16) . . . 2_676 ?
O3 Cu1 N1 C7 -24.3(2) 2_676 . . . ?
O1 Cu1 N1 C7 -175.9(6) . . . . ?
N2 Cu1 N1 C7 175.7(2) . . . . ?
O40 Cu1 N1 C7 73.6(2) . . . . ?
O3 Cu1 N1 C11 163.36(16) 2_676 . . . ?
O1 Cu1 N1 C11 11.8(8) . . . . ?
N2 Cu1 N1 C11 3.29(16) . . . . ?
O40 Cu1 N1 C11 -98.80(17) . . . . ?
O3 Cu1 N2 C16 111.1(2) 2_676 . . . ?
O1 Cu1 N2 C16 -0.9(2) . . . . ?
N1 Cu1 N2 C16 178.2(2) . . . . ?
O40 Cu1 N2 C16 -91.0(2) . . . . ?
O3 Cu1 N2 C12 -65.1(3) 2_676 . . . ?
O1 Cu1 N2 C12 -177.07(16) . . . . ?
N1 Cu1 N2 C12 2.04(16) . . . . ?
O40 Cu1 N2 C12 92.87(16) . . . . ?
O3 P1 C1 C2 -158.09(18) . . . . ?
O1 P1 C1 C2 77.0(2) . . . . ?
O2 P1 C1 C2 -36.4(2) . . . . ?
O3 P1 C1 C6 20.9(2) . . . . ?
O1 P1 C1 C6 -104.08(19) . . . . ?
O2 P1 C1 C6 142.51(18) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
P1 C1 C2 C3 178.12(17) . . . . ?
C1 C2 C3 C4 -1.7(3) . . . . ?
C1 C2 C3 P2 177.94(17) . . . . ?
O5 P2 C3 C4 -110.64(19) . . . . ?
O6 P2 C3 C4 13.2(2) . . . . ?
O4 P2 C3 C4 129.21(19) . . . . ?
O5 P2 C3 C2 69.7(2) . . . . ?
O6 P2 C3 C2 -166.39(19) . . . . ?
O4 P2 C3 C2 -50.4(2) . . . . ?
C2 C3 C4 C5 2.3(3) . . . . ?
P2 C3 C4 C5 -177.32(17) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C3 C4 C5 P3 -179.71(17) . . . . ?
O7 P3 C5 C6 -9.2(2) . . . . ?
O8 P3 C5 C6 -133.87(19) . . . . ?
O9 P3 C5 C6 111.26(19) . . . . ?
O7 P3 C5 C4 170.14(17) . . . . ?
O8 P3 C5 C4 45.4(2) . . . . ?
O9 P3 C5 C4 -69.4(2) . . . . ?
C4 C5 C6 C1 -2.3(3) . . . . ?
P3 C5 C6 C1 177.06(17) . . . . ?
C2 C1 C6 C5 2.9(3) . . . . ?
P1 C1 C6 C5 -176.11(17) . . . . ?
C11 N1 C7 C8 -0.6(4) . . . . ?
Cu1 N1 C7 C8 -172.76(18) . . . . ?
N1 C7 C8 C9 2.3(4) . . . . ?
C7 C8 C9 C10 -1.6(4) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C7 N1 C11 C10 -1.7(3) . . . . ?
Cu1 N1 C11 C10 171.19(17) . . . . ?
C7 N1 C11 C12 179.4(2) . . . . ?
Cu1 N1 C11 C12 -7.7(2) . . . . ?
C9 C10 C11 N1 2.3(4) . . . . ?
C9 C10 C11 C12 -178.9(2) . . . . ?
C16 N2 C12 C13 -3.0(3) . . . . ?
Cu1 N2 C12 C13 173.42(18) . . . . ?
C16 N2 C12 C11 177.0(2) . . . . ?
Cu1 N2 C12 C11 -6.6(2) . . . . ?
N1 C11 C12 N2 9.3(3) . . . . ?
C10 C11 C12 N2 -169.5(2) . . . . ?
N1 C11 C12 C13 -170.6(2) . . . . ?
C10 C11 C12 C13 10.5(4) . . . . ?
N2 C12 C13 C14 1.1(4) . . . . ?
C11 C12 C13 C14 -178.9(2) . . . . ?
C12 C13 C14 C15 1.1(4) . . . . ?
C13 C14 C15 C16 -1.3(4) . . . . ?
C12 N2 C16 C15 2.8(3) . . . . ?
Cu1 N2 C16 C15 -173.24(18) . . . . ?
C14 C15 C16 N2 -0.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.097

#[Cu(bipy){(HO3P)2C6H3(PO3H2)}] ?H2O 18
data_[Cu(bipy){(HO3P)2C6H3(PO3H2)}]?H2O18
_database_code_depnum_ccdc_archive 'CCDC 734639'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H15 Cu N2 O9 P3, O'
_chemical_formula_sum            'C16 H17 Cu N2 O10 P3'
_chemical_formula_weight         553.77

