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


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Hegen Zheng'
_publ_contact_author_email       zhenghg@nju.edu.cn
_publ_author_name                'Hegen Zheng'

data_1
_database_code_depnum_ccdc_archive 'CCDC 893081'
#TrackingRef '- 1-new.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H21 Cu N2 O7.5'
_chemical_formula_weight         436.86

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   ' Fddd'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   16.6727(11)
_cell_length_b                   30.982(2)
_cell_length_c                   33.554(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17332.5(19)
_cell_formula_units_Z            32
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7274
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8203
_exptl_absorpt_correction_T_max  0.8950
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23442
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3811
_reflns_number_gt                3200
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SMART (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;

TITL L42-Cu in Fddd
CELL 0.71073 16.6727 30.9822 33.5539 90.000 90.000 90.000
ZERR 32.00 0.0011 0.0020 0.0021 0.000 0.000 0.000
LATT 4
SYMM 0.75-X, 0.75-Y, Z
SYMM 0.75-X, Y, 0.75-Z
SYMM X, 0.75-Y, 0.75-Z
SFAC C H N O Cu
UNIT 544 512 64 160 32
omit 0 10 2
omit 1 7 7
omit 2 0 6
omit 6 10 0
omit 1 3 9
omit 4 4 4
omit 4 0 4
omit 0 2 2
omit 3 7 7
omit 3 3 9
omit 0 8 4
omit 1 5 5
omit 2 2 8
omit 0 4 4
omit 2 2 0
omit 2 2 2
omit 1 3 7
omit 2 4 14
omit 1 1 7
omit 1 1 1
omit 1 9 3
omit 1 5 13
OMIT -2.00 50.06
L.S. 8
ACTA
BOND $h
FMAP 2
PLAN 0
size 0.20 0.16 0.11
conf
delu 0.001 cu1 o2 o3 o4 o5 c15
delu 0.001 N3' C17' N3 C15 N3 C17
simu Cu1 O2
delu 0.001 N3' C15 O5 C15'
isor 0.001 n17 n17'
delu 0.01 n17 n17'
sadi n3 c16 n3' c16'
sadi n3 c17 n3' c17'
sadi c15' n3' c15 n3
sadi c15' o5 c15 o5
WGHT 0.084200 193.744100
FVAR 0.247430 0.474820
TEMP 23.000

