# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110815c
#TrackingRef 'complex 1. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H78 Cl2 Mn N12 O8'
_chemical_formula_weight         1437.36

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3

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

_cell_length_a                   13.4688(12)
_cell_length_b                   13.4688(12)
_cell_length_c                   10.4961(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1649.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2740
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      28.19

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             753
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9556
_exptl_absorpt_correction_T_max  0.9723
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8453
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1953
_reflns_number_gt                1405
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.0220P)²+2.2657P] 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         1953
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Mn1 Mn 0.0000 0.0000 0.5000 0.0150(3) Uani 1 6 d S . .
N1 N 0.08081(19) 0.16547(19) 0.3844(2) 0.0197(6) Uani 1 1 d . . .
N2 N 0.1532(2) 0.3542(2) 0.3599(2) 0.0237(6) Uani 1 1 d . . .
C1 C 0.1548(2) 0.2026(3) 0.2796(3) 0.0246(7) Uani 1 1 d . . .
C2 C 0.2021(3) 0.3217(3) 0.2645(3) 0.0227(7) Uani 1 1 d . . .
C3 C 0.2790(3) 0.3835(3) 0.1702(3) 0.0283(7) Uani 1 1 d . . .
H3 H 0.3098 0.4639 0.1618 0.034 Uiso 1 1 calc R . .
C4 C 0.3094(3) 0.3229(3) 0.0881(3) 0.0338(8) Uani 1 1 d . . .
H4 H 0.3636 0.3625 0.0225 0.041 Uiso 1 1 calc R . .
C5 C 0.2622(3) 0.2059(3) 0.0999(3) 0.0379(9) Uani 1 1 d . . .
H5 H 0.2841 0.1669 0.0407 0.045 Uiso 1 1 calc R . .
C6 C 0.1847(3) 0.1432(3) 0.1942(3) 0.0340(8) Uani 1 1 d . . .
H6 H 0.1530 0.0625 0.2004 0.041 Uiso 1 1 calc R . .
C7 C 0.0836(2) 0.2597(2) 0.4263(3) 0.0230(7) Uani 1 1 d . . .
H7 H 0.0399 0.2601 0.4972 0.028 Uiso 1 1 calc R . .
C8 C 0.1794(3) 0.4725(2) 0.3828(3) 0.0300(8) Uani 1 1 d . . .
H8A H 0.1975 0.5137 0.3004 0.036 Uiso 1 1 calc R . .
H8B H 0.2486 0.5116 0.4372 0.036 Uiso 1 1 calc R . .
C9 C 0.0830(3) 0.4809(2) 0.4461(3) 0.0239(7) Uani 1 1 d . . .
C10 C -0.0070(3) 0.4715(2) 0.3707(3) 0.0258(7) Uani 1 1 d . . .
C11 C 0.0890(3) 0.5064(2) 0.5763(3) 0.0266(7) Uani 1 1 d . . .
C12 C -0.0170(3) 0.4320(3) 0.2336(3) 0.0358(8) Uani 1 1 d . . .
H12A H 0.0515 0.4865 0.1862 0.054 Uiso 1 1 calc R . .
H12B H -0.0850 0.4280 0.1945 0.054 Uiso 1 1 calc R . .
H12C H -0.0241 0.3560 0.2315 0.054 Uiso 1 1 calc R . .
C13 C 0.1780(3) 0.5028(3) 0.6605(3) 0.0397(9) Uani 1 1 d . . .
H13A H 0.2341 0.5808 0.6874 0.060 Uiso 1 1 calc R . .
H13B H 0.2170 0.4695 0.6131 0.060 Uiso 1 1 calc R . .
H13C H 0.1406 0.4557 0.7358 0.060 Uiso 1 1 calc R . .
Cl1 Cl 0.3333 0.6667 0.02539(13) 0.0336(4) Uani 1 3 d S . .
O1 O 0.3333 0.6667 0.1615(3) 0.0315(9) Uani 1 3 d S . .
O2 O 0.3609(3) 0.7778(2) -0.0165(3) 0.0705(9) Uani 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
Mn1 N1 2.280(2) 4_556 ?
Mn1 N1 2.280(2) . ?
Mn1 N1 2.280(2) 2 ?
Mn1 N1 2.280(2) 6_556 ?
Mn1 N1 2.280(2) 5_556 ?
Mn1 N1 2.280(2) 3 ?
N1 C7 1.326(4) . ?
N1 C1 1.398(4) . ?
N2 C7 1.338(4) . ?
N2 C2 1.385(4) . ?
N2 C8 1.470(4) . ?
C1 C6 1.390(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.372(4) . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.512(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.399(4) . ?
C9 C11 1.401(4) . ?
C10 C11 1.395(4) 4_566 ?
C10 C12 1.516(4) . ?
C11 C10 1.395(4) 4_566 ?
C11 C13 1.510(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
Cl1 O2 1.420(3) 2_665 ?
Cl1 O2 1.420(3) 3_565 ?
Cl1 O2 1.420(3) . ?
Cl1 O1 1.429(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
N1 Mn1 N1 180.0 4_556 . ?
N1 Mn1 N1 85.69(8) 4_556 2 ?
N1 Mn1 N1 94.31(8) . 2 ?
N1 Mn1 N1 94.31(8) 4_556 6_556 ?
N1 Mn1 N1 85.69(8) . 6_556 ?
N1 Mn1 N1 85.69(8) 2 6_556 ?
N1 Mn1 N1 94.31(8) 4_556 5_556 ?
N1 Mn1 N1 85.69(8) . 5_556 ?
N1 Mn1 N1 180.00(13) 2 5_556 ?
N1 Mn1 N1 94.31(8) 6_556 5_556 ?
N1 Mn1 N1 85.69(8) 4_556 3 ?
N1 Mn1 N1 94.31(8) . 3 ?
N1 Mn1 N1 94.31(8) 2 3 ?
N1 Mn1 N1 180.0 6_556 3 ?
N1 Mn1 N1 85.69(8) 5_556 3 ?
C7 N1 C1 104.1(2) . . ?
C7 N1 Mn1 122.03(19) . . ?
C1 N1 Mn1 132.46(19) . . ?
C7 N2 C2 107.1(2) . . ?
C7 N2 C8 128.3(2) . . ?
C2 N2 C8 124.5(2) . . ?
C6 C1 N1 131.4(3) . . ?
C6 C1 C2 119.2(3) . . ?
N1 C1 C2 109.4(3) . . ?
C3 C2 N2 131.6(3) . . ?
C3 C2 C1 123.2(3) . . ?
N2 C2 C1 105.2(3) . . ?
C2 C3 C4 116.6(3) . . ?
C2 C3 H3 121.7 . . ?
C4 C3 H3 121.7 . . ?
C5 C4 C3 121.1(3) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 122.7(3) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C1 117.3(3) . . ?
C5 C6 H6 121.3 . . ?
C1 C6 H6 121.3 . . ?
N1 C7 N2 114.1(3) . . ?
N1 C7 H7 122.9 . . ?
N2 C7 H7 122.9 . . ?
N2 C8 C9 113.8(2) . . ?
N2 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N2 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C11 121.0(3) . . ?
C10 C9 C8 118.8(3) . . ?
C11 C9 C8 120.0(3) . . ?
C11 C10 C9 119.8(3) 4_566 . ?
C11 C10 C12 120.8(3) 4_566 . ?
C9 C10 C12 119.4(3) . . ?
C10 C11 C9 119.1(3) 4_566 . ?
C10 C11 C13 120.0(3) 4_566 . ?
C9 C11 C13 120.8(3) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O2 Cl1 O2 110.87(13) 2_665 3_565 ?
O2 Cl1 O2 110.87(13) 2_665 . ?
O2 Cl1 O2 110.87(13) 3_565 . ?
O2 Cl1 O1 108.03(14) 2_665 . ?
O2 Cl1 O1 108.03(14) 3_565 . ?
O2 Cl1 O1 108.03(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Mn1 N1 C7 54.7(4) 4_556 . . . ?
N1 Mn1 N1 C7 101.5(3) 2 . . . ?
N1 Mn1 N1 C7 16.1(2) 6_556 . . . ?
N1 Mn1 N1 C7 -78.5(3) 5_556 . . . ?
N1 Mn1 N1 C7 -163.9(2) 3 . . . ?
N1 Mn1 N1 C1 -141.0(5) 4_556 . . . ?
N1 Mn1 N1 C1 -94.2(2) 2 . . . ?
N1 Mn1 N1 C1 -179.5(3) 6_556 . . . ?
N1 Mn1 N1 C1 85.8(2) 5_556 . . . ?
N1 Mn1 N1 C1 0.5(3) 3 . . . ?
C7 N1 C1 C6 -177.8(3) . . . . ?
Mn1 N1 C1 C6 15.8(5) . . . . ?
C7 N1 C1 C2 1.3(3) . . . . ?
Mn1 N1 C1 C2 -165.11(19) . . . . ?
C7 N2 C2 C3 -179.9(3) . . . . ?
C8 N2 C2 C3 -2.1(5) . . . . ?
C7 N2 C2 C1 0.7(3) . . . . ?
C8 N2 C2 C1 178.6(3) . . . . ?
C6 C1 C2 C3 -1.5(5) . . . . ?
N1 C1 C2 C3 179.3(3) . . . . ?
C6 C1 C2 N2 177.9(3) . . . . ?
N1 C1 C2 N2 -1.3(3) . . . . ?
N2 C2 C3 C4 -179.2(3) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C3 C4 C5 C6 -1.2(6) . . . . ?
C4 C5 C6 C1 -0.3(5) . . . . ?
N1 C1 C6 C5 -179.5(3) . . . . ?
C2 C1 C6 C5 1.5(5) . . . . ?
C1 N1 C7 N2 -0.8(3) . . . . ?
Mn1 N1 C7 N2 167.35(18) . . . . ?
C2 N2 C7 N1 0.1(3) . . . . ?
C8 N2 C7 N1 -177.7(3) . . . . ?
C7 N2 C8 C9 -29.1(4) . . . . ?
C2 N2 C8 C9 153.5(3) . . . . ?
N2 C8 C9 C10 -82.0(3) . . . . ?
N2 C8 C9 C11 102.9(3) . . . . ?
C11 C9 C10 C11 3.4(5) . . . 4_566 ?
C8 C9 C10 C11 -171.7(3) . . . 4_566 ?
C11 C9 C10 C12 -173.8(3) . . . . ?
C8 C9 C10 C12 11.1(4) . . . . ?
C10 C9 C11 C10 -3.4(5) . . . 4_566 ?
C8 C9 C11 C10 171.7(3) . . . 4_566 ?
C10 C9 C11 C13 172.8(3) . . . . ?
C8 C9 C11 C13 -12.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 923228'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110630b
#TrackingRef 'complex 2. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H32 Cu N4 O7 S'
_chemical_formula_weight         608.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.608(2)
_cell_length_b                   13.831(3)
_cell_length_c                   17.334(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.575(9)
_cell_angle_gamma                90.00
_cell_volume                     2628.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2615
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      24.86