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  -P1

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

_cell_length_a                   9.8914(9)
_cell_length_b                   10.0130(9)
_cell_length_c                   11.5152(10)
_cell_angle_alpha                104.2480(10)
_cell_angle_beta                 98.961(2)
_cell_angle_gamma                115.9090(10)
_cell_volume                     947.88(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    6273
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             562
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_T_max  0.7575
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            9498
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         28.08
_reflns_number_total             4574
_reflns_number_gt                4428
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0431P)²+1.3547P] where P=(Fo²+2Fc²)/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         4574
_refine_ls_number_parameters     305
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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 0.96646(3) 0.23934(3) 0.10941(2) 0.00914(8) Uani 1 1 d . . .
P1 P 0.21740(6) 0.10994(6) 0.08677(5) 0.00861(11) Uani 1 1 d . . .
P2 P 0.77173(6) 0.14021(6) 0.32576(5) 0.00889(11) Uani 1 1 d . . .
P3 P 0.74371(6) 0.69167(6) 0.37512(5) 0.00927(12) Uani 1 1 d . . .
O1 O 0.15923(17) -0.06514(17) 0.05491(14) 0.0107(3) Uani 1 1 d . . .
O2 O 0.12351(18) 0.17565(18) 0.14603(14) 0.0119(3) Uani 1 1 d . . .
O3 O 0.23375(19) 0.1540(2) -0.03451(16) 0.0130(3) Uani 1 1 d . . .
O4 O 0.66789(19) -0.00414(19) 0.35588(16) 0.0139(3) Uani 1 1 d . . .
O5 O 0.91423(19) 0.27008(19) 0.44019(16) 0.0157(3) Uani 1 1 d . . .
O6 O 0.82253(19) 0.09660(19) 0.21150(15) 0.0142(3) Uani 1 1 d . . .
O7 O 0.70798(19) 0.7237(2) 0.50317(15) 0.0141(3) Uani 1 1 d . . .
O8 O 0.91955(17) 0.76626(18) 0.39571(15) 0.0121(3) Uani 1 1 d . . .
O9 O 0.66163(19) 0.74126(18) 0.28546(15) 0.0141(3) Uani 1 1 d . . .
O90 O 0.9161(2) 0.98598(19) 0.67499(15) 0.0175(3) Uani 1 1 d . . .
N1 N 1.1108(2) 0.4599(2) 0.23414(17) 0.0113(3) Uani 1 1 d . . .
N2 N 0.8422(2) 0.3424(2) 0.07053(17) 0.0106(3) Uani 1 1 d . . .
C1 C 0.4170(2) 0.2211(2) 0.19348(19) 0.0099(4) Uani 1 1 d . . .
C2 C 0.5008(2) 0.1478(2) 0.22738(19) 0.0101(4) Uani 1 1 d . . .
H2 H 0.4488 0.0354 0.2022 0.012 Uiso 1 1 calc R . .
C3 C 0.6603(2) 0.2375(2) 0.29779(19) 0.0091(4) Uani 1 1 d . . .
C4 C 0.7343(2) 0.4027(2) 0.33971(19) 0.0102(4) Uani 1 1 d . . .
H4 H 0.8424 0.4643 0.3881 0.012 Uiso 1 1 calc R . .
C5 C 0.6508(2) 0.4784(2) 0.31116(19) 0.0095(4) Uani 1 1 d . . .
C6 C 0.4937(2) 0.3873(2) 0.2363(2) 0.0106(4) Uani 1 1 d . . .
H6 H 0.4379 0.4386 0.2140 0.013 Uiso 1 1 calc R . .
C7 C 1.2411(3) 0.5078(3) 0.3259(2) 0.0138(4) Uani 1 1 d . . .
H7 H 1.2607 0.4303 0.3462 0.017 Uiso 1 1 calc R . .
C8 C 1.3481(3) 0.6671(3) 0.3921(2) 0.0159(4) Uani 1 1 d . . .
H8 H 1.4394 0.6981 0.4571 0.019 Uiso 1 1 calc R . .
C9 C 1.3201(3) 0.7803(3) 0.3622(2) 0.0160(4) Uani 1 1 d . . .
H9 H 1.3939 0.8901 0.4045 0.019 Uiso 1 1 calc R . .
C10 C 1.1827(3) 0.7316(3) 0.2695(2) 0.0144(4) Uani 1 1 d . . .
H10 H 1.1603 0.8072 0.2482 0.017 Uiso 1 1 calc R . .
C11 C 1.0795(2) 0.5703(3) 0.20887(19) 0.0104(4) Uani 1 1 d . . .
C12 C 0.9226(2) 0.5029(3) 0.1182(2) 0.0105(4) Uani 1 1 d . . .
C13 C 0.8564(3) 0.5919(3) 0.0891(2) 0.0126(4) Uani 1 1 d . . .
H13 H 0.9155 0.7045 0.1210 0.015 Uiso 1 1 calc R . .
C14 C 0.7009(3) 0.5119(3) 0.0120(2) 0.0144(4) Uani 1 1 d . . .
H14 H 0.6526 0.5699 -0.0092 0.017 Uiso 1 1 calc R . .
C15 C 0.6168(3) 0.3470(3) -0.0337(2) 0.0141(4) Uani 1 1 d . . .
H15 H 0.5103 0.2907 -0.0853 0.017 Uiso 1 1 calc R . .
C16 C 0.6923(3) 0.2667(3) -0.0020(2) 0.0134(4) Uani 1 1 d . . .
H16 H 0.6356 0.1539 -0.0328 0.016 Uiso 1 1 calc R . .
H2' H 0.963(5) 0.248(5) 0.490(4) 0.042(11) Uiso 1 1 d . . .
H3' H 0.231(4) 0.092(5) -0.082(4) 0.036(11) Uiso 1 1 d . . .
H4' H 0.669(7) -0.112(7) 0.326(6) 0.11(2) Uiso 1 1 d . . .
H7' H 0.772(5) 0.804(5) 0.553(4) 0.047(12) Uiso 1 1 d . . .


_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 O2 1.9473(15) 1_655 ?
Cu1 O1 1.9789(15) 2_655 ?
Cu1 N2 1.9857(18) . ?
Cu1 N1 2.0054(18) . ?
Cu1 O6 2.2409(16) . ?
P1 O2 1.5071(16) . ?
P1 O1 1.5083(15) . ?
P1 O3 1.5756(17) . ?
P1 C1 1.816(2) . ?
P2 O6 1.5131(16) . ?
P2 O4 1.5247(16) . ?
P2 O5 1.5460(17) . ?
P2 C3 1.803(2) . ?
P3 O8 1.5127(16) . ?
P3 O9 1.5216(16) . ?
P3 O7 1.5590(17) . ?
P3 C5 1.802(2) . ?
O1 Cu1 1.9789(15) 2_655 ?
O2 Cu1 1.9473(15) 1_455 ?
O3 H3' 0.71(4) . ?
O4 H4' 1.06(6) . ?
O5 H2' 0.82(4) . ?
O7 H7' 0.77(4) . ?
N1 C7 1.339(3) . ?
N1 C11 1.354(3) . ?
N2 C16 1.338(3) . ?
N2 C12 1.353(3) . ?
C1 C2 1.396(3) . ?
C1 C6 1.402(3) . ?
C2 C3 1.399(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(3) . ?
C4 C5 1.396(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.479(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.393(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
O2 Cu1 O1 95.30(6) 1_655 2_655 ?
O2 Cu1 N2 168.47(7) 1_655 . ?
O1 Cu1 N2 89.44(7) 2_655 . ?
O2 Cu1 N1 91.93(7) 1_655 . ?
O1 Cu1 N1 159.31(7) 2_655 . ?
N2 Cu1 N1 80.21(7) . . ?
O2 Cu1 O6 91.17(6) 1_655 . ?
O1 Cu1 O6 92.27(6) 2_655 . ?
N2 Cu1 O6 99.15(7) . . ?
N1 Cu1 O6 106.96(7) . . ?
O2 P1 O1 117.61(9) . . ?
O2 P1 O3 108.34(9) . . ?
O1 P1 O3 109.62(9) . . ?
O2 P1 C1 106.93(9) . . ?
O1 P1 C1 109.00(9) . . ?
O3 P1 C1 104.53(9) . . ?
O6 P2 O4 112.65(9) . . ?
O6 P2 O5 111.61(10) . . ?
O4 P2 O5 112.55(10) . . ?
O6 P2 C3 109.26(9) . . ?
O4 P2 C3 107.70(9) . . ?
O5 P2 C3 102.46(9) . . ?
O8 P3 O9 113.77(9) . . ?
O8 P3 O7 110.61(9) . . ?
O9 P3 O7 111.13(9) . . ?
O8 P3 C5 110.43(9) . . ?
O9 P3 C5 107.08(9) . . ?
O7 P3 C5 103.24(9) . . ?
P1 O1 Cu1 128.60(9) . 2_655 ?
P1 O2 Cu1 143.05(10) . 1_455 ?
P1 O3 H3' 110(3) . . ?
P2 O4 H4' 122(3) . . ?
P2 O5 H2' 122(3) . . ?
P2 O6 Cu1 133.09(9) . . ?
P3 O7 H7' 112(3) . . ?
C7 N1 C11 118.92(19) . . ?
C7 N1 Cu1 126.76(15) . . ?
C11 N1 Cu1 113.73(14) . . ?
C16 N2 C12 119.45(19) . . ?
C16 N2 Cu1 125.42(15) . . ?
C12 N2 Cu1 115.05(14) . . ?
C2 C1 C6 118.68(19) . . ?
C2 C1 P1 122.63(16) . . ?
C6 C1 P1 118.53(15) . . ?
C1 C2 C3 121.02(19) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 119.33(19) . . ?
C4 C3 P2 120.32(15) . . ?
C2 C3 P2 120.24(16) . . ?
C3 C4 C5 120.52(19) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.42(19) . . ?
C6 C5 P3 120.47(16) . . ?
C4 C5 P3 120.07(16) . . ?
C5 C6 C1 120.91(19) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
N1 C7 C8 122.0(2) . . ?
N1 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 119.1(2) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.3(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 118.4(2) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
N1 C11 C10 122.1(2) . . ?
N1 C11 C12 113.90(19) . . ?
C10 C11 C12 123.8(2) . . ?
N2 C12 C13 121.7(2) . . ?
N2 C12 C11 113.65(18) . . ?
C13 C12 C11 124.5(2) . . ?
C12 C13 C14 118.4(2) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 118.3(2) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
N2 C16 C15 122.3(2) . . ?
N2 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?