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+193.7441P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3811
_refine_ls_number_parameters     261
_refine_ls_number_restraints     256
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1667
_refine_ls_wR_factor_gt          0.1583
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.169
_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
O3 O 0.5801(2) 0.44513(11) 0.00844(10) 0.0340(8) Uani 1 1 d U . .
O1 O 0.5801(2) 0.49822(11) -0.05536(10) 0.0327(8) Uani 1 1 d U . .
O2 O 0.5885(2) 0.55141(11) -0.01049(10) 0.0333(6) Uani 1 1 d U . .
C1 C 0.6824(3) 0.54992(15) -0.06252(14) 0.0277(10) Uani 1 1 d U . .
C2 C 0.7170(3) 0.52802(17) -0.09462(15) 0.0360(11) Uani 1 1 d U . .
H2 H 0.6955 0.5017 -0.1027 0.043 Uiso 1 1 calc R . .
C3 C 0.7817(3) 0.54456(17) -0.11437(16) 0.0370(11) Uani 1 1 d U . .
H3 H 0.8049 0.5290 -0.1351 0.044 Uiso 1 1 calc R . .
C4 C 0.8134(3) 0.58457(15) -0.10364(14) 0.0293(10) Uani 1 1 d U . .
C5 C 0.7791(3) 0.60653(16) -0.07177(14) 0.0307(10) Uani 1 1 d U . .
H5 H 0.8001 0.6330 -0.0640 0.037 Uiso 1 1 calc R . .
C6 C 0.7148(3) 0.58973(15) -0.05161(14) 0.0298(10) Uani 1 1 d U . .
H6 H 0.6926 0.6050 -0.0305 0.036 Uiso 1 1 calc R . .
C7 C 0.6121(3) 0.53181(14) -0.04120(14) 0.0271(10) Uani 1 1 d U . .
C8 C 0.6110(3) 0.46302(14) 0.03860(14) 0.0271(10) Uani 1 1 d U A .
C9 C 0.6821(3) 0.44083(15) 0.05669(14) 0.0286(10) Uani 1 1 d U . .
C10 C 0.7132(3) 0.45378(15) 0.09334(14) 0.0282(10) Uani 1 1 d U . .
H10 H 0.6904 0.4770 0.1068 0.034 Uiso 1 1 calc R . .
C11 C 0.7775(3) 0.43221(15) 0.10975(14) 0.0304(10) Uani 1 1 d U . .
H11 H 0.7974 0.4410 0.1343 0.037 Uiso 1 1 calc R . .
C12 C 0.8134(3) 0.39746(15) 0.09027(14) 0.0307(10) Uani 1 1 d U . .
C13 C 0.7825(3) 0.38538(17) 0.05309(15) 0.0372(11) Uani 1 1 d U . .
H13 H 0.8063 0.3629 0.0391 0.045 Uiso 1 1 calc R . .
C14 C 0.71745(18) 0.40637(10) 0.03702(9) 0.0362(11) Uani 1 1 d U . .
H14 H 0.6969 0.3973 0.0126 0.043 Uiso 1 1 calc R . .
O5 O 0.50899(18) 0.59054(10) 0.06032(9) 0.0418(7) Uani 1 1 d U . .
C15 C 0.4763(7) 0.6231(3) 0.0462(4) 0.0429(11) Uani 0.475(6) 1 d PDU A 1
H15 H 0.4637 0.6284 0.0197 0.052 Uiso 0.475(6) 1 calc PR A 1
N3 N 0.4611(6) 0.6530(3) 0.0823(3) 0.0494(16) Uani 0.475(6) 1 d PDU A 1
C16 C 0.5360(10) 0.6767(6) 0.0774(6) 0.075(4) Uani 0.475(6) 1 d PDU A 1
H16A H 0.5797 0.6567 0.0754 0.113 Uiso 0.475(6) 1 calc PR A 1
H16B H 0.5441 0.6953 0.0999 0.113 Uiso 0.475(6) 1 calc PR A 1
H16C H 0.5333 0.6938 0.0535 0.113 Uiso 0.475(6) 1 calc PR A 1
C17 C 0.3918(8) 0.6747(4) 0.0980(4) 0.0552(18) Uani 0.475(6) 1 d PDU A 1
H17A H 0.3475 0.6549 0.0989 0.083 Uiso 0.475(6) 1 calc PR A 1
H17B H 0.3784 0.6987 0.0812 0.083 Uiso 0.475(6) 1 calc PR A 1
H17C H 0.4032 0.6849 0.1244 0.083 Uiso 0.475(6) 1 calc PR A 1
C15' C 0.4542(6) 0.6135(3) 0.0688(3) 0.0459(13) Uani 0.525(6) 1 d PDU A 2
H15' H 0.4045 0.6049 0.0785 0.055 Uiso 0.525(6) 1 calc PR A 2
N3' N 0.4832(6) 0.6627(3) 0.0601(3) 0.0495(13) Uani 0.525(6) 1 d PDU A 2
C17' C 0.4491(8) 0.7000(4) 0.0403(4) 0.0599(19) Uani 0.525(6) 1 d PDU A 2
H17D H 0.4118 0.6907 0.0203 0.090 Uiso 0.525(6) 1 calc PR A 2
H17E H 0.4912 0.7165 0.0280 0.090 Uiso 0.525(6) 1 calc PR A 2
H17F H 0.4217 0.7177 0.0595 0.090 Uiso 0.525(6) 1 calc PR A 2
C16' C 0.5408(9) 0.6711(5) 0.0930(5) 0.066(4) Uani 0.525(6) 1 d PDU A 2
H16D H 0.5567 0.6442 0.1048 0.098 Uiso 0.525(6) 1 calc PR A 2
H16E H 0.5158 0.6890 0.1128 0.098 Uiso 0.525(6) 1 calc PR A 2
H16F H 0.5872 0.6856 0.0825 0.098 Uiso 0.525(6) 1 calc PR A 2
Cu1 Cu 0.50466(3) 0.531561(17) 0.026097(15) 0.0221(2) Uani 1 1 d U . .
N1 N 0.8750 0.60418(19) -0.1250 0.0348(13) Uani 1 2 d SU . .
H1N H 0.8750 0.6319 -0.1250 0.042 Uiso 1 2 calc SR . .
N2 N 0.8750 0.3750 0.10868(18) 0.0342(13) Uani 1 2 d SU . .
H2N H 0.8750 0.3750 0.1343 0.041 Uiso 1 2 calc SR . .
O4 O 0.5870(2) 0.49779(11) 0.05417(10) 0.0334(6) Uani 1 1 d U . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O3 0.0321(11) 0.0341(11) 0.0358(11) 0.0014(9) -0.0028(9) 0.0026(9)
O1 0.0306(11) 0.0341(11) 0.0334(11) 0.0016(9) 0.0033(9) -0.0023(9)
O2 0.0302(10) 0.0345(11) 0.0351(9) 0.0037(7) 0.0056(8) -0.0043(8)
C1 0.0261(13) 0.0283(13) 0.0286(13) 0.0014(10) 0.0012(10) -0.0001(10)
C2 0.0348(14) 0.0359(14) 0.0374(14) -0.0003(10) 0.0025(10) -0.0007(10)
C3 0.0359(14) 0.0373(14) 0.0378(14) -0.0015(10) 0.0035(10) -0.0009(10)
C4 0.0272(13) 0.0299(13) 0.0306(13) 0.0012(10) 0.0022(10) 0.0005(10)
C5 0.0292(13) 0.0304(13) 0.0324(13) -0.0008(10) 0.0017(10) -0.0004(10)
C6 0.0285(13) 0.0305(13) 0.0303(13) -0.0001(10) 0.0026(10) 0.0000(10)
C7 0.0260(13) 0.0277(13) 0.0277(13) 0.0024(10) -0.0004(10) 0.0006(10)
C8 0.0257(13) 0.0278(13) 0.0278(13) 0.0025(10) 0.0009(10) 0.0002(10)
C9 0.0268(13) 0.0295(13) 0.0295(13) 0.0019(10) 0.0001(10) 0.0006(10)
C10 0.0266(13) 0.0286(13) 0.0294(13) 0.0007(10) 0.0002(10) 0.0006(10)
C11 0.0294(13) 0.0315(13) 0.0304(13) 0.0002(10) -0.0008(10) 0.0008(10)
C12 0.0288(13) 0.0318(13) 0.0315(13) 0.0014(10) 0.0003(10) 0.0023(10)
C13 0.0363(14) 0.0379(14) 0.0373(14) -0.0021(10) -0.0004(10) 0.0031(10)
C14 0.0349(14) 0.0375(14) 0.0362(14) -0.0011(10) -0.0009(10) 0.0023(10)
O5 0.0439(11) 0.0397(8) 0.0417(11) -0.0064(8) 0.0001(9) 0.0017(8)
C15 0.0452(16) 0.0372(10) 0.0464(16) -0.0007(9) -0.0011(11) -0.0010(11)
N3 0.0510(19) 0.0489(19) 0.0484(18) -0.0027(10) 0.0011(11) 0.0006(11)
C16 0.075(4) 0.075(4) 0.075(4) -0.0003(11) -0.0001(11) -0.0007(11)
C17 0.055(2) 0.055(2) 0.055(2) -0.0040(11) 0.0031(11) 0.0038(11)
C15' 0.0448(15) 0.0460(14) 0.0469(17) -0.0012(11) 0.0015(11) 0.0028(9)
N3' 0.0511(17) 0.0461(11) 0.0513(18) -0.0031(11) 0.0014(11) 0.0003(10)
C17' 0.061(2) 0.058(2) 0.061(2) 0.0025(11) -0.0018(11) 0.0027(11)
C16' 0.066(4) 0.065(4) 0.065(4) -0.0001(11) -0.0003(11) -0.0005(11)
Cu1 0.0140(3) 0.0251(3) 0.0271(3) 0.0035(2) 0.0008(2) 0.0003(2)
N1 0.0340(16) 0.0342(16) 0.0363(16) 0.000 0.0031(10) 0.000
N2 0.0331(16) 0.0360(16) 0.0337(16) 0.000 0.000 0.0025(10)
O4 0.0301(10) 0.0358(9) 0.0342(10) 0.0038(8) -0.0050(8) 0.0033(8)