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1268
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8532
_exptl_absorpt_correction_T_max  0.8768
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13201
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4632
_reflns_number_gt                3382
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.0591P)²+4.7994P] 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         4632
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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 0.67186(5) 0.39454(3) 0.55991(3) 0.02590(18) Uani 1 1 d . . .
S1 S 0.60693(12) 0.57811(8) 0.43676(7) 0.0307(3) Uani 1 1 d . . .
O1 O 0.6808(3) 0.4896(2) 0.48016(19) 0.0327(7) Uani 1 1 d . . .
O2 O 0.5500(3) 0.6106(2) 0.4892(2) 0.0369(8) Uani 1 1 d . . .
O3 O 0.5108(3) 0.5520(2) 0.3480(2) 0.0391(8) Uani 1 1 d . . .
O4 O 0.6867(4) 0.6502(2) 0.4336(2) 0.0484(9) Uani 1 1 d . . .
O6 O 0.6758(3) 0.5008(2) 0.63595(18) 0.0293(7) Uani 1 1 d . . .
H6A H 0.6408 0.5434 0.5959 0.044 Uiso 1 1 d R . .
H6B H 0.6242 0.4861 0.6521 0.044 Uiso 1 1 d R . .
O7 O 0.9270(4) 0.4623(3) 0.6000(3) 0.0780(14) Uani 1 1 d . . .
H7A H 0.9894 0.4314 0.6070 0.117 Uiso 1 1 d R . .
H7B H 0.8986 0.4896 0.5498 0.117 Uiso 1 1 d R . .
O8 O 0.8971(5) 0.6212(4) 0.4279(4) 0.110(2) Uani 1 1 d . . .
H8A H 0.8400 0.6176 0.4406 0.165 Uiso 1 1 d R . .
H8B H 0.9470 0.5768 0.4583 0.165 Uiso 1 1 d R . .
N1 N 0.6395(3) 0.2898(2) 0.4753(2) 0.0259(8) Uani 1 1 d . . .
N2 N 0.5232(3) 0.1966(2) 0.3604(2) 0.0239(8) Uani 1 1 d . . .
N3 N -0.0977(3) 0.2547(2) 0.2848(2) 0.0222(8) Uani 1 1 d . . .
N4 N -0.2495(3) 0.1901(2) 0.1637(2) 0.0242(8) Uani 1 1 d . . .
C1 C 0.6418(4) 0.1693(3) 0.3883(3) 0.0198(9) Uani 1 1 d . . .
C2 C 0.7151(4) 0.2280(3) 0.4608(3) 0.0219(9) Uani 1 1 d . . .
C3 C 0.8401(4) 0.2188(3) 0.5044(3) 0.0277(10) Uani 1 1 d . . .
H3 H 0.8899 0.2579 0.5525 0.033 Uiso 1 1 calc R . .
C4 C 0.8878(4) 0.1497(3) 0.4742(3) 0.0317(11) Uani 1 1 d . . .
H4 H 0.9720 0.1414 0.5029 0.038 Uiso 1 1 calc R . .
C5 C 0.8148(4) 0.0913(3) 0.4017(3) 0.0302(10) Uani 1 1 d . . .
H5 H 0.8512 0.0450 0.3834 0.036 Uiso 1 1 calc R . .
C6 C 0.6907(4) 0.1005(3) 0.3569(3) 0.0238(9) Uani 1 1 d . . .
H6 H 0.6416 0.0625 0.3078 0.029 Uiso 1 1 calc R . .
C7 C 0.5283(4) 0.2679(3) 0.4141(3) 0.0278(10) Uani 1 1 d . . .
H7 H 0.4595 0.2990 0.4085 0.033 Uiso 1 1 calc R . .
C8 C 0.4111(4) 0.1547(3) 0.2879(3) 0.0267(10) Uani 1 1 d . . .
H8' H 0.4183 0.0849 0.2885 0.032 Uiso 1 1 calc R . .
H8" H 0.3989 0.1782 0.2314 0.032 Uiso 1 1 calc R . .
C9 C 0.3039(4) 0.1823(3) 0.2987(3) 0.0246(9) Uani 1 1 d . . .
C10 C 0.2800(4) 0.1294(3) 0.3577(3) 0.0274(10) Uani 1 1 d . . .
C11 C 0.1859(4) 0.1570(3) 0.3720(3) 0.0274(10) Uani 1 1 d . . .
C12 C 0.1205(4) 0.2407(3) 0.3323(3) 0.0237(9) Uani 1 1 d . . .
C13 C 0.1420(4) 0.2938(3) 0.2730(3) 0.0227(9) Uani 1 1 d . . .
C14 C 0.2336(4) 0.2641(3) 0.2556(3) 0.0244(9) Uani 1 1 d . . .
C15 C 0.3592(5) 0.0440(4) 0.4075(3) 0.0409(13) Uani 1 1 d . . .
H15A H 0.3775 0.0464 0.4682 0.061 Uiso 1 1 calc R . .
H15B H 0.4337 0.0464 0.4052 0.061 Uiso 1 1 calc R . .
H15C H 0.3167 -0.0149 0.3807 0.061 Uiso 1 1 calc R . .
C16 C 0.1546(5) 0.0961(4) 0.4305(3) 0.0450(13) Uani 1 1 d . . .
H16A H 0.1795 0.0305 0.4306 0.068 Uiso 1 1 calc R . .
H16B H 0.0682 0.0981 0.4082 0.068 Uiso 1 1 calc R . .
H16C H 0.1963 0.1211 0.4899 0.068 Uiso 1 1 calc R . .
C17 C 0.0678(4) 0.3832(3) 0.2285(3) 0.0284(10) Uani 1 1 d . . .
H17A H -0.0021 0.3854 0.2368 0.043 Uiso 1 1 calc R . .
H17B H 0.0414 0.3811 0.1663 0.043 Uiso 1 1 calc R . .
H17C H 0.1170 0.4397 0.2543 0.043 Uiso 1 1 calc R . .
C18 C 0.2594(5) 0.3226(3) 0.1936(3) 0.0384(12) Uani 1 1 d . . .
H18A H 0.1848 0.3502 0.1480 0.058 Uiso 1 1 calc R . .
H18B H 0.2940 0.2815 0.1672 0.058 Uiso 1 1 calc R . .
H18C H 0.3158 0.3734 0.2261 0.058 Uiso 1 1 calc R . .
C19 C 0.0262(4) 0.2769(3) 0.3548(3) 0.0274(10) Uani 1 1 d . . .
H19A H 0.0402 0.2475 0.4099 0.033 Uiso 1 1 calc R . .
H19B H 0.0347 0.3464 0.3636 0.033 Uiso 1 1 calc R . .
C20 C -0.2027(4) 0.3010(3) 0.2709(3) 0.0219(9) Uani 1 1 d . . .
C21 C -0.2978(4) 0.2601(3) 0.1943(3) 0.0232(9) Uani 1 1 d . . .
C22 C -0.4157(4) 0.2927(3) 0.1623(3) 0.0312(10) Uani 1 1 d . . .
H22 H -0.4800 0.2674 0.1106 0.037 Uiso 1 1 calc R . .
C23 C -0.4346(4) 0.3635(3) 0.2095(3) 0.0328(11) Uani 1 1 d . . .