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
O2 P1 O1 Cu1 98.76(13) . . . 2_655 ?
O3 P1 O1 Cu1 -25.54(14) . . . 2_655 ?
C1 P1 O1 Cu1 -139.40(11) . . . 2_655 ?
O1 P1 O2 Cu1 -99.65(17) . . . 1_455 ?
O3 P1 O2 Cu1 25.29(19) . . . 1_455 ?
C1 P1 O2 Cu1 137.45(16) . . . 1_455 ?
O4 P2 O6 Cu1 178.08(11) . . . . ?
O5 P2 O6 Cu1 -54.17(15) . . . . ?
C3 P2 O6 Cu1 58.42(15) . . . . ?
O2 Cu1 O6 P2 118.42(13) 1_655 . . . ?
O1 Cu1 O6 P2 -146.23(13) 2_655 . . . ?
N2 Cu1 O6 P2 -56.43(14) . . . . ?
N1 Cu1 O6 P2 26.05(15) . . . . ?
O2 Cu1 N1 C7 -16.41(19) 1_655 . . . ?
O1 Cu1 N1 C7 -126.9(2) 2_655 . . . ?
N2 Cu1 N1 C7 172.1(2) . . . . ?
O6 Cu1 N1 C7 75.41(19) . . . . ?
O2 Cu1 N1 C11 154.63(15) 1_655 . . . ?
O1 Cu1 N1 C11 44.1(3) 2_655 . . . ?
N2 Cu1 N1 C11 -16.90(15) . . . . ?
O6 Cu1 N1 C11 -113.56(15) . . . . ?
O2 Cu1 N2 C16 143.9(3) 1_655 . . . ?
O1 Cu1 N2 C16 29.44(18) 2_655 . . . ?
N1 Cu1 N2 C16 -168.56(19) . . . . ?
O6 Cu1 N2 C16 -62.77(18) . . . . ?
O2 Cu1 N2 C12 -32.7(4) 1_655 . . . ?
O1 Cu1 N2 C12 -147.21(15) 2_655 . . . ?
N1 Cu1 N2 C12 14.79(15) . . . . ?
O6 Cu1 N2 C12 120.57(15) . . . . ?
O2 P1 C1 C2 133.35(18) . . . . ?
O1 P1 C1 C2 5.2(2) . . . . ?
O3 P1 C1 C2 -111.89(19) . . . . ?
O2 P1 C1 C6 -51.35(19) . . . . ?
O1 P1 C1 C6 -179.46(16) . . . . ?
O3 P1 C1 C6 63.41(19) . . . . ?
C6 C1 C2 C3 -2.9(3) . . . . ?
P1 C1 C2 C3 172.40(16) . . . . ?
C1 C2 C3 C4 3.1(3) . . . . ?
C1 C2 C3 P2 -173.16(16) . . . . ?
O6 P2 C3 C4 -95.41(18) . . . . ?
O4 P2 C3 C4 141.93(17) . . . . ?
O5 P2 C3 C4 23.06(19) . . . . ?
O6 P2 C3 C2 80.79(19) . . . . ?
O4 P2 C3 C2 -41.87(19) . . . . ?
O5 P2 C3 C2 -160.74(17) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
P2 C3 C4 C5 175.80(16) . . . . ?
C3 C4 C5 C6 -2.3(3) . . . . ?
C3 C4 C5 P3 175.59(16) . . . . ?
O8 P3 C5 C6 -152.47(17) . . . . ?
O9 P3 C5 C6 -28.1(2) . . . . ?
O7 P3 C5 C6 89.27(18) . . . . ?
O8 P3 C5 C4 29.7(2) . . . . ?
O9 P3 C5 C4 154.03(17) . . . . ?
O7 P3 C5 C4 -88.61(18) . . . . ?
C4 C5 C6 C1 2.5(3) . . . . ?
P3 C5 C6 C1 -175.40(16) . . . . ?
C2 C1 C6 C5 0.1(3) . . . . ?
P1 C1 C6 C5 -175.41(16) . . . . ?
C11 N1 C7 C8 -2.8(3) . . . . ?
Cu1 N1 C7 C8 167.84(17) . . . . ?
N1 C7 C8 C9 -0.3(3) . . . . ?
C7 C8 C9 C10 2.2(3) . . . . ?
C8 C9 C10 C11 -0.9(3) . . . . ?
C7 N1 C11 C10 4.1(3) . . . . ?
Cu1 N1 C11 C10 -167.71(17) . . . . ?
C7 N1 C11 C12 -172.10(19) . . . . ?
Cu1 N1 C11 C12 16.1(2) . . . . ?
C9 C10 C11 N1 -2.2(3) . . . . ?
C9 C10 C11 C12 173.6(2) . . . . ?
C16 N2 C12 C13 -3.2(3) . . . . ?
Cu1 N2 C12 C13 173.71(16) . . . . ?
C16 N2 C12 C11 172.85(19) . . . . ?
Cu1 N2 C12 C11 -10.3(2) . . . . ?
N1 C11 C12 N2 -4.0(3) . . . . ?
C10 C11 C12 N2 179.9(2) . . . . ?
N1 C11 C12 C13 171.9(2) . . . . ?
C10 C11 C12 C13 -4.2(3) . . . . ?
N2 C12 C13 C14 2.2(3) . . . . ?
C11 C12 C13 C14 -173.4(2) . . . . ?
C12 C13 C14 C15 -0.1(3) . . . . ?
C13 C14 C15 C16 -0.9(3) . . . . ?
C12 N2 C16 C15 2.0(3) . . . . ?
Cu1 N2 C16 C15 -174.48(16) . . . . ?
C14 C15 C16 N2 0.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.100

#[Cu(phen){(H2O3P)C6H3(PO3H)2}] ?2H2O 19
data_[Cu(phen){(H2O3P)C6H3(PO3H)2}]?2H2O19
_database_code_depnum_ccdc_archive 'CCDC 734640'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H19 Cu N2 O9 P3, 2(O)'
_chemical_formula_sum            'C18 H19 Cu N2 O11 P3'
_chemical_formula_weight         595.80