_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
O3 C8 1.264(6) . ?
O3 Cu1 1.964(3) 17_665 ?
O1 C7 1.262(6) . ?
O1 Cu1 1.952(3) 17_665 ?
O2 C7 1.259(6) . ?
O2 Cu1 1.959(3) . ?
C1 C6 1.396(7) . ?
C1 C2 1.398(7) . ?
C1 C7 1.484(6) . ?
C2 C3 1.366(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(7) . ?
C4 N1 1.392(5) . ?
C5 C6 1.369(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 O4 1.263(6) . ?
C8 C9 1.499(6) . ?
C9 C14 1.387(6) . ?
C9 C10 1.393(7) . ?
C10 C11 1.379(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.394(7) . ?
C11 H11 0.9300 . ?
C12 N2 1.386(5) . ?
C12 C13 1.401(7) . ?
C13 C14 1.375(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
O5 C15' 1.192(10) . ?
O5 C15 1.241(11) . ?
O5 Cu1 2.159(3) . ?
C15 N3 1.546(13) . ?
C15 H15 0.9300 . ?
N3 C17 1.436(14) . ?
N3 C16 1.458(16) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C15' N3' 1.626(13) . ?
C15' H15' 0.9300 . ?
N3' C17' 1.450(13) . ?
N3' C16' 1.484(14) . ?
C17' H17D 0.9600 . ?
C17' H17E 0.9600 . ?
C17' H17F 0.9600 . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
Cu1 O1 1.952(3) 17_665 ?
Cu1 O3 1.964(3) 17_665 ?
Cu1 O4 1.966(3) . ?
Cu1 Cu1 2.6298(11) 17_665 ?
N1 C4 1.392(5) 3_654 ?
N1 H1N 0.8600 . ?
N2 C12 1.386(5) 2_655 ?
N2 H2N 0.8600 . ?