H23 H -0.5132 0.3866 0.1892 0.039 Uiso 1 1 calc R . .
C24 C -0.3392(5) 0.4019(3) 0.2873(3) 0.0335(11) Uani 1 1 d . . .
H24 H -0.3559 0.4489 0.3181 0.040 Uiso 1 1 calc R . .
C25 C -0.2217(4) 0.3719(3) 0.3190(3) 0.0275(10) Uani 1 1 d . . .
H25 H -0.1576 0.3979 0.3703 0.033 Uiso 1 1 calc R . .
C26 C -0.1314(4) 0.1886(3) 0.2196(3) 0.0236(9) Uani 1 1 d . . .
H26 H -0.0774 0.1467 0.2148 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 O1 1.951(3) . ?
Cu1 N1 1.956(3) . ?
Cu1 N4 1.957(3) 4_666 ?
Cu1 O6 1.958(3) . ?
S1 O4 1.436(4) . ?
S1 O3 1.458(3) . ?
S1 O2 1.479(3) . ?
S1 O1 1.497(3) . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8500 . ?
O7 H7A 0.8496 . ?
O7 H7B 0.8500 . ?
O8 H8A 0.8504 . ?
O8 H8B 0.8507 . ?
N1 C7 1.309(6) . ?
N1 C2 1.393(5) . ?
N2 C7 1.335(5) . ?
N2 C1 1.378(5) . ?
N2 C8 1.470(5) . ?
N3 C26 1.349(5) . ?
N3 C20 1.380(5) . ?
N3 C19 1.461(5) . ?
N4 C26 1.316(5) . ?
N4 C21 1.380(5) . ?
N4 Cu1 1.957(3) 4_465 ?
C1 C6 1.383(5) . ?
C1 C2 1.395(6) . ?
C2 C3 1.377(6) . ?
C3 C4 1.363(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.392(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.502(6) . ?
C8 H8' 0.9700 . ?
C8 H8" 0.9700 . ?
C9 C14 1.404(6) . ?
C9 C10 1.407(6) . ?
C10 C11 1.380(6) . ?
C10 C15 1.512(6) . ?
C11 C12 1.390(6) . ?
C11 C16 1.512(6) . ?
C12 C13 1.395(6) . ?
C12 C19 1.508(6) . ?
C13 C14 1.392(6) . ?
C13 C17 1.511(6) . ?
C14 C18 1.503(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C25 1.382(6) . ?
C20 C21 1.397(6) . ?
C21 C22 1.381(6) . ?
C22 C23 1.371(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.366(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 H26 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 N1 91.81(13) . . ?
O1 Cu1 N4 150.97(15) . 4_666 ?
N1 Cu1 N4 93.99(14) . 4_666 ?
O1 Cu1 O6 88.86(12) . . ?
N1 Cu1 O6 170.80(15) . . ?
N4 Cu1 O6 89.84(13) 4_666 . ?
O4 S1 O3 111.4(2) . . ?
O4 S1 O2 111.9(2) . . ?
O3 S1 O2 108.7(2) . . ?
O4 S1 O1 108.3(2) . . ?
O3 S1 O1 108.36(19) . . ?
O2 S1 O1 108.03(17) . . ?
S1 O1 Cu1 131.92(19) . . ?
Cu1 O6 H6A 98.1 . . ?
Cu1 O6 H6B 105.9 . . ?
H6A O6 H6B 105.1 . . ?
H7A O7 H7B 105.1 . . ?
H8A O8 H8B 105.1 . . ?
C7 N1 C2 105.4(3) . . ?
C7 N1 Cu1 121.5(3) . . ?
C2 N1 Cu1 133.0(3) . . ?
C7 N2 C1 106.7(3) . . ?
C7 N2 C8 125.6(4) . . ?
C1 N2 C8 127.7(3) . . ?
C26 N3 C20 106.8(3) . . ?
C26 N3 C19 127.1(3) . . ?
C20 N3 C19 126.0(3) . . ?
C26 N4 C21 106.3(3) . . ?
C26 N4 Cu1 122.9(3) . 4_465 ?
C21 N4 Cu1 130.8(3) . 4_465 ?
N2 C1 C6 131.9(4) . . ?
N2 C1 C2 106.2(3) . . ?
C6 C1 C2 121.9(4) . . ?
C3 C2 N1 131.1(4) . . ?
C3 C2 C1 120.7(4) . . ?
N1 C2 C1 108.1(4) . . ?
C4 C3 C2 117.1(4) . . ?
C4 C3 H3 121.4 . . ?
C2 C3 H3 121.4 . . ?
C3 C4 C5 122.2(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C6 C5 C4 121.4(4) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 116.6(4) . . ?
C5 C6 H6 121.7 . . ?
C1 C6 H6 121.7 . . ?
N1 C7 N2 113.6(4) . . ?
N1 C7 H7 123.2 . . ?
N2 C7 H7 123.2 . . ?
N2 C8 C9 109.7(3) . . ?
N2 C8 H8' 109.7 . . ?
C9 C8 H8' 109.7 . . ?
N2 C8 H8" 109.7 . . ?
C9 C8 H8" 109.7 . . ?
H8' C8 H8" 108.2 . . ?
C14 C9 C10 120.0(4) . . ?
C14 C9 C8 120.6(4) . . ?
C10 C9 C8 119.2(4) . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 C15 119.8(4) . . ?
C9 C10 C15 120.2(4) . . ?
C10 C11 C12 119.6(4) . . ?
C10 C11 C16 119.9(4) . . ?
C12 C11 C16 120.5(4) . . ?
C11 C12 C13 121.3(4) . . ?
C11 C12 C19 120.0(4) . . ?
C13 C12 C19 118.7(4) . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 C17 120.1(4) . . ?
C12 C13 C17 120.7(4) . . ?
C13 C14 C9 119.8(4) . . ?
C13 C14 C18 119.5(4) . . ?
C9 C14 C18 120.7(4) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C12 111.8(3) . . ?
N3 C19 H19A 109.3 . . ?
C12 C19 H19A 109.3 . . ?
N3 C19 H19B 109.3 . . ?
C12 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
N3 C20 C25 131.4(4) . . ?
N3 C20 C21 106.1(3) . . ?
C25 C20 C21 122.5(4) . . ?
N4 C21 C22 131.8(4) . . ?
N4 C21 C20 108.4(4) . . ?
C22 C21 C20 119.9(4) . . ?
C23 C22 C21 117.6(4) . . ?
C23 C22 H22 121.2 . . ?
C21 C22 H22 121.2 . . ?
C22 C23 C24 121.9(4) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C25 C24 C23 121.3(4) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C20 116.7(4) . . ?
C24 C25 H25 121.6 . . ?
C20 C25 H25 121.6 . . ?
N4 C26 N3 112.4(4) . . ?
N4 C26 H26 123.8 . . ?
N3 C26 H26 123.8 . . ?