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_Hall  -P2yn

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                   7.3298(7)
_cell_length_b                   16.0346(14)
_cell_length_c                   18.8682(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.239(2)
_cell_angle_gamma                90.00
_cell_volume                     2194.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    4869
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.21

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1212
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8311
_exptl_absorpt_correction_T_max  0.8311
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            21453
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         28.00
_reflns_number_total             5298
_reflns_number_gt                5207
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0372P)²+19.8827P] where P=(Fo²+2Fc²)/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_extinction_coef       ?
_refine_ls_number_reflns         5298
_refine_ls_number_parameters     320
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0943
_refine_ls_wR_factor_ref         0.1922
_refine_ls_wR_factor_gt          0.1917
_refine_ls_goodness_of_fit_ref   1.405
_refine_ls_restrained_S_all      1.404
_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 0.21464(10) 0.30750(4) 0.10100(4) 0.01106(19) Uani 1 1 d . . .
P1 P 0.1139(2) 0.30482(9) 0.25651(7) 0.0106(3) Uani 1 1 d . . .
P2 P 0.1142(2) -0.02263(9) 0.34018(8) 0.0098(3) Uani 1 1 d . . .
P3 P 0.1974(2) 0.22429(9) 0.54737(7) 0.0096(3) Uani 1 1 d . . .
O1 O 0.2402(6) 0.2802(2) 0.2032(2) 0.0119(8) Uani 1 1 d . . .
O2 O 0.1468(6) 0.3906(2) 0.2890(2) 0.0161(9) Uani 1 1 d . . .
O3 O -0.0933(6) 0.2959(3) 0.2218(2) 0.0193(9) Uani 1 1 d . . .
H3' H -0.0995 0.2933 0.1770 0.029 Uiso 1 1 calc R . .
O4 O -0.0765(6) -0.0523(3) 0.3541(3) 0.0197(9) Uani 1 1 d . . .
H4' H -0.0654 -0.0969 0.3778 0.030 Uiso 1 1 calc R . .
O5 O 0.2699(6) -0.0714(2) 0.3814(2) 0.0125(8) Uani 1 1 d . . .
O6 O 0.1157(6) -0.0225(3) 0.2585(2) 0.0169(9) Uani 1 1 d . . .
H6' H 0.2062 -0.0503 0.2489 0.025 Uiso 1 1 calc R . .
O7 O 0.3823(6) 0.1982(3) 0.5858(2) 0.0171(9) Uani 1 1 d . . .
O8 O 0.0428(6) 0.1849(3) 0.5819(2) 0.0127(8) Uani 1 1 d . . .
O9 O 0.1704(7) 0.3213(3) 0.5434(2) 0.0173(9) Uani 1 1 d . . .
H9' H 0.2021 0.3420 0.5842 0.026 Uiso 1 1 calc R . .
O90 O 0.8566(7) 0.5000(3) 0.2578(2) 0.0210(10) Uani 1 1 d . . .
O91 O 0.2617(9) 0.3790(4) 0.6701(3) 0.0429(15) Uani 1 1 d . . .
N1 N 0.2272(7) 0.1861(3) 0.0730(2) 0.0109(9) Uani 1 1 d . . .
N2 N 0.1714(7) 0.3239(3) -0.0050(3) 0.0108(9) Uani 1 1 d . . .
C1 C 0.1352(8) 0.2297(4) 0.3283(3) 0.0115(11) Uani 1 1 d . . .
C2 C 0.1205(8) 0.1457(3) 0.3108(3) 0.0089(10) Uani 1 1 d . . .
H2 H 0.1040 0.1291 0.2619 0.011 Uiso 1 1 calc R . .
C3 C 0.1298(8) 0.0854(3) 0.3645(3) 0.0109(11) Uani 1 1 d . . .
C4 C 0.1524(8) 0.1105(3) 0.4358(3) 0.0099(10) Uani 1 1 d . . .
H4 H 0.1572 0.0698 0.4725 0.012 Uiso 1 1 calc R . .
C5 C 0.1683(8) 0.1957(3) 0.4543(3) 0.0106(10) Uani 1 1 d . . .
C6 C 0.1596(8) 0.2552(3) 0.3998(3) 0.0110(11) Uani 1 1 d . . .
H6 H 0.1702 0.3128 0.4113 0.013 Uiso 1 1 calc R . .
C7 C 0.2609(8) 0.1194(4) 0.1137(3) 0.0150(12) Uani 1 1 d . . .
H7 H 0.2826 0.1260 0.1643 0.018 Uiso 1 1 calc R . .
C8 C 0.2654(10) 0.0393(4) 0.0848(3) 0.0201(13) Uani 1 1 d . . .
H8 H 0.2906 -0.0075 0.1155 0.024 Uiso 1 1 calc R . .
C9 C 0.2337(10) 0.0284(4) 0.0122(4) 0.0239(14) Uani 1 1 d . . .
H9 H 0.2357 -0.0259 -0.0077 0.029 Uiso 1 1 calc R . .
C10 C 0.1980(9) 0.0984(4) -0.0330(3) 0.0166(12) Uani 1 1 d . . .
C11 C 0.1980(8) 0.1765(4) 0.0002(3) 0.0126(11) Uani 1 1 d . . .
C12 C 0.1613(10) 0.0947(4) -0.1098(4) 0.0247(14) Uani 1 1 d . . .
H12 H 0.1577 0.0419 -0.1330 0.030 Uiso 1 1 calc R . .
C13 C 0.1318(9) 0.1643(5) -0.1496(3) 0.0240(14) Uani 1 1 d . . .
H13 H 0.1091 0.1598 -0.2004 0.029 Uiso 1 1 calc R . .
C14 C 0.1341(8) 0.2461(4) -0.1166(3) 0.0153(12) Uani 1 1 d . . .
C15 C 0.1682(7) 0.2511(4) -0.0412(3) 0.0089(10) Uani 1 1 d U . .
C16 C 0.1036(9) 0.3217(5) -0.1540(3) 0.0215(14) Uani 1 1 d . . .
H16 H 0.0822 0.3219 -0.2048 0.026 Uiso 1 1 calc R . .
C17 C 0.1049(9) 0.3950(4) -0.1167(3) 0.0193(13) Uani 1 1 d . . .
H17 H 0.0827 0.4465 -0.1414 0.023 Uiso 1 1 calc R . .
C18 C 0.1391(8) 0.3936(4) -0.0421(3) 0.0148(11) Uani 1 1 d . . .
H18 H 0.1391 0.4449 -0.0168 0.018 Uiso 1 1 calc R . .