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
C8 O3 Cu1 127.2(3) . 17_665 ?
C7 O1 Cu1 120.4(3) . 17_665 ?
C7 O2 Cu1 125.8(3) . . ?
C6 C1 C2 118.1(4) . . ?
C6 C1 C7 120.9(4) . . ?
C2 C1 C7 121.0(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 N1 119.1(4) . . ?
C5 C4 C3 118.6(4) . . ?
N1 C4 C3 122.3(4) . . ?
C6 C5 C4 121.0(4) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O2 C7 O1 125.0(4) . . ?
O2 C7 C1 117.3(4) . . ?
O1 C7 C1 117.6(4) . . ?
O4 C8 O3 125.1(4) . . ?
O4 C8 C9 118.4(4) . . ?
O3 C8 C9 116.5(4) . . ?
C14 C9 C10 119.0(4) . . ?
C14 C9 C8 119.8(4) . . ?
C10 C9 C8 121.3(4) . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 121.4(4) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
N2 C12 C11 119.8(4) . . ?
N2 C12 C13 122.4(5) . . ?
C11 C12 C13 117.8(4) . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.8(4) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
C15' O5 C15 43.1(7) . . ?
C15' O5 Cu1 127.3(6) . . ?
C15 O5 Cu1 118.1(6) . . ?
O5 C15 N3 105.1(9) . . ?
O5 C15 H15 127.4 . . ?
N3 C15 H15 127.4 . . ?
C17 N3 C16 119.7(12) . . ?
C17 N3 C15 134.4(10) . . ?
C16 N3 C15 94.1(11) . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C15' N3' 106.8(8) . . ?
O5 C15' H15' 126.6 . . ?
N3' C15' H15' 126.6 . . ?
C17' N3' C16' 117.0(10) . . ?
C17' N3' C15' 135.5(9) . . ?
C16' N3' C15' 103.0(9) . . ?
N3' C17' H17D 109.5 . . ?
N3' C17' H17E 109.5 . . ?
H17D C17' H17E 109.5 . . ?
N3' C17' H17F 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
N3' C16' H16D 109.5 . . ?
N3' C16' H16E 109.5 . . ?
H16D C16' H16E 109.5 . . ?
N3' C16' H16F 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
O1 Cu1 O2 168.43(14) 17_665 . ?
O1 Cu1 O3 87.14(14) 17_665 17_665 ?
O2 Cu1 O3 91.58(15) . 17_665 ?
O1 Cu1 O4 90.72(14) 17_665 . ?
O2 Cu1 O4 88.25(14) . . ?
O3 Cu1 O4 168.55(14) 17_665 . ?
O1 Cu1 O5 99.02(13) 17_665 . ?
O2 Cu1 O5 92.51(13) . . ?
O3 Cu1 O5 91.52(13) 17_665 . ?
O4 Cu1 O5 99.92(13) . . ?
O1 Cu1 Cu1 86.60(10) 17_665 17_665 ?
O2 Cu1 Cu1 81.85(10) . 17_665 ?
O3 Cu1 Cu1 80.68(10) 17_665 17_665 ?
O4 Cu1 Cu1 87.97(10) . 17_665 ?
O5 Cu1 Cu1 170.20(9) . 17_665 ?
C4 N1 C4 128.3(6) 3_654 . ?
C4 N1 H1N 115.9 3_654 . ?
C4 N1 H1N 115.9 . . ?
C12 N2 C12 127.1(6) . 2_655 ?
C12 N2 H2N 116.5 . . ?
C12 N2 H2N 116.5 2_655 . ?
C8 O4 Cu1 118.5(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
C6 C1 C2 C3 1.3(8) . . . . ?
C7 C1 C2 C3 180.0(5) . . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C2 C3 C4 C5 1.9(8) . . . . ?
C2 C3 C4 N1 -174.6(5) . . . . ?
N1 C4 C5 C6 175.6(4) . . . . ?
C3 C4 C5 C6 -1.0(7) . . . . ?
C4 C5 C6 C1 0.3(7) . . . . ?
C2 C1 C6 C5 -0.4(7) . . . . ?
C7 C1 C6 C5 -179.1(4) . . . . ?
Cu1 O2 C7 O1 7.1(7) . . . . ?
Cu1 O2 C7 C1 -173.5(3) . . . . ?
Cu1 O1 C7 O2 -7.6(6) 17_665 . . . ?
Cu1 O1 C7 C1 173.0(3) 17_665 . . . ?
C6 C1 C7 O2 -7.3(7) . . . . ?
C2 C1 C7 O2 174.0(4) . . . . ?
C6 C1 C7 O1 172.1(4) . . . . ?
C2 C1 C7 O1 -6.6(7) . . . . ?
Cu1 O3 C8 O4 7.3(7) 17_665 . . . ?
Cu1 O3 C8 C9 -172.3(3) 17_665 . . . ?
O4 C8 C9 C14 -170.4(4) . . . . ?
O3 C8 C9 C14 9.3(6) . . . . ?
O4 C8 C9 C10 10.5(7) . . . . ?
O3 C8 C9 C10 -169.8(4) . . . . ?
C14 C9 C10 C11 -0.6(7) . . . . ?
C8 C9 C10 C11 178.6(4) . . . . ?
C9 C10 C11 C12 0.5(7) . . . . ?
C10 C11 C12 N2 -176.3(4) . . . . ?
C10 C11 C12 C13 0.8(7) . . . . ?
N2 C12 C13 C14 175.1(4) . . . . ?
C11 C12 C13 C14 -1.9(7) . . . . ?
C12 C13 C14 C9 1.8(7) . . . . ?
C10 C9 C14 C13 -0.6(6) . . . . ?
C8 C9 C14 C13 -179.7(4) . . . . ?
C15' O5 C15 N3 43.3(9) . . . . ?
Cu1 O5 C15 N3 159.1(6) . . . . ?
O5 C15 N3 C17 -126.5(14) . . . . ?
O5 C15 N3 C16 93.5(12) . . . . ?
C15 O5 C15' N3' -41.5(9) . . . . ?
Cu1 O5 C15' N3' -134.5(6) . . . . ?
O5 C15' N3' C17' 133.3(13) . . . . ?
O5 C15' N3' C16' -72.6(11) . . . . ?
C7 O2 Cu1 O1 0.3(9) . . . 17_665 ?
C7 O2 Cu1 O3 -83.1(4) . . . 17_665 ?
C7 O2 Cu1 O4 85.4(4) . . . . ?
C7 O2 Cu1 O5 -174.7(4) . . . . ?
C7 O2 Cu1 Cu1 -2.8(4) . . . 17_665 ?
C15' O5 Cu1 O1 -51.6(7) . . . 17_665 ?
C15 O5 Cu1 O1 -102.2(7) . . . 17_665 ?
C15' O5 Cu1 O2 127.4(7) . . . . ?
C15 O5 Cu1 O2 76.8(7) . . . . ?
C15' O5 Cu1 O3 35.7(7) . . . 17_665 ?
C15 O5 Cu1 O3 -14.9(7) . . . 17_665 ?
C15' O5 Cu1 O4 -144.0(7) . . . . ?
C15 O5 Cu1 O4 165.4(7) . . . . ?
C15' O5 Cu1 Cu1 72.8(9) . . . 17_665 ?
C15 O5 Cu1 Cu1 22.2(10) . . . 17_665 ?
C5 C4 N1 C4 153.1(5) . . . 3_654 ?
C3 C4 N1 C4 -30.4(4) . . . 3_654 ?
C11 C12 N2 C12 -152.6(5) . . . 2_655 ?
C13 C12 N2 C12 30.4(4) . . . 2_655 ?
O3 C8 O4 Cu1 -8.7(6) . . . . ?
C9 C8 O4 Cu1 170.9(3) . . . . ?
O1 Cu1 O4 C8 91.9(3) 17_665 . . . ?
O2 Cu1 O4 C8 -76.6(3) . . . . ?
O3 Cu1 O4 C8 12.8(9) 17_665 . . . ?
O5 Cu1 O4 C8 -168.8(3) . . . . ?
Cu1 Cu1 O4 C8 5.3(3) 17_665 . . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.480 -0.017 -0.014 4747 842 ' '

_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of
diffuse solvent which could not be sensibly modelled
in terms of atomic sites. Their contribution to the
diffraction pattern was removed and modified F(obs)**2
written to a new HKL file. The number of electrons thus located,
842 per unit cell, is included in the formula, formula weight,
calculated density, and F(000). This residual electron density
was assigned to two and one half molecules of the water solvent,
[842/32 = 26e per ligand; two and one half molecules
of the water would give 25e].
;
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.752
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.098

# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.90 <> 1.10
From the CIF: _cell_formula_units_Z 32
From the CIF: _chemical_formula_weight 436.86
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 17.00 204.19
H 1.01 16.00 16.13
N 14.01 2.00 28.01
O 16.00 5.00 79.99
Cu 63.55 1.00 63.55
Calculated formula weight 391.87

RESPONSE: The contribution of any disordered solvent removed by
the SQUEEZE process has now been included in the overall
formula, formula weight, density, F(000), etc.,
;
# end Validation Reply Form

# Attachment '- 2-new.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 893082'
#TrackingRef '- 2-new.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H22 Cu2 N2 O11.5'
_chemical_formula_sum            'C28 H22 Cu2 N2 O11.5'
_chemical_formula_weight         697.55

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

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I4(1)22 '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'-x+1/2, y, -z+3/4'
'x, -y+1/2, -z+1/4'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'-x+1, y+1/2, -z+5/4'
'x+1/2, -y+1, -z+3/4'
'y+1, x+1, -z+1'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   16.6307(8)
_cell_length_b                   16.6307(8)
_cell_length_c                   16.3071(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4510.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cubic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1414
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7708
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12547
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2001
_reflns_number_gt                1703
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SMART (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(1)
_refine_ls_number_reflns         2001
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.5766(2) 0.4282(2) 0.11231(19) 0.0410(8) Uani 1 1 d . . .
C2 C 0.6207(2) 0.3902(2) 0.18261(18) 0.0413(9) Uani 1 1 d . . .
C3 C 0.5990(2) 0.3161(3) 0.2131(2) 0.0457(10) Uani 1 1 d . . .
H3 H 0.5558 0.2890 0.1897 0.055 Uiso 1 1 calc R . .
C4 C 0.6401(2) 0.2811(2) 0.2777(2) 0.0454(11) Uani 1 1 d . . .
H4 H 0.6251 0.2309 0.2975 0.055 Uiso 1 1 calc R . .
C5 C 0.7046(2) 0.3228(2) 0.3128(2) 0.0444(10) Uani 1 1 d . . .
C6 C 0.7258(3) 0.3964(3) 0.2814(2) 0.0591(12) Uani 1 1 d . . .
H6 H 0.7689 0.4241 0.3043 0.071 Uiso 1 1 calc R . .
C7 C 0.6854(3) 0.4290(2) 0.2182(2) 0.0504(10) Uani 1 1 d . . .
H7 H 0.7014 0.4787 0.1979 0.061 Uiso 1 1 calc R . .
Cu1 Cu 0.44413(3) 0.44413(3) 0.0000 0.0364(2) Uani 1 2 d S . .
N1 N 0.7500 0.2824(3) 0.3750 0.0526(14) Uani 1 2 d S . .
H1A H 0.7152 0.2499 0.4014 0.063 Uiso 0.25 1 d PR . .
O1 O 0.60478(18) 0.49304(18) 0.08640(15) 0.0514(8) Uani 1 1 d . . .
O2 O 0.3521(2) 0.3521(2) 0.0000 0.1052(17) Uani 1 2 d S . .
H2A H 0.3647 0.3122 -0.0406 0.158 Uiso 0.25 1 d PR . .
H2B H 0.3010 0.3760 -0.0125 0.158 Uiso 0.25 1 d PR . .
O3 O 0.51571(18) 0.39378(18) 0.08397(16) 0.0522(8) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.049(3) 0.049(3) 0.0248(16) -0.0009(17) -0.0010(17) 0.0140(16)
C2 0.050(3) 0.047(3) 0.0269(16) 0.0057(17) -0.0055(17) 0.0075(17)
C3 0.044(2) 0.064(3) 0.0294(18) -0.0065(18) -0.0063(18) 0.007(2)
C4 0.061(3) 0.046(2) 0.029(2) 0.0055(16) -0.0081(17) 0.004(2)
C5 0.056(3) 0.049(2) 0.0286(17) -0.0079(16) -0.0108(17) 0.0048(19)
C6 0.077(3) 0.054(3) 0.045(2) 0.005(2) -0.022(2) -0.007(2)
C7 0.074(3) 0.042(3) 0.0347(19) 0.0034(18) -0.018(2) -0.006(2)
Cu1 0.0428(2) 0.0428(2) 0.0236(3) -0.0005(2) 0.0005(2) 0.0065(3)
N1 0.079(4) 0.053(3) 0.026(2) 0.000 -0.021(2) 0.000
O1 0.0550(19) 0.057(2) 0.0422(16) 0.0133(15) -0.0125(14) 0.0012(16)
O2 0.114(3) 0.114(3) 0.087(4) -0.012(3) 0.012(3) -0.038(3)
O3 0.0560(19) 0.062(2) 0.0390(16) 0.0090(15) -0.0135(14) 0.0073(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.249(5) . ?
C1 O3 1.252(5) . ?
C1 C2 1.500(4) . ?
C2 C3 1.377(6) . ?
C2 C7 1.382(6) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.372(6) . ?
C5 N1 1.433(4) . ?
C6 C7 1.345(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
Cu1 O1 1.934(2) 10_554 ?
Cu1 O1 1.934(2) 8_665 ?
Cu1 O3 1.998(3) . ?
Cu1 O3 1.998(3) 15_444 ?
Cu1 O2 2.165(5) . ?
Cu1 Cu1 2.6281(12) 10_554 ?
N1 C5 1.433(4) 5_655 ?
N1 H1A 0.9000 . ?
O1 Cu1 1.934(2) 10_554 ?
O2 H2A 0.9600 . ?
O2 H2B 0.9600 . ?