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
O4 S1 O1 Cu1 144.0(3) . . . . ?
O3 S1 O1 Cu1 -95.0(3) . . . . ?
O2 S1 O1 Cu1 22.6(3) . . . . ?
N1 Cu1 O1 S1 119.0(3) . . . . ?
N4 Cu1 O1 S1 -139.5(3) 4_666 . . . ?
O6 Cu1 O1 S1 -51.9(3) . . . . ?
O1 Cu1 N1 C7 -88.6(3) . . . . ?
N4 Cu1 N1 C7 119.9(3) 4_666 . . . ?
O6 Cu1 N1 C7 5.5(10) . . . . ?
O1 Cu1 N1 C2 88.4(4) . . . . ?
N4 Cu1 N1 C2 -63.1(4) 4_666 . . . ?
O6 Cu1 N1 C2 -177.5(6) . . . . ?
C7 N2 C1 C6 -179.1(4) . . . . ?
C8 N2 C1 C6 2.7(7) . . . . ?
C7 N2 C1 C2 0.3(4) . . . . ?
C8 N2 C1 C2 -177.9(4) . . . . ?
C7 N1 C2 C3 179.8(4) . . . . ?
Cu1 N1 C2 C3 2.5(7) . . . . ?
C7 N1 C2 C1 -0.2(4) . . . . ?
Cu1 N1 C2 C1 -177.5(3) . . . . ?
N2 C1 C2 C3 180.0(4) . . . . ?
C6 C1 C2 C3 -0.5(6) . . . . ?
N2 C1 C2 N1 -0.1(4) . . . . ?
C6 C1 C2 N1 179.4(3) . . . . ?
N1 C2 C3 C4 179.5(4) . . . . ?
C1 C2 C3 C4 -0.6(6) . . . . ?
C2 C3 C4 C5 0.8(7) . . . . ?
C3 C4 C5 C6 0.2(7) . . . . ?
C4 C5 C6 C1 -1.2(6) . . . . ?
N2 C1 C6 C5 -179.3(4) . . . . ?
C2 C1 C6 C5 1.4(6) . . . . ?
C2 N1 C7 N2 0.4(5) . . . . ?
Cu1 N1 C7 N2 178.1(3) . . . . ?
C1 N2 C7 N1 -0.4(5) . . . . ?
C8 N2 C7 N1 177.8(4) . . . . ?
C7 N2 C8 C9 -16.3(6) . . . . ?
C1 N2 C8 C9 161.6(4) . . . . ?
N2 C8 C9 C14 93.8(5) . . . . ?
N2 C8 C9 C10 -81.5(5) . . . . ?
C14 C9 C10 C11 1.2(6) . . . . ?
C8 C9 C10 C11 176.5(4) . . . . ?
C14 C9 C10 C15 -177.2(4) . . . . ?
C8 C9 C10 C15 -1.8(6) . . . . ?
C9 C10 C11 C12 -4.2(7) . . . . ?
C15 C10 C11 C12 174.1(4) . . . . ?
C9 C10 C11 C16 175.8(4) . . . . ?
C15 C10 C11 C16 -5.9(7) . . . . ?
C10 C11 C12 C13 4.8(6) . . . . ?
C16 C11 C12 C13 -175.2(4) . . . . ?
C10 C11 C12 C19 -173.8(4) . . . . ?
C16 C11 C12 C19 6.2(6) . . . . ?
C11 C12 C13 C14 -2.1(6) . . . . ?
C19 C12 C13 C14 176.4(4) . . . . ?
C11 C12 C13 C17 178.3(4) . . . . ?
C19 C12 C13 C17 -3.1(6) . . . . ?
C12 C13 C14 C9 -1.0(6) . . . . ?
C17 C13 C14 C9 178.6(4) . . . . ?
C12 C13 C14 C18 -178.4(4) . . . . ?
C17 C13 C14 C18 1.2(6) . . . . ?
C10 C9 C14 C13 1.4(6) . . . . ?
C8 C9 C14 C13 -173.8(4) . . . . ?
C10 C9 C14 C18 178.8(4) . . . . ?
C8 C9 C14 C18 3.5(6) . . . . ?
C26 N3 C19 C12 18.0(6) . . . . ?
C20 N3 C19 C12 -159.0(4) . . . . ?
C11 C12 C19 N3 -102.9(5) . . . . ?
C13 C12 C19 N3 78.6(5) . . . . ?
C26 N3 C20 C25 177.5(4) . . . . ?
C19 N3 C20 C25 -5.0(7) . . . . ?
C26 N3 C20 C21 -1.0(4) . . . . ?
C19 N3 C20 C21 176.5(4) . . . . ?
C26 N4 C21 C22 -180.0(4) . . . . ?
Cu1 N4 C21 C22 0.2(7) 4_465 . . . ?
C26 N4 C21 C20 0.5(4) . . . . ?
Cu1 N4 C21 C20 -179.3(3) 4_465 . . . ?
N3 C20 C21 N4 0.4(4) . . . . ?
C25 C20 C21 N4 -178.3(4) . . . . ?
N3 C20 C21 C22 -179.2(4) . . . . ?
C25 C20 C21 C22 2.1(6) . . . . ?
N4 C21 C22 C23 179.0(4) . . . . ?
C20 C21 C22 C23 -1.5(6) . . . . ?
C21 C22 C23 C24 -0.1(6) . . . . ?
C22 C23 C24 C25 1.4(7) . . . . ?
C23 C24 C25 C20 -0.9(6) . . . . ?
N3 C20 C25 C24 -179.2(4) . . . . ?
C21 C20 C25 C24 -0.8(6) . . . . ?
C21 N4 C26 N3 -1.2(4) . . . . ?
Cu1 N4 C26 N3 178.6(2) 4_465 . . . ?
C20 N3 C26 N4 1.4(4) . . . . ?
C19 N3 C26 N4 -176.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 923229'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110714a
#TrackingRef 'complex 3. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H44 Co N4 O8'
_chemical_formula_weight         695.66