_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 1.961(4) . ?
Cu1 O5 1.970(4) 2 ?
Cu1 N2 1.997(5) . ?
Cu1 N1 2.023(5) . ?
Cu1 O7 2.414(4) 4_565 ?
P1 O2 1.511(4) . ?
P1 O1 1.513(4) . ?
P1 O3 1.572(5) . ?
P1 C1 1.802(6) . ?
P2 O5 1.505(4) . ?
P2 O4 1.535(5) . ?
P2 O6 1.542(4) . ?
P2 C3 1.791(6) . ?
P3 O7 1.501(4) . ?
P3 O8 1.524(4) . ?
P3 O9 1.568(4) . ?
P3 C5 1.797(6) . ?
O3 H3' 0.8400 . ?
O4 H4' 0.8400 . ?
O5 Cu1 1.970(4) 2_545 ?
O6 H6' 0.8400 . ?
O7 Cu1 2.414(4) 4_666 ?
O9 H9' 0.8400 . ?
N1 C7 1.320(7) . ?
N1 C11 1.368(7) . ?
N2 C18 1.322(7) . ?
N2 C15 1.351(7) . ?
C1 C2 1.387(8) . ?
C1 C6 1.396(8) . ?
C2 C3 1.395(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(8) . ?
C4 C5 1.410(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.411(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.401(8) . ?
C10 C12 1.436(9) . ?
C11 C15 1.429(8) . ?
C12 C13 1.346(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.452(9) . ?
C13 H13 0.9500 . ?
C14 C16 1.403(9) . ?
C14 C15 1.410(7) . ?
C16 C17 1.370(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?

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 O5 93.41(17) . 2 ?
O1 Cu1 N2 173.60(18) . . ?
O5 Cu1 N2 92.07(18) 2 . ?
O1 Cu1 N1 92.32(18) . . ?
O5 Cu1 N1 171.39(19) 2 . ?
N2 Cu1 N1 82.62(19) . . ?
O1 Cu1 O7 93.49(16) . 4_565 ?
O5 Cu1 O7 95.15(17) 2 4_565 ?
N2 Cu1 O7 82.72(17) . 4_565 ?
N1 Cu1 O7 90.90(18) . 4_565 ?
O2 P1 O1 115.5(2) . . ?
O2 P1 O3 109.9(3) . . ?
O1 P1 O3 110.2(2) . . ?
O2 P1 C1 108.2(3) . . ?
O1 P1 C1 109.2(2) . . ?
O3 P1 C1 103.1(3) . . ?
O5 P2 O4 113.1(2) . . ?
O5 P2 O6 113.8(2) . . ?
O4 P2 O6 108.0(3) . . ?
O5 P2 C3 110.8(3) . . ?
O4 P2 C3 106.4(3) . . ?
O6 P2 C3 104.2(2) . . ?
O7 P3 O8 110.7(2) . . ?
O7 P3 O9 113.5(3) . . ?
O8 P3 O9 109.5(2) . . ?
O7 P3 C5 111.9(3) . . ?
O8 P3 C5 108.7(2) . . ?
O9 P3 C5 102.1(2) . . ?
P1 O1 Cu1 127.9(2) . . ?
P1 O3 H3' 109.5 . . ?
P2 O4 H4' 109.5 . . ?
P2 O5 Cu1 128.3(3) . 2_545 ?
P2 O6 H6' 109.5 . . ?
P3 O7 Cu1 153.3(3) . 4_666 ?
P3 O9 H9' 109.5 . . ?
C7 N1 C11 118.9(5) . . ?
C7 N1 Cu1 129.7(4) . . ?
C11 N1 Cu1 111.4(4) . . ?
C18 N2 C15 118.3(5) . . ?
C18 N2 Cu1 129.2(4) . . ?
C15 N2 Cu1 112.5(4) . . ?
C2 C1 C6 120.6(5) . . ?
C2 C1 P1 118.4(4) . . ?
C6 C1 P1 121.0(4) . . ?
C1 C2 C3 120.4(5) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 119.2(5) . . ?
C4 C3 P2 121.5(4) . . ?
C2 C3 P2 119.3(4) . . ?
C3 C4 C5 121.0(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 119.0(5) . . ?
C6 C5 P3 122.1(4) . . ?
C4 C5 P3 118.9(4) . . ?
C1 C6 C5 119.8(5) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
N1 C7 C8 122.0(6) . . ?
N1 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 120.0(6) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.6(6) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 116.9(5) . . ?
C11 C10 C12 118.5(6) . . ?
C9 C10 C12 124.6(6) . . ?
N1 C11 C10 122.7(5) . . ?
N1 C11 C15 116.4(5) . . ?
C10 C11 C15 120.9(5) . . ?
C13 C12 C10 121.4(6) . . ?
C13 C12 H12 119.3 . . ?
C10 C12 H12 119.3 . . ?
C12 C13 C14 121.2(6) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C16 C14 C15 116.8(6) . . ?
C16 C14 C13 125.0(5) . . ?
C15 C14 C13 118.3(6) . . ?
N2 C15 C14 123.2(5) . . ?
N2 C15 C11 117.1(5) . . ?
C14 C15 C11 119.7(5) . . ?
C17 C16 C14 119.6(5) . . ?
C17 C16 H16 120.2 . . ?
C14 C16 H16 120.2 . . ?
C16 C17 C18 119.4(6) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
N2 C18 C17 122.8(6) . . ?
N2 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?