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 C1 O3 125.0(3) . . ?
O1 C1 C2 116.0(4) . . ?
O3 C1 C2 119.0(4) . . ?
C3 C2 C7 118.0(3) . . ?
C3 C2 C1 121.6(4) . . ?
C7 C2 C1 120.3(4) . . ?
C2 C3 C4 121.4(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.1(3) . . ?
C6 C5 N1 123.2(4) . . ?
C4 C5 N1 117.4(3) . . ?
C7 C6 C5 121.1(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C2 121.5(4) . . ?
C6 C7 H7 119.2 . . ?
C2 C7 H7 119.2 . . ?
O1 Cu1 O1 170.3(2) 10_554 8_665 ?
O1 Cu1 O3 88.72(10) 10_554 . ?
O1 Cu1 O3 90.06(10) 8_665 . ?
O1 Cu1 O3 90.06(10) 10_554 15_444 ?
O1 Cu1 O3 88.72(10) 8_665 15_444 ?
O3 Cu1 O3 165.65(19) . 15_444 ?
O1 Cu1 O2 94.86(10) 10_554 . ?
O1 Cu1 O2 94.86(10) 8_665 . ?
O3 Cu1 O2 97.18(10) . . ?
O3 Cu1 O2 97.18(10) 15_444 . ?
O1 Cu1 Cu1 85.14(10) 10_554 10_554 ?
O1 Cu1 Cu1 85.14(10) 8_665 10_554 ?
O3 Cu1 Cu1 82.82(10) . 10_554 ?
O3 Cu1 Cu1 82.82(10) 15_444 10_554 ?
O2 Cu1 Cu1 180.00(13) . 10_554 ?
C5 N1 C5 124.0(4) 5_655 . ?
C5 N1 H1A 106.3 5_655 . ?
C5 N1 H1A 106.3 . . ?
C1 O1 Cu1 123.7(3) . 10_554 ?
Cu1 O2 H2A 109.5 . . ?
Cu1 O2 H2B 109.5 . . ?
H2A O2 H2B 109.5 . . ?
C1 O3 Cu1 122.9(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 C1 C2 C3 -175.5(3) . . . . ?
O3 C1 C2 C3 4.3(5) . . . . ?
O1 C1 C2 C7 3.7(5) . . . . ?
O3 C1 C2 C7 -176.4(3) . . . . ?
C7 C2 C3 C4 0.4(5) . . . . ?
C1 C2 C3 C4 179.7(3) . . . . ?
C2 C3 C4 C5 0.4(5) . . . . ?
C3 C4 C5 C6 -0.8(6) . . . . ?
C3 C4 C5 N1 -175.0(3) . . . . ?
C4 C5 C6 C7 0.4(6) . . . . ?
N1 C5 C6 C7 174.2(3) . . . . ?
C5 C6 C7 C2 0.5(6) . . . . ?
C3 C2 C7 C6 -0.9(6) . . . . ?
C1 C2 C7 C6 179.8(4) . . . . ?
C6 C5 N1 C5 30.8(3) . . . 5_655 ?
C4 C5 N1 C5 -155.3(4) . . . 5_655 ?
O3 C1 O1 Cu1 3.2(5) . . . 10_554 ?
C2 C1 O1 Cu1 -177.0(2) . . . 10_554 ?
O1 C1 O3 Cu1 -7.8(5) . . . . ?
C2 C1 O3 Cu1 172.3(2) . . . . ?
O1 Cu1 O3 C1 -78.8(3) 10_554 . . . ?
O1 Cu1 O3 C1 91.6(3) 8_665 . . . ?
O3 Cu1 O3 C1 6.5(3) 15_444 . . . ?
O2 Cu1 O3 C1 -173.5(3) . . . . ?
Cu1 Cu1 O3 C1 6.5(3) 10_554 . . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.003 -0.013 2215 58 ' '

_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of
diffuse solvent which could not be sensibly modelled
in terms of atomic sites. Their contribution to the
diffraction pattern was removed and modified F(obs)**2
written to a new HKL file. The number of electrons thus located,
842 per unit cell, is included in the formula, formula weight,
calculated density, and F(000). This residual electron density
was assigned to three half molecules of the water solvent,
[58/4 = 15e per two ligand; three half molecules
of the water would give 15e].
;

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.062

# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 697.55
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 28.00 336.31
H 1.01 19.00 19.15
N 14.01 2.00 28.01
O 16.00 10.00 159.99
Cu 63.55 2.00 127.09
Calculated formula weight 670.56

RESPONSE: The contribution of any disordered solvent removed by
the SQUEEZE process has now been included in the overall
formula, formula weight, density, F(000), etc.,
;
# end Validation Reply Form
# Attachment '- 3-new.cif'

data_3
_database_code_depnum_ccdc_archive 'CCDC 893083'
#TrackingRef '- 3-new.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H13 Cu1 N1 O6'
_chemical_formula_sum            'C14 H13 Cu N O6'
_chemical_formula_weight         354.79

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

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.924(3)
_cell_length_b                   17.924(3)
_cell_length_c                   17.225(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5534(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4056
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      25.23

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2896
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_T_max  0.7391
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19657
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2439
_reflns_number_gt                1802
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_reduction        'SMART (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;

TITL 3 in I4(1)/a
CELL 0.71073 17.9235 17.9235 17.2254 90.000 90.000 90.000
ZERR 16.00 0.0030 0.0030 0.0057 0.000 0.000 0.000
LATT 2
SYMM 0.5-X, -Y, 0.5+Z
SYMM 0.75-Y, 0.25+X, 0.25+Z
SYMM 0.75+Y, 0.75-X, 0.75+Z
SFAC C H N O Cu
UNIT 224 208 16 96 16
OMIT 0.00 50.00
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 10
SIZE 0.2 0.24 0.28
dfix 0.90 N1 H1N
delu 0.01 O
SIMU 0.01 O
DFIX 2.12 0.01 H3C H1WA_$2
DFIX 2.20 0.01 H3C H3_$1
eqiv_$2 -x,1.5-y,z
eqiv_$1 -0.25+y,0.75-x,-0.25+z
TEMP 23.000