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'
Co Co 0.3494 0.9721 '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

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

_cell_length_a                   9.144(4)
_cell_length_b                   9.914(4)
_cell_length_c                   10.981(5)
_cell_angle_alpha                113.235(6)
_cell_angle_beta                 104.079(7)
_cell_angle_gamma                92.301(7)
_cell_volume                     876.8(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1858
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.05

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             367
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9229
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4469
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3069
_reflns_number_gt                2535
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.1033P)²+0.8721P] 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         3069
_refine_ls_number_parameters     224
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1833
_refine_ls_wR_factor_gt          0.1699
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
Co1 Co 0.5000 0.5000 0.0000 0.0242(3) Uani 1 2 d S . .
O1 O 0.7271(3) 0.5025(3) -0.0004(3) 0.0319(7) Uani 1 1 d . . .
O2 O 0.7166(3) 0.3071(3) -0.1947(3) 0.0423(8) Uani 1 1 d . . .
O3 O 0.5695(3) 0.6918(3) 0.1934(3) 0.0343(7) Uani 1 1 d . . .
H3' H 0.4832 0.7114 0.2056 0.052 Uiso 1 1 d R . .
N1 N 0.5347(3) 0.3528(3) 0.0933(3) 0.0294(7) Uani 1 1 d . . .
N2 N 0.6616(4) 0.2501(4) 0.2270(4) 0.0358(8) Uani 1 1 d . . .
C1 C 0.5161(5) 0.1683(4) 0.1651(4) 0.0366(10) Uani 1 1 d . . .
C2 C 0.4379(4) 0.2340(4) 0.0826(4) 0.0306(9) Uani 1 1 d . . .
C3 C 0.2865(5) 0.1782(4) 0.0042(4) 0.0364(10) Uani 1 1 d . . .
H3 H 0.2321 0.2220 -0.0524 0.044 Uiso 1 1 calc R . .
C4 C 0.2196(5) 0.0563(5) 0.0128(5) 0.0457(12) Uani 1 1 d . . .
H4 H 0.1164 0.0156 -0.0388 0.055 Uiso 1 1 calc R . .
C5 C 0.2999(6) -0.0092(5) 0.0957(5) 0.0522(13) Uani 1 1 d . . .
H5 H 0.2494 -0.0930 0.0987 0.063 Uiso 1 1 calc R . .
C6 C 0.4489(6) 0.0440(5) 0.1727(5) 0.0472(12) Uani 1 1 d . . .
H6 H 0.5034 -0.0012 0.2280 0.057 Uiso 1 1 calc R . .
C7 C 0.6642(4) 0.3556(4) 0.1792(4) 0.0331(9) Uani 1 1 d . . .
H7 H 0.7522 0.4261 0.2052 0.040 Uiso 1 1 calc R . .
C8 C 0.7870(5) 0.2277(5) 0.3261(5) 0.0444(11) Uani 1 1 d . . .
H8A H 0.8415 0.1499 0.2755 0.053 Uiso 1 1 calc R . .
H8B H 0.7452 0.1934 0.3858 0.053 Uiso 1 1 calc R . .
C9 C 0.8978(5) 0.3704(5) 0.4149(4) 0.0382(10) Uani 1 1 d . . .
C10 C 0.8625(5) 0.4757(5) 0.5294(4) 0.0389(10) Uani 1 1 d . . .
C11 C 1.0326(5) 0.3963(5) 0.3836(4) 0.0385(10) Uani 1 1 d . . .
C12 C 0.7118(5) 0.4535(6) 0.5575(5) 0.0479(11) Uani 1 1 d . . .
H12A H 0.7255 0.4136 0.6275 0.072 Uiso 1 1 calc R . .
H12B H 0.6376 0.3836 0.4721 0.072 Uiso 1 1 calc R . .
H12C H 0.6743 0.5490 0.5912 0.072 Uiso 1 1 calc R . .
C13 C 1.0660(6) 0.2893(6) 0.2536(5) 0.0520(12) Uani 1 1 d . . .
H13A H 1.1229 0.2154 0.2738 0.078 Uiso 1 1 calc R . .
H13B H 1.1269 0.3444 0.2212 0.078 Uiso 1 1 calc R . .
H13C H 0.9698 0.2391 0.1819 0.078 Uiso 1 1 calc R . .
C14 C 0.7875(4) 0.4175(4) -0.0856(4) 0.0298(9) Uani 1 1 d . . .
C15 C 0.9568(4) 0.4475(4) -0.0559(5) 0.0329(9) Uani 1 1 d . . .
H15 H 1.0031 0.3864 -0.1224 0.039 Uiso 1 1 calc R . .
C16 C 0.6818(8) 0.7258(8) 0.3199(7) 0.098(3) Uani 1 1 d . . .
H16A H 0.6597 0.6558 0.3582 0.146 Uiso 1 1 calc R . .
H16B H 0.6810 0.8272 0.3852 0.146 Uiso 1 1 calc R . .
H16C H 0.7825 0.7178 0.3036 0.146 Uiso 1 1 calc R . .
O4 O 0.1533(7) 0.8608(6) 0.3969(6) 0.0787(18) Uani 0.807(7) 1 d PD A 1
C17 C 0.0764(10) 0.9648(9) 0.3428(10) 0.083(3) Uani 0.807(7) 1 d PD A 1
C17' C 0.129(3) 0.914(5) 0.361(5) 0.083(3) Uani 0.193(7) 1 d PD A 2
O4' O 0.289(3) 0.927(3) 0.447(2) 0.0787(18) Uani 0.193(7) 1 d PD A 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
Co1 O1 2.077(3) 2_665 ?
Co1 O1 2.077(3) . ?
Co1 N1 2.083(3) . ?
Co1 N1 2.083(3) 2_665 ?
Co1 O3 2.142(3) . ?
Co1 O3 2.142(3) 2_665 ?
O1 C14 1.248(5) . ?
O2 C14 1.259(5) . ?
O3 C16 1.417(6) . ?
O3 H3' 0.8500 . ?
N1 C7 1.314(5) . ?
N1 C2 1.393(5) . ?
N2 C7 1.344(5) . ?
N2 C1 1.389(5) . ?
N2 C8 1.467(5) . ?
C1 C2 1.395(6) . ?
C1 C6 1.396(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.379(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.514(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.397(7) . ?
C9 C10 1.402(6) . ?
C10 C11 1.394(6) 2_766 ?
C10 C12 1.510(7) . ?
C11 C10 1.394(6) 2_766 ?
C11 C13 1.517(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.494(5) . ?
C15 C15 1.291(8) 2_765 ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O4 C17 1.4990(11) . ?
C17' O4' 1.5002(12) . ?