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
O2 P1 O1 Cu1 -83.5(3) . . . . ?
O3 P1 O1 Cu1 41.8(4) . . . . ?
C1 P1 O1 Cu1 154.4(3) . . . . ?
O5 Cu1 O1 P1 61.2(3) 2 . . . ?
N2 Cu1 O1 P1 -87.7(17) . . . . ?
N1 Cu1 O1 P1 -125.3(3) . . . . ?
O7 Cu1 O1 P1 -34.2(3) 4_565 . . . ?
O4 P2 O5 Cu1 40.8(4) . . . 2_545 ?
O6 P2 O5 Cu1 -82.9(4) . . . 2_545 ?
C3 P2 O5 Cu1 160.2(3) . . . 2_545 ?
O8 P3 O7 Cu1 174.5(5) . . . 4_666 ?
O9 P3 O7 Cu1 -61.9(6) . . . 4_666 ?
C5 P3 O7 Cu1 53.1(7) . . . 4_666 ?
O1 Cu1 N1 C7 -6.2(5) . . . . ?
O5 Cu1 N1 C7 125.5(12) 2 . . . ?
N2 Cu1 N1 C7 177.8(5) . . . . ?
O7 Cu1 N1 C7 -99.7(5) 4_565 . . . ?
O1 Cu1 N1 C11 174.9(4) . . . . ?
O5 Cu1 N1 C11 -53.4(14) 2 . . . ?
N2 Cu1 N1 C11 -1.1(4) . . . . ?
O7 Cu1 N1 C11 81.4(4) 4_565 . . . ?
O1 Cu1 N2 C18 140.1(16) . . . . ?
O5 Cu1 N2 C18 -8.8(5) 2 . . . ?
N1 Cu1 N2 C18 178.0(5) . . . . ?
O7 Cu1 N2 C18 86.1(5) 4_565 . . . ?
O1 Cu1 N2 C15 -36.8(19) . . . . ?
O5 Cu1 N2 C15 174.3(4) 2 . . . ?
N1 Cu1 N2 C15 1.1(4) . . . . ?
O7 Cu1 N2 C15 -90.7(4) 4_565 . . . ?
O2 P1 C1 C2 -176.5(4) . . . . ?
O1 P1 C1 C2 -50.0(5) . . . . ?
O3 P1 C1 C2 67.2(5) . . . . ?
O2 P1 C1 C6 5.7(6) . . . . ?
O1 P1 C1 C6 132.1(5) . . . . ?
O3 P1 C1 C6 -110.7(5) . . . . ?
C6 C1 C2 C3 0.0(9) . . . . ?
P1 C1 C2 C3 -177.8(4) . . . . ?
C1 C2 C3 C4 0.5(9) . . . . ?
C1 C2 C3 P2 -179.0(4) . . . . ?
O5 P2 C3 C4 -50.2(6) . . . . ?
O4 P2 C3 C4 73.1(5) . . . . ?
O6 P2 C3 C4 -173.0(5) . . . . ?
O5 P2 C3 C2 129.3(5) . . . . ?
O4 P2 C3 C2 -107.4(5) . . . . ?
O6 P2 C3 C2 6.6(5) . . . . ?
C2 C3 C4 C5 -0.8(9) . . . . ?
P2 C3 C4 C5 178.7(4) . . . . ?
C3 C4 C5 C6 0.5(8) . . . . ?
C3 C4 C5 P3 -179.9(4) . . . . ?
O7 P3 C5 C6 -111.7(5) . . . . ?
O8 P3 C5 C6 125.8(5) . . . . ?
O9 P3 C5 C6 10.0(5) . . . . ?
O7 P3 C5 C4 68.8(5) . . . . ?
O8 P3 C5 C4 -53.8(5) . . . . ?
O9 P3 C5 C4 -169.5(5) . . . . ?
C2 C1 C6 C5 -0.4(8) . . . . ?
P1 C1 C6 C5 177.4(4) . . . . ?
C4 C5 C6 C1 0.1(8) . . . . ?
P3 C5 C6 C1 -179.4(4) . . . . ?
C11 N1 C7 C8 -0.7(9) . . . . ?
Cu1 N1 C7 C8 -179.6(5) . . . . ?
N1 C7 C8 C9 -0.3(10) . . . . ?
C7 C8 C9 C10 0.5(11) . . . . ?
C8 C9 C10 C11 0.2(10) . . . . ?
C8 C9 C10 C12 -179.4(7) . . . . ?
C7 N1 C11 C10 1.5(9) . . . . ?
Cu1 N1 C11 C10 -179.4(5) . . . . ?
C7 N1 C11 C15 -178.0(5) . . . . ?
Cu1 N1 C11 C15 1.0(6) . . . . ?
C9 C10 C11 N1 -1.2(9) . . . . ?
C12 C10 C11 N1 178.4(6) . . . . ?
C9 C10 C11 C15 178.3(6) . . . . ?
C12 C10 C11 C15 -2.0(9) . . . . ?
C11 C10 C12 C13 1.6(10) . . . . ?
C9 C10 C12 C13 -178.7(7) . . . . ?
C10 C12 C13 C14 -0.6(11) . . . . ?
C12 C13 C14 C16 -179.5(7) . . . . ?
C12 C13 C14 C15 0.0(10) . . . . ?
C18 N2 C15 C14 0.7(8) . . . . ?
Cu1 N2 C15 C14 177.9(4) . . . . ?
C18 N2 C15 C11 -178.1(5) . . . . ?
Cu1 N2 C15 C11 -0.9(6) . . . . ?
C16 C14 C15 N2 0.4(8) . . . . ?
C13 C14 C15 N2 -179.2(5) . . . . ?
C16 C14 C15 C11 179.2(5) . . . . ?
C13 C14 C15 C11 -0.4(8) . . . . ?
N1 C11 C15 N2 -0.1(8) . . . . ?
C10 C11 C15 N2 -179.6(5) . . . . ?
N1 C11 C15 C14 -179.0(5) . . . . ?
C10 C11 C15 C14 1.5(8) . . . . ?
C15 C14 C16 C17 -1.1(9) . . . . ?
C13 C14 C16 C17 178.4(6) . . . . ?
C14 C16 C17 C18 0.9(9) . . . . ?
C15 N2 C18 C17 -1.0(9) . . . . ?
Cu1 N2 C18 C17 -177.7(4) . . . . ?
C16 C17 C18 N2 0.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.163

#[Cu(bpa){(H2O3P)C6H3(PO3H)2}] ?H2O 20
data_[Cu(bpa){(H2O3P)C6H3(PO3H)2}]?H2O20
_database_code_depnum_ccdc_archive 'CCDC 734641'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 Cu N3 O9 P3, H2 O'
_chemical_formula_sum            'C16 H18 Cu N3 O10 P3'
_chemical_formula_weight         568.78