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+28.2833P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2439
_refine_ls_number_parameters     211
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1745
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.007
_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 0.1006(2) 0.4233(2) 0.5288(2) 0.0413(10) Uani 1 1 d U . .
O3 O 0.0174(3) 0.6331(3) 0.3525(3) 0.0612(13) Uani 1 1 d U . .
H3A H -0.0231 0.6569 0.3457 0.092 Uiso 1 1 d R . .
H3C H 0.0291 0.6106 0.3109 0.092 Uiso 1 1 d RD . .
C10 C 0.5282(4) 0.3497(4) 0.6242(4) 0.0516(16) Uani 1 1 d U . .
H10 H 0.5157 0.3439 0.6762 0.07(2) Uiso 1 1 calc R . .
Cu1 Cu 0.00277(4) 0.55006(4) 0.44543(4) 0.0311(3) Uani 1 1 d U . .
O5 O 0.1045(2) 0.5128(2) 0.4384(2) 0.0412(10) Uani 1 1 d U . .
C2 C 0.2143(3) 0.4462(3) 0.4634(3) 0.0296(11) Uani 1 1 d U . .
C5 C 0.3685(3) 0.4284(3) 0.4492(3) 0.0336(12) Uani 1 1 d U . .
N1 N 0.4455(3) 0.4218(3) 0.4427(3) 0.0416(12) Uani 1 1 d DU . .
C7 C 0.2561(3) 0.4939(3) 0.4173(3) 0.0359(12) Uani 1 1 d U . .
H7 H 0.2323 0.5324 0.3909 0.06(2) Uiso 1 1 calc R . .
C9 C 0.4779(4) 0.3818(4) 0.5745(4) 0.0520(16) Uani 1 1 d U . .
H9 H 0.4321 0.3984 0.5932 0.06(2) Uiso 1 1 calc R . .
C3 C 0.2513(3) 0.3879(3) 0.4980(3) 0.0364(13) Uani 1 1 d U . .
H3 H 0.2237 0.3544 0.5277 0.041(17) Uiso 1 1 calc R . .
C6 C 0.3318(3) 0.4852(3) 0.4098(3) 0.0363(13) Uani 1 1 d U . .
H6 H 0.3587 0.5176 0.3782 0.038(16) Uiso 1 1 calc R . .
C8 C 0.4951(3) 0.3895(4) 0.4956(4) 0.0401(13) Uani 1 1 d U . .
C1 C 0.1345(3) 0.4614(3) 0.4776(3) 0.0344(12) Uani 1 1 d U . .
C13 C 0.5638(3) 0.3659(4) 0.4711(4) 0.0453(15) Uani 1 1 d U . .
H13 H 0.5763 0.3710 0.4190 0.052(19) Uiso 1 1 calc R . .
C4 C 0.3255(3) 0.3764(4) 0.4913(3) 0.0380(13) Uani 1 1 d U . .
H4 H 0.3478 0.3350 0.5140 0.06(2) Uiso 1 1 calc R . .
C11 C 0.5976(3) 0.3257(3) 0.5982(4) 0.0397(13) Uani 1 1 d U . .
C12 C 0.6145(4) 0.3350(4) 0.5208(4) 0.0454(14) Uani 1 1 d U . .
H12 H 0.6608 0.3200 0.5021 0.07(2) Uiso 1 1 calc R . .
H1N H 0.470(4) 0.447(4) 0.406(4) 0.08(3) Uiso 1 1 d D . .
O1W O 0.0857(8) 0.9363(8) 0.2659(10) 0.270(8) Uani 1 1 d . . .
H1WA H 0.0579 0.9657 0.2917 0.406 Uiso 1 1 d R . .
H1WB H 0.1311 0.9443 0.2775 0.406 Uiso 1 1 d R . .
C14 C 0.6530(4) 0.2946(3) 0.6540(4) 0.0408(13) Uani 1 1 d U . .
O1 O 0.7185(2) 0.2827(2) 0.6293(3) 0.0446(11) Uani 1 1 d U . .
O4 O 0.6313(2) 0.2851(3) 0.7231(3) 0.0493(12) Uani 1 1 d U . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.028(2) 0.053(3) 0.043(2) 0.0072(19) 0.0048(17) 0.0081(19)
O3 0.074(4) 0.051(3) 0.059(3) 0.007(2) 0.007(3) -0.007(3)
C10 0.044(3) 0.074(4) 0.037(3) 0.011(3) -0.008(3) 0.005(3)
Cu1 0.0276(4) 0.0309(4) 0.0347(4) -0.0053(3) 0.0001(3) 0.0012(3)
O5 0.029(2) 0.049(3) 0.046(2) 0.0068(19) 0.0031(18) 0.0073(19)
C2 0.028(2) 0.035(3) 0.026(2) -0.005(2) 0.000(2) 0.004(2)
C5 0.028(2) 0.042(3) 0.031(3) 0.003(2) -0.002(2) 0.005(2)
N1 0.026(2) 0.058(3) 0.041(3) 0.015(2) -0.001(2) 0.006(2)
C7 0.034(3) 0.035(3) 0.038(3) 0.003(2) -0.005(2) 0.006(2)
C9 0.038(3) 0.078(4) 0.041(3) 0.009(3) -0.004(3) 0.015(3)
C3 0.033(3) 0.042(3) 0.034(3) 0.008(2) 0.002(2) 0.000(2)
C6 0.032(3) 0.039(3) 0.037(3) 0.008(2) 0.001(2) 0.001(2)
C8 0.032(3) 0.050(3) 0.038(3) 0.003(3) -0.006(2) 0.005(3)
C1 0.030(3) 0.041(3) 0.032(3) -0.004(2) -0.002(2) 0.003(2)
C13 0.033(3) 0.063(4) 0.039(3) 0.003(3) 0.001(2) 0.007(3)
C4 0.034(3) 0.042(3) 0.038(3) 0.011(2) -0.002(2) 0.008(3)
C11 0.038(3) 0.037(3) 0.044(3) 0.001(2) -0.011(2) -0.001(2)
C12 0.033(3) 0.056(4) 0.047(3) -0.003(3) -0.006(3) 0.010(3)
O1W 0.236(17) 0.32(2) 0.260(18) -0.023(16) 0.046(15) -0.047(14)
C14 0.044(3) 0.032(3) 0.047(3) 0.005(2) -0.015(3) -0.005(3)
O1 0.041(2) 0.046(2) 0.047(2) 0.002(2) -0.0157(19) 0.011(2)
O4 0.038(2) 0.058(3) 0.052(3) 0.017(2) -0.018(2) -0.004(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C1 1.269(7) . ?
O2 Cu1 1.963(4) 9_566 ?
O3 Cu1 2.202(5) . ?
O3 H3A 0.8499 . ?
O3 H3C 0.8499 . ?
C10 C9 1.370(9) . ?
C10 C11 1.390(9) . ?
C10 H10 0.9300 . ?
Cu1 O5 1.945(4) . ?
Cu1 O4 1.953(4) 15_566 ?
Cu1 O1 1.959(4) 7_444 ?
Cu1 O2 1.963(4) 9_566 ?
Cu1 Cu1 2.6008(15) 9_566 ?
O5 C1 1.264(7) . ?
C2 C3 1.374(8) . ?
C2 C7 1.386(8) . ?
C2 C1 1.477(8) . ?
C5 C6 1.389(8) . ?
C5 N1 1.390(7) . ?
C5 C4 1.411(8) . ?
N1 C8 1.398(8) . ?
N1 H1N 0.90(2) . ?
C7 C6 1.373(8) . ?
C7 H7 0.9300 . ?
C9 C8 1.401(9) . ?
C9 H9 0.9300 . ?
C3 C4 1.350(8) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C8 C13 1.368(9) . ?
C13 C12 1.365(9) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C11 C12 1.378(9) . ?
C11 C14 1.490(8) . ?
C12 H12 0.9300 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?
C14 O4 1.264(8) . ?
C14 O1 1.267(8) . ?
O1 Cu1 1.959(4) 8_444 ?
O4 Cu1 1.953(4) 12_767 ?