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 Co1 O1 180.0 2_665 . ?
O1 Co1 N1 92.77(11) 2_665 . ?
O1 Co1 N1 87.23(11) . . ?
O1 Co1 N1 87.23(11) 2_665 2_665 ?
O1 Co1 N1 92.77(11) . 2_665 ?
N1 Co1 N1 180.0 . 2_665 ?
O1 Co1 O3 91.41(10) 2_665 . ?
O1 Co1 O3 88.59(10) . . ?
N1 Co1 O3 93.26(12) . . ?
N1 Co1 O3 86.74(12) 2_665 . ?
O1 Co1 O3 88.59(10) 2_665 2_665 ?
O1 Co1 O3 91.41(10) . 2_665 ?
N1 Co1 O3 86.74(12) . 2_665 ?
N1 Co1 O3 93.26(12) 2_665 2_665 ?
O3 Co1 O3 180.0 . 2_665 ?
C14 O1 Co1 130.4(2) . . ?
C16 O3 Co1 133.4(3) . . ?
C16 O3 H3' 111.8 . . ?
Co1 O3 H3' 100.5 . . ?
C7 N1 C2 104.5(3) . . ?
C7 N1 Co1 124.1(3) . . ?
C2 N1 Co1 131.4(3) . . ?
C7 N2 C1 106.2(3) . . ?
C7 N2 C8 126.7(4) . . ?
C1 N2 C8 127.1(4) . . ?
N2 C1 C2 105.7(3) . . ?
N2 C1 C6 132.0(4) . . ?
C2 C1 C6 122.3(4) . . ?
N1 C2 C1 109.4(3) . . ?
N1 C2 C3 129.8(4) . . ?
C1 C2 C3 120.9(4) . . ?
C4 C3 C2 116.8(4) . . ?
C4 C3 H3 121.6 . . ?
C2 C3 H3 121.6 . . ?
C3 C4 C5 121.7(4) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 122.1(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C1 116.2(5) . . ?
C5 C6 H6 121.9 . . ?
C1 C6 H6 121.9 . . ?
N1 C7 N2 114.2(3) . . ?
N1 C7 H7 122.9 . . ?
N2 C7 H7 122.9 . . ?
N2 C8 C9 110.9(3) . . ?
N2 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C11 C9 C10 120.7(4) . . ?
C11 C9 C8 120.7(4) . . ?
C10 C9 C8 118.6(4) . . ?
C11 C10 C9 119.1(4) 2_766 . ?
C11 C10 C12 120.0(4) 2_766 . ?
C9 C10 C12 120.9(4) . . ?
C10 C11 C9 120.1(4) 2_766 . ?
C10 C11 C13 118.7(4) 2_766 . ?
C9 C11 C13 121.2(4) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 O2 124.9(3) . . ?
O1 C14 C15 117.9(3) . . ?
O2 C14 C15 117.2(4) . . ?
C15 C15 C14 123.2(5) 2_765 . ?
C15 C15 H15 118.4 2_765 . ?
C14 C15 H15 118.4 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

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
O1 Co1 O1 C14 1.3(6) 2_665 . . . ?
N1 Co1 O1 C14 85.8(3) . . . . ?
N1 Co1 O1 C14 -94.2(3) 2_665 . . . ?
O3 Co1 O1 C14 179.1(3) . . . . ?
O3 Co1 O1 C14 -0.9(3) 2_665 . . . ?
O1 Co1 O3 C16 129.0(6) 2_665 . . . ?
O1 Co1 O3 C16 -51.0(6) . . . . ?
N1 Co1 O3 C16 36.1(6) . . . . ?
N1 Co1 O3 C16 -143.9(6) 2_665 . . . ?
O3 Co1 O3 C16 148(28) 2_665 . . . ?
O1 Co1 N1 C7 -147.1(3) 2_665 . . . ?
O1 Co1 N1 C7 32.9(3) . . . . ?
N1 Co1 N1 C7 -116(10) 2_665 . . . ?
O3 Co1 N1 C7 -55.5(3) . . . . ?
O3 Co1 N1 C7 124.5(3) 2_665 . . . ?
O1 Co1 N1 C2 33.7(4) 2_665 . . . ?
O1 Co1 N1 C2 -146.3(4) . . . . ?
N1 Co1 N1 C2 65(10) 2_665 . . . ?
O3 Co1 N1 C2 125.3(3) . . . . ?
O3 Co1 N1 C2 -54.7(3) 2_665 . . . ?
C7 N2 C1 C2 -0.8(5) . . . . ?
C8 N2 C1 C2 178.5(4) . . . . ?
C7 N2 C1 C6 178.1(5) . . . . ?
C8 N2 C1 C6 -2.6(8) . . . . ?
C7 N1 C2 C1 -0.1(4) . . . . ?
Co1 N1 C2 C1 179.2(3) . . . . ?
C7 N1 C2 C3 -179.1(4) . . . . ?
Co1 N1 C2 C3 0.2(7) . . . . ?
N2 C1 C2 N1 0.5(5) . . . . ?
C6 C1 C2 N1 -178.5(4) . . . . ?
N2 C1 C2 C3 179.7(4) . . . . ?
C6 C1 C2 C3 0.7(7) . . . . ?
N1 C2 C3 C4 179.0(4) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C3 C4 C5 C6 0.0(7) . . . . ?
C4 C5 C6 C1 0.7(7) . . . . ?
N2 C1 C6 C5 -179.8(5) . . . . ?
C2 C1 C6 C5 -1.0(7) . . . . ?
C2 N1 C7 N2 -0.4(5) . . . . ?
Co1 N1 C7 N2 -179.8(3) . . . . ?
C1 N2 C7 N1 0.8(5) . . . . ?
C8 N2 C7 N1 -178.5(4) . . . . ?
C7 N2 C8 C9 23.9(6) . . . . ?
C1 N2 C8 C9 -155.2(4) . . . . ?
N2 C8 C9 C11 -98.3(5) . . . . ?
N2 C8 C9 C10 81.9(5) . . . . ?
C11 C9 C10 C11 -3.3(7) . . . 2_766 ?
C8 C9 C10 C11 176.5(4) . . . 2_766 ?
C11 C9 C10 C12 175.4(4) . . . . ?
C8 C9 C10 C12 -4.8(6) . . . . ?
C10 C9 C11 C10 3.4(7) . . . 2_766 ?
C8 C9 C11 C10 -176.4(4) . . . 2_766 ?
C10 C9 C11 C13 -174.9(4) . . . . ?
C8 C9 C11 C13 5.4(6) . . . . ?
Co1 O1 C14 O2 0.2(6) . . . . ?
Co1 O1 C14 C15 -179.2(2) . . . . ?
O1 C14 C15 C15 3.1(7) . . . 2_765 ?
O2 C14 C15 C15 -176.3(5) . . . 2_765 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.094
_database_code_depnum_ccdc_archive 'CCDC 923230'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110629a
#TrackingRef 'complex 4. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14.50 H16.50 Co0.50 N3.50 O3.50'
_chemical_formula_weight         325.28