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  -P1

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

_cell_length_a                   9.9542(14)
_cell_length_b                   10.0152(14)
_cell_length_c                   12.0621(16)
_cell_angle_alpha                100.631(2)
_cell_angle_beta                 106.609(2)
_cell_angle_gamma                115.494(2)
_cell_volume                     972.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    3419
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             578
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8132
_exptl_absorpt_correction_T_max  0.8937
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_detector_area_resol_mean 512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.001
_diffrn_reflns_number            9702
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         28.08
_reflns_number_total             4689
_reflns_number_gt                4151
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker, 2002)'
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2002)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² 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/[σ²(Fo²)+(0.0470P)²+2.5842P] where P=(Fo²+2Fc²)/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         4689
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1196
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_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 0.75840(5) 0.98392(5) 0.62032(4) 0.00900(12) Uani 1 1 d . . .
P1 P 0.64060(10) 0.77479(10) 0.81551(8) 0.00900(18) Uani 1 1 d . . .
P2 P 1.19996(10) 0.76043(10) 0.86384(8) 0.01024(18) Uani 1 1 d . . .
P3 P 0.60181(10) 0.21201(10) 0.58546(8) 0.00910(18) Uani 1 1 d . . .
O1 O 0.4888(3) 0.6657(3) 0.8295(3) 0.0138(5) Uani 1 1 d . . .
O2 O 0.7729(3) 0.9117(3) 0.9390(3) 0.0191(6) Uani 1 1 d . . .
O3 O 0.6084(3) 0.8380(3) 0.7122(2) 0.0156(5) Uani 1 1 d . . .
O4 O 1.2439(3) 0.6817(3) 0.7712(2) 0.0159(5) Uani 1 1 d . . .
O5 O 1.2431(3) 0.7244(3) 0.9854(3) 0.0161(5) Uani 1 1 d . . .
O6 O 1.2699(3) 0.9358(3) 0.8920(2) 0.0139(5) Uani 1 1 d . . .
O7 O 0.4219(3) 0.1499(3) 0.5472(2) 0.0111(5) Uani 1 1 d . . .
O8 O 0.6454(3) 0.2215(3) 0.4699(2) 0.0141(5) Uani 1 1 d . . .
O9 O 0.6692(3) 0.1231(3) 0.6465(2) 0.0116(5) Uani 1 1 d . . .
O90 O 0.5097(4) 0.8903(4) 0.1826(3) 0.0286(7) Uani 1 1 d . . .
N1 N 0.8611(3) 0.8585(3) 0.5847(3) 0.0103(5) Uani 1 1 d . . .
N2 N 0.9713(3) 1.1448(3) 0.7613(3) 0.0108(6) Uani 1 1 d . . .
N3 N 1.1279(4) 1.0810(4) 0.6710(3) 0.0153(6) Uani 1 1 d . . .
C1 C 0.7357(4) 0.6635(4) 0.7861(3) 0.0080(6) Uani 1 1 d . . .
C2 C 0.9047(4) 0.7422(4) 0.8255(3) 0.0093(6) Uani 1 1 d . . .
H2 H 0.9682 0.8532 0.8696 0.011 Uiso 1 1 calc R . .
C3 C 0.9811(4) 0.6592(4) 0.8007(3) 0.0080(6) Uani 1 1 d . . .
C4 C 0.8868(4) 0.4969(4) 0.7327(3) 0.0101(6) Uani 1 1 d . . .
H4 H 0.9388 0.4403 0.7156 0.012 Uiso 1 1 calc R . .
C5 C 0.7165(4) 0.4167(4) 0.6895(3) 0.0091(6) Uani 1 1 d . . .
C6 C 0.6414(4) 0.5001(4) 0.7185(3) 0.0088(6) Uani 1 1 d . . .
H6 H 0.5263 0.4460 0.6924 0.011 Uiso 1 1 calc R . .
C7 C 0.7607(4) 0.6996(4) 0.5230(3) 0.0131(7) Uani 1 1 d . . .
H7 H 0.6501 0.6528 0.5126 0.016 Uiso 1 1 calc R . .
C8 C 0.8108(5) 0.6040(4) 0.4753(3) 0.0159(7) Uani 1 1 d . . .
H8 H 0.7362 0.4939 0.4313 0.019 Uiso 1 1 calc R . .
C9 C 0.9744(5) 0.6719(5) 0.4925(3) 0.0171(7) Uani 1 1 d . . .
H9 H 1.0120 0.6087 0.4587 0.021 Uiso 1 1 calc R . .
C10 C 1.0800(5) 0.8305(5) 0.5588(3) 0.0158(7) Uani 1 1 d . . .
H10 H 1.1920 0.8782 0.5731 0.019 Uiso 1 1 calc R . .
C11 C 1.0194(4) 0.9213(4) 0.6050(3) 0.0116(6) Uani 1 1 d . . .
C12 C 1.1175(4) 1.1800(4) 0.7597(3) 0.0121(7) Uani 1 1 d . . .
C13 C 1.2625(4) 1.3184(4) 0.8448(4) 0.0171(7) Uani 1 1 d . . .
H13 H 1.3632 1.3431 0.8392 0.021 Uiso 1 1 calc R . .
C14 C 1.2573(4) 1.4171(4) 0.9359(4) 0.0179(7) Uani 1 1 d . . .
H14 H 1.3539 1.5127 0.9933 0.021 Uiso 1 1 calc R . .
C15 C 1.1078(4) 1.3757(4) 0.9436(3) 0.0143(7) Uani 1 1 d . . .
H15 H 1.1019 1.4399 1.0085 0.017 Uiso 1 1 calc R . .
C16 C 0.9707(4) 1.2413(4) 0.8562(3) 0.0129(7) Uani 1 1 d . . .
H16 H 0.8695 1.2136 0.8619 0.015 Uiso 1 1 calc R . .
H1' H 0.432(9) 0.669(9) 0.821(7) 0.07(3) Uiso 1 1 d . . .
H2' H 0.747(6) 0.933(6) 0.980(5) 0.021(14) Uiso 1 1 d . . .
H5' H 1.325(8) 0.792(7) 1.036(6) 0.049(18) Uiso 1 1 d . . .
H8' H 0.558(8) 0.209(8) 0.406(6) 0.06(2) Uiso 1 1 d . . .
H3'' H 1.221(6) 1.110(6) 0.675(5) 0.030(13) Uiso 1 1 d . . .
H90A H 0.485(8) 0.952(8) 0.227(7) 0.06(2) Uiso 1 1 d . . .
H90B H 0.577(8) 0.952(8) 0.166(6) 0.052(19) Uiso 1 1 d . . .


_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 O9 1.974(2) 1_565 ?
Cu1 O7 1.990(2) 2_666 ?
Cu1 N1 1.992(3) . ?
Cu1 N2 1.992(3) . ?
Cu1 O3 2.293(3) . ?
P1 O3 1.514(3) . ?
P1 O1 1.516(3) . ?
P1 O2 1.551(3) . ?
P1 C1 1.794(3) . ?
P1 H1' 1.90(7) . ?
P2 O6 1.509(3) . ?
P2 O4 1.521(2) . ?
P2 O5 1.560(3) . ?
P2 C3 1.794(3) . ?
P3 O9 1.502(2) . ?
P3 O7 1.506(2) . ?
P3 O8 1.581(3) . ?
P3 C5 1.816(3) . ?
O1 H1' 0.56(7) . ?
O2 H2' 0.66(5) . ?
O5 H5' 0.76(7) . ?
O7 Cu1 1.990(2) 2_666 ?
O8 H8' 0.92(7) . ?
O9 Cu1 1.974(2) 1_545 ?
O90 H90A 0.90(7) . ?
O90 H90B 0.80(7) . ?
N1 C11 1.344(4) . ?
N1 C7 1.361(5) . ?
N2 C12 1.348(4) . ?
N2 C16 1.359(4) . ?
N3 C12 1.378(5) . ?
N3 C11 1.382(5) . ?
N3 H3'' 0.83(5) . ?
C1 C2 1.393(4) . ?
C1 C6 1.404(5) . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.397(5) . ?
C4 C5 1.399(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.367(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.400(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.407(5) . ?
C10 H10 0.9500 . ?
C12 C13 1.401(5) . ?
C13 C14 1.365(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.363(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
O9 Cu1 O7 91.47(10) 1_565 2_666 ?
O9 Cu1 N1 173.65(11) 1_565 . ?
O7 Cu1 N1 88.11(11) 2_666 . ?
O9 Cu1 N2 90.68(11) 1_565 . ?
O7 Cu1 N2 164.25(11) 2_666 . ?
N1 Cu1 N2 88.05(12) . . ?
O9 Cu1 O3 87.59(10) 1_565 . ?
O7 Cu1 O3 91.97(10) 2_666 . ?
N1 Cu1 O3 98.76(11) . . ?
N2 Cu1 O3 103.72(11) . . ?
O3 P1 O1 114.45(16) . . ?
O3 P1 O2 110.78(16) . . ?
O1 P1 O2 112.19(17) . . ?
O3 P1 C1 109.10(15) . . ?
O1 P1 C1 106.85(16) . . ?
O2 P1 C1 102.68(16) . . ?
O3 P1 H1' 103(2) . . ?
O1 P1 H1' 14(2) . . ?
O2 P1 H1' 113(2) . . ?
C1 P1 H1' 119(2) . . ?
O6 P2 O4 114.82(15) . . ?
O6 P2 O5 110.87(15) . . ?
O4 P2 O5 111.24(15) . . ?
O6 P2 C3 110.13(15) . . ?
O4 P2 C3 106.42(15) . . ?
O5 P2 C3 102.55(15) . . ?
O9 P3 O7 116.77(14) . . ?
O9 P3 O8 108.31(14) . . ?
O7 P3 O8 109.94(14) . . ?
O9 P3 C5 108.00(15) . . ?
O7 P3 C5 109.24(14) . . ?
O8 P3 C5 103.78(15) . . ?
P1 O1 H1' 127(8) . . ?
P1 O2 H2' 117(5) . . ?
P1 O3 Cu1 136.48(15) . . ?
P2 O5 H5' 112(5) . . ?
P3 O7 Cu1 128.09(15) . 2_666 ?
P3 O8 H8' 109(4) . . ?
P3 O9 Cu1 142.69(16) . 1_545 ?
H90A O90 H90B 103(6) . . ?
C11 N1 C7 117.5(3) . . ?
C11 N1 Cu1 124.5(2) . . ?
C7 N1 Cu1 117.5(2) . . ?
C12 N2 C16 117.4(3) . . ?
C12 N2 Cu1 123.7(2) . . ?
C16 N2 Cu1 118.2(2) . . ?
C12 N3 C11 127.8(3) . . ?
C12 N3 H3'' 115(4) . . ?
C11 N3 H3'' 113(4) . . ?
C2 C1 C6 119.8(3) . . ?
C2 C1 P1 119.3(2) . . ?
C6 C1 P1 120.8(2) . . ?
C1 C2 C3 120.4(3) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 P2 119.4(2) . . ?
C4 C3 P2 120.9(2) . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 P3 117.8(2) . . ?
C6 C5 P3 122.8(2) . . ?
C5 C6 C1 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
N1 C7 C8 123.4(3) . . ?
N1 C7 H7 118.3 . . ?
C8 C7 H7 118.3 . . ?
C7 C8 C9 118.5(3) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 118.8(3) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N1 C11 N3 119.9(3) . . ?
N1 C11 C10 122.3(3) . . ?
N3 C11 C10 117.8(3) . . ?
N2 C12 N3 120.3(3) . . ?
N2 C12 C13 122.0(3) . . ?
N3 C12 C13 117.7(3) . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 118.7(3) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
N2 C16 C15 123.3(3) . . ?
N2 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?