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
C1 O2 Cu1 118.6(4) . 9_566 ?
Cu1 O3 H3A 109.7 . . ?
Cu1 O3 H3C 108.7 . . ?
H3A O3 H3C 109.5 . . ?
C9 C10 C11 121.2(6) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
O5 Cu1 O4 89.03(19) . 15_566 ?
O5 Cu1 O1 90.71(19) . 7_444 ?
O4 Cu1 O1 169.5(2) 15_566 7_444 ?
O5 Cu1 O2 168.97(18) . 9_566 ?
O4 Cu1 O2 87.93(19) 15_566 9_566 ?
O1 Cu1 O2 90.36(19) 7_444 9_566 ?
O5 Cu1 O3 94.29(18) . . ?
O4 Cu1 O3 93.50(19) 15_566 . ?
O1 Cu1 O3 96.94(19) 7_444 . ?
O2 Cu1 O3 96.48(18) 9_566 . ?
O5 Cu1 Cu1 81.03(13) . 9_566 ?
O4 Cu1 Cu1 85.79(15) 15_566 9_566 ?
O1 Cu1 Cu1 83.85(14) 7_444 9_566 ?
O2 Cu1 Cu1 88.17(13) 9_566 9_566 ?
O3 Cu1 Cu1 175.28(14) . 9_566 ?
C1 O5 Cu1 128.1(4) . . ?
C3 C2 C7 117.3(5) . . ?
C3 C2 C1 122.3(5) . . ?
C7 C2 C1 120.3(5) . . ?
C6 C5 N1 119.6(5) . . ?
C6 C5 C4 118.5(5) . . ?
N1 C5 C4 121.8(5) . . ?
C5 N1 C8 127.9(5) . . ?
C5 N1 H1N 120(6) . . ?
C8 N1 H1N 111(6) . . ?
C6 C7 C2 121.2(5) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C10 C9 C8 120.2(6) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C4 C3 C2 123.6(5) . . ?
C4 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
C7 C6 C5 120.3(6) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C13 C8 N1 120.0(6) . . ?
C13 C8 C9 117.8(6) . . ?
N1 C8 C9 122.2(6) . . ?
O5 C1 O2 124.0(5) . . ?
O5 C1 C2 117.3(5) . . ?
O2 C1 C2 118.8(5) . . ?
C12 C13 C8 122.1(6) . . ?
C12 C13 H13 118.9 . . ?
C8 C13 H13 118.9 . . ?
C3 C4 C5 118.8(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C12 C11 C10 118.1(6) . . ?
C12 C11 C14 121.6(6) . . ?
C10 C11 C14 120.3(6) . . ?
C13 C12 C11 120.6(6) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
H1WA O1W H1WB 109.5 . . ?
O4 C14 O1 125.3(6) . . ?
O4 C14 C11 117.0(6) . . ?
O1 C14 C11 117.6(6) . . ?
C14 O1 Cu1 123.4(4) . 8_444 ?
C14 O4 Cu1 121.6(4) . 12_767 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.701
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.127