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'
Co Co 0.3494 0.9721 '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

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                   16.620(3)
_cell_length_b                   9.5294(16)
_cell_length_c                   19.384(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.236(5)
_cell_angle_gamma                90.00
_cell_volume                     2975.7(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3394
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.31

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8996
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7248
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2626
_reflns_number_gt                2172
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.1728P)²+10.6319P] 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         2626
_refine_ls_number_parameters     226
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.2543
_refine_ls_wR_factor_gt          0.2381
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.028
_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
Co1 Co 0.0000 0.61433(9) 0.2500 0.0460(5) Uani 1 2 d S . .
N1 N 0.0857(3) 0.6248(4) 0.1865(2) 0.0415(12) Uani 1 1 d . . .
O2 O 0.0554(3) 0.4361(4) 0.31778(19) 0.0471(10) Uani 1 1 d . . .
C9 C 0.0619(3) 0.8996(4) 0.0150(2) 0.0272(10) Uani 1 1 d . . .
C2 C 0.1790(3) 0.5940(5) 0.1199(2) 0.0284(10) Uani 1 1 d . A .
O1 O 0.0998(3) 0.6426(4) 0.3496(2) 0.0638(14) Uani 1 1 d . . .
N2 N 0.1273(3) 0.7046(4) 0.0927(2) 0.0317(9) Uani 1 1 d . A .
C11 C -0.0173(3) 0.8602(4) -0.0218(2) 0.0290(10) Uani 1 1 d . . .
C1 C 0.1529(3) 0.5459(5) 0.1787(2) 0.0262(10) Uani 1 1 d . . .
C7 C 0.0743(4) 0.7162(5) 0.1346(3) 0.0478(16) Uani 1 1 d . . .
H7 H 0.0318 0.7853 0.1272 0.057 Uiso 1 1 calc R A .
C8 C 0.1305(3) 0.7897(5) 0.0304(3) 0.0360(12) Uani 1 1 d . . .
H8A H 0.1247 0.7279 -0.0116 0.043 Uiso 1 1 calc R A .
H8B H 0.1852 0.8370 0.0390 0.043 Uiso 1 1 calc R . .
C5 C 0.2580(3) 0.3712(7) 0.1954(3) 0.0535(17) Uani 1 1 d . . .
H5 H 0.2862 0.2933 0.2210 0.064 Uiso 1 1 calc R A .
O3 O 0.1465(3) 0.4652(7) 0.4184(3) 0.091(2) Uani 1 1 d . . .
C13 C -0.0384(4) 0.7092(5) -0.0424(3) 0.0463(14) Uani 1 1 d . . .
H13A H -0.0385 0.6954 -0.0926 0.070 Uiso 1 1 calc R . .
H13B H -0.0934 0.6869 -0.0355 0.070 Uiso 1 1 calc R . .
H13C H 0.0031 0.6473 -0.0127 0.070 Uiso 1 1 calc R . .
C6 C 0.1943(3) 0.4333(5) 0.2181(2) 0.0338(12) Uani 1 1 d . . .
H6 H 0.1789 0.4005 0.2594 0.041 Uiso 1 1 calc R . .
C10 C 0.0804(3) 1.0373(5) 0.0386(2) 0.0286(10) Uani 1 1 d . . .
N3 N 0.1022(3) 0.5142(6) 0.3638(2) 0.0559(14) Uani 1 1 d . . .
C4 C 0.2819(3) 0.4205(7) 0.1355(4) 0.0588(19) Uani 1 1 d . . .
H4 H 0.3259 0.3747 0.1211 0.071 Uiso 1 1 calc R . .
C3 C 0.2439(3) 0.5326(6) 0.0972(3) 0.0416(13) Uani 1 1 d . . .
H3A H 0.2609 0.5670 0.0570 0.050 Uiso 1 1 calc R A .
C12 C 0.1657(4) 1.0768(6) 0.0823(3) 0.0502(14) Uani 1 1 d . . .
H12A H 0.1916 0.9953 0.1098 0.075 Uiso 1 1 calc R . .
H12B H 0.1610 1.1533 0.1148 0.075 Uiso 1 1 calc R . .
H12C H 0.2000 1.1075 0.0505 0.075 Uiso 1 1 calc R . .
N4 N 0.0225(4) 1.0566(6) 0.2551(6) 0.032(2) Uani 0.50 1 d PD A -1
C15 C 0.0896(7) 1.1566(11) 0.2517(10) 0.051(4) Uani 0.50 1 d PD A -1
H15A H 0.1351 1.1062 0.2387 0.076 Uiso 0.50 1 calc PR A -1
H15B H 0.1100 1.2013 0.2982 0.076 Uiso 0.50 1 calc PR A -1
H15C H 0.0679 1.2286 0.2158 0.076 Uiso 0.50 1 calc PR A -1
O4 O -0.0262(3) 0.8320(6) 0.2402(4) 0.0263(15) Uani 0.50 1 d PD A -1
C14 C 0.0289(4) 0.9187(6) 0.2415(5) 0.031(2) Uani 0.50 1 d PD A -1
H14 H 0.0794 0.8866 0.2323 0.037 Uiso 0.50 1 calc PR A -1
C16 C -0.0535(7) 1.1179(12) 0.2690(10) 0.057(5) Uani 0.50 1 d PD A -1
H16A H -0.0883 1.0428 0.2807 0.086 Uiso 0.50 1 calc PR A -1
H16B H -0.0843 1.1680 0.2266 0.086 Uiso 0.50 1 calc PR A -1
H16C H -0.0384 1.1835 0.3091 0.086 Uiso 0.50 1 calc PR A -1