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
O1 P1 O3 Cu1 -173.12(19) . . . . ?
O2 P1 O3 Cu1 58.8(3) . . . . ?
C1 P1 O3 Cu1 -53.5(3) . . . . ?
O9 Cu1 O3 P1 -129.1(2) 1_565 . . . ?
O7 Cu1 O3 P1 139.6(2) 2_666 . . . ?
N1 Cu1 O3 P1 51.2(2) . . . . ?
N2 Cu1 O3 P1 -39.0(2) . . . . ?
O9 P3 O7 Cu1 -99.7(2) . . . 2_666 ?
O8 P3 O7 Cu1 24.2(2) . . . 2_666 ?
C5 P3 O7 Cu1 137.44(18) . . . 2_666 ?
O7 P3 O9 Cu1 109.9(3) . . . 1_545 ?
O8 P3 O9 Cu1 -14.8(3) . . . 1_545 ?
C5 P3 O9 Cu1 -126.6(2) . . . 1_545 ?
O9 Cu1 N1 C11 46.4(11) 1_565 . . . ?
O7 Cu1 N1 C11 132.6(3) 2_666 . . . ?
N2 Cu1 N1 C11 -32.1(3) . . . . ?
O3 Cu1 N1 C11 -135.7(3) . . . . ?
O9 Cu1 N1 C7 -125.9(9) 1_565 . . . ?
O7 Cu1 N1 C7 -39.7(3) 2_666 . . . ?
N2 Cu1 N1 C7 155.6(3) . . . . ?
O3 Cu1 N1 C7 52.0(3) . . . . ?
O9 Cu1 N2 C12 -139.3(3) 1_565 . . . ?
O7 Cu1 N2 C12 -41.4(6) 2_666 . . . ?
N1 Cu1 N2 C12 34.5(3) . . . . ?
O3 Cu1 N2 C12 133.1(3) . . . . ?
O9 Cu1 N2 C16 30.2(3) 1_565 . . . ?
O7 Cu1 N2 C16 128.0(4) 2_666 . . . ?
N1 Cu1 N2 C16 -156.0(3) . . . . ?
O3 Cu1 N2 C16 -57.5(3) . . . . ?
O3 P1 C1 C2 85.9(3) . . . . ?
O1 P1 C1 C2 -149.9(3) . . . . ?
O2 P1 C1 C2 -31.7(3) . . . . ?
O3 P1 C1 C6 -90.7(3) . . . . ?
O1 P1 C1 C6 33.5(3) . . . . ?
O2 P1 C1 C6 151.7(3) . . . . ?
C6 C1 C2 C3 -1.5(5) . . . . ?
P1 C1 C2 C3 -178.1(3) . . . . ?
C1 C2 C3 C4 1.9(5) . . . . ?
C1 C2 C3 P2 -174.7(3) . . . . ?
O6 P2 C3 C2 -23.4(3) . . . . ?
O4 P2 C3 C2 -148.4(3) . . . . ?
O5 P2 C3 C2 94.7(3) . . . . ?
O6 P2 C3 C4 160.1(3) . . . . ?
O4 P2 C3 C4 35.0(3) . . . . ?
O5 P2 C3 C4 -81.9(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
P2 C3 C4 C5 176.4(3) . . . . ?
C3 C4 C5 C6 -2.0(5) . . . . ?
C3 C4 C5 P3 172.3(3) . . . . ?
O9 P3 C5 C4 53.7(3) . . . . ?
O7 P3 C5 C4 -178.3(3) . . . . ?
O8 P3 C5 C4 -61.1(3) . . . . ?
O9 P3 C5 C6 -132.2(3) . . . . ?
O7 P3 C5 C6 -4.2(3) . . . . ?
O8 P3 C5 C6 113.0(3) . . . . ?
C4 C5 C6 C1 2.4(5) . . . . ?
P3 C5 C6 C1 -171.6(3) . . . . ?
C2 C1 C6 C5 -0.7(5) . . . . ?
P1 C1 C6 C5 175.9(3) . . . . ?
C11 N1 C7 C8 -3.8(5) . . . . ?
Cu1 N1 C7 C8 169.0(3) . . . . ?
N1 C7 C8 C9 1.2(5) . . . . ?
C7 C8 C9 C10 1.5(5) . . . . ?
C8 C9 C10 C11 -1.5(5) . . . . ?
C7 N1 C11 N3 -177.7(3) . . . . ?
Cu1 N1 C11 N3 10.0(5) . . . . ?
C7 N1 C11 C10 3.8(5) . . . . ?
Cu1 N1 C11 C10 -168.5(3) . . . . ?
C12 N3 C11 N1 26.8(5) . . . . ?
C12 N3 C11 C10 -154.7(4) . . . . ?
C9 C10 C11 N1 -1.2(5) . . . . ?
C9 C10 C11 N3 -179.7(3) . . . . ?
C16 N2 C12 N3 175.4(3) . . . . ?
Cu1 N2 C12 N3 -15.0(5) . . . . ?
C16 N2 C12 C13 -6.0(5) . . . . ?
Cu1 N2 C12 C13 163.5(3) . . . . ?
C11 N3 C12 N2 -24.0(6) . . . . ?
C11 N3 C12 C13 157.4(4) . . . . ?
N2 C12 C13 C14 3.1(6) . . . . ?
N3 C12 C13 C14 -178.3(3) . . . . ?
C12 C13 C14 C15 1.5(6) . . . . ?
C13 C14 C15 C16 -3.0(5) . . . . ?
C12 N2 C16 C15 4.5(5) . . . . ?
Cu1 N2 C16 C15 -165.6(3) . . . . ?
C14 C15 C16 N2 -0.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.08
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.127