_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
Co1 N1 2.101(4) 2 ?
Co1 N1 2.101(4) . ?
Co1 O4 2.118(6) . ?
Co1 O4 2.118(6) 2 ?
Co1 O2 2.205(4) 2 ?
Co1 O2 2.205(4) . ?
Co1 O1 2.231(5) 2 ?
Co1 O1 2.231(5) . ?
N1 C7 1.308(6) . ?
N1 C1 1.386(6) . ?
O2 N3 1.270(6) . ?
C9 C11 1.387(7) . ?
C9 C10 1.398(6) . ?
C9 C8 1.523(6) . ?
C2 N2 1.380(6) . ?
C2 C3 1.390(7) . ?
C2 C1 1.393(6) . ?
O1 N3 1.252(7) . ?
N2 C7 1.342(6) . ?
N2 C8 1.466(6) . ?
C11 C10 1.412(6) 5_575 ?
C11 C13 1.512(7) . ?
C1 C6 1.396(7) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C5 C6 1.376(8) . ?
C5 C4 1.398(8) . ?
C5 H5 0.9500 . ?
O3 N3 1.224(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C6 H6 0.9500 . ?
C10 C11 1.412(6) 5_575 ?
C10 C12 1.509(7) . ?
C4 C3 1.365(8) . ?
C4 H4 0.9500 . ?
C3 H3A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N4 C14 1.3497(11) . ?
N4 C16 1.475(8) . ?
N4 C15 1.480(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O4 C14 1.2299(11) . ?
C14 H14 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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 Co1 N1 174.5(2) 2 . ?
N1 Co1 O4 81.48(18) 2 . ?
N1 Co1 O4 93.14(18) . . ?
N1 Co1 O4 93.14(18) 2 2 ?
N1 Co1 O4 81.48(18) . 2 ?
O4 Co1 O4 23.4(3) . 2 ?
N1 Co1 O2 98.18(15) 2 2 ?
N1 Co1 O2 86.05(16) . 2 ?
O4 Co1 O2 130.9(2) . 2 ?
O4 Co1 O2 148.6(2) 2 2 ?
N1 Co1 O2 86.05(16) 2 . ?
N1 Co1 O2 98.18(15) . . ?
O4 Co1 O2 148.6(2) . . ?
O4 Co1 O2 130.9(2) 2 . ?
O2 Co1 O2 79.27(19) 2 . ?
N1 Co1 O1 92.00(17) 2 2 ?
N1 Co1 O1 87.34(17) . 2 ?
O4 Co1 O1 73.2(2) . 2 ?
O4 Co1 O1 93.0(2) 2 2 ?
O2 Co1 O1 57.64(15) 2 2 ?
O2 Co1 O1 136.16(16) . 2 ?
N1 Co1 O1 87.34(17) 2 . ?
N1 Co1 O1 92.00(17) . . ?
O4 Co1 O1 93.0(2) . . ?
O4 Co1 O1 73.2(2) 2 . ?
O2 Co1 O1 136.16(16) 2 . ?
O2 Co1 O1 57.64(15) . . ?
O1 Co1 O1 166.1(2) 2 . ?
C7 N1 C1 104.2(4) . . ?
C7 N1 Co1 119.4(4) . . ?
C1 N1 Co1 135.9(3) . . ?
N3 O2 Co1 93.5(3) . . ?
C11 C9 C10 121.8(4) . . ?
C11 C9 C8 119.0(4) . . ?
C10 C9 C8 119.2(4) . . ?
N2 C2 C3 131.2(4) . . ?
N2 C2 C1 105.9(4) . . ?
C3 C2 C1 122.8(4) . . ?
N3 O1 Co1 92.8(3) . . ?
C7 N2 C2 105.7(4) . . ?
C7 N2 C8 128.0(4) . . ?
C2 N2 C8 126.3(4) . . ?
C9 C11 C10 119.3(4) . 5_575 ?
C9 C11 C13 121.6(4) . . ?
C10 C11 C13 119.1(4) 5_575 . ?
N1 C1 C2 109.4(4) . . ?
N1 C1 C6 131.3(4) . . ?
C2 C1 C6 119.3(4) . . ?
N1 C7 N2 114.8(5) . . ?
N1 C7 H7 122.6 . . ?
N2 C7 H7 122.6 . . ?
N2 C8 C9 111.4(4) . . ?
N2 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N2 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C6 C5 C4 121.3(5) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C5 C6 C1 118.0(4) . . ?
C5 C6 H6 121.0 . . ?
C1 C6 H6 121.0 . . ?
C9 C10 C11 118.9(4) . 5_575 ?
C9 C10 C12 121.2(4) . . ?
C11 C10 C12 119.9(4) 5_575 . ?
O3 N3 O1 122.9(5) . . ?
O3 N3 O2 121.2(6) . . ?
O1 N3 O2 115.9(5) . . ?
C3 C4 C5 121.8(5) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C4 C3 C2 116.7(5) . . ?
C4 C3 H3A 121.7 . . ?
C2 C3 H3A 121.7 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 N4 C16 122.2(6) . . ?
C14 N4 C15 121.4(6) . . ?
C16 N4 C15 116.2(6) . . ?
C14 O4 Co1 121.4(4) . . ?
O4 C14 N4 124.3(7) . . ?
O4 C14 H14 117.8 . . ?
N4 C14 H14 117.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 N1 C7 -42.5(4) 2 . . . ?
O4 Co1 N1 C7 -32.3(5) . . . . ?
O4 Co1 N1 C7 -52.7(5) 2 . . . ?
O2 Co1 N1 C7 98.5(5) 2 . . . ?
O2 Co1 N1 C7 177.0(4) . . . . ?
O1 Co1 N1 C7 40.7(5) 2 . . . ?
O1 Co1 N1 C7 -125.4(5) . . . . ?
N1 Co1 N1 C1 146.2(5) 2 . . . ?
O4 Co1 N1 C1 156.3(5) . . . . ?
O4 Co1 N1 C1 135.9(5) 2 . . . ?
O2 Co1 N1 C1 -72.9(5) 2 . . . ?
O2 Co1 N1 C1 5.6(5) . . . . ?
O1 Co1 N1 C1 -130.7(5) 2 . . . ?
O1 Co1 N1 C1 63.2(5) . . . . ?
N1 Co1 O2 N3 -87.2(3) 2 . . . ?
N1 Co1 O2 N3 89.3(3) . . . . ?
O4 Co1 O2 N3 -20.7(5) . . . . ?
O4 Co1 O2 N3 3.5(4) 2 . . . ?
O2 Co1 O2 N3 173.7(4) 2 . . . ?
O1 Co1 O2 N3 -176.0(3) 2 . . . ?
O1 Co1 O2 N3 2.1(3) . . . . ?
N1 Co1 O1 N3 84.9(3) 2 . . . ?
N1 Co1 O1 N3 -100.6(3) . . . . ?
O4 Co1 O1 N3 166.2(3) . . . . ?
O4 Co1 O1 N3 178.9(4) 2 . . . ?
O2 Co1 O1 N3 -14.2(4) 2 . . . ?
O2 Co1 O1 N3 -2.2(3) . . . . ?
O1 Co1 O1 N3 172.4(3) 2 . . . ?
C3 C2 N2 C7 178.2(6) . . . . ?
C1 C2 N2 C7 -0.5(5) . . . . ?
C3 C2 N2 C8 -1.4(9) . . . . ?
C1 C2 N2 C8 179.9(4) . . . . ?
C10 C9 C11 C10 2.7(7) . . . 5_575 ?
C8 C9 C11 C10 -177.6(4) . . . 5_575 ?
C10 C9 C11 C13 -175.4(4) . . . . ?
C8 C9 C11 C13 4.3(6) . . . . ?
C7 N1 C1 C2 -0.8(6) . . . . ?
Co1 N1 C1 C2 171.4(4) . . . . ?
C7 N1 C1 C6 179.8(5) . . . . ?
Co1 N1 C1 C6 -7.9(8) . . . . ?
N2 C2 C1 N1 0.9(5) . . . . ?
C3 C2 C1 N1 -178.0(5) . . . . ?
N2 C2 C1 C6 -179.7(4) . . . . ?
C3 C2 C1 C6 1.5(7) . . . . ?
C1 N1 C7 N2 0.5(7) . . . . ?
Co1 N1 C7 N2 -173.3(4) . . . . ?
C2 N2 C7 N1 0.0(7) . . . . ?
C8 N2 C7 N1 179.6(5) . . . . ?
C7 N2 C8 C9 -1.3(8) . . . . ?
C2 N2 C8 C9 178.3(4) . . . . ?
C11 C9 C8 N2 -81.2(6) . . . . ?
C10 C9 C8 N2 98.5(5) . . . . ?
C4 C5 C6 C1 1.2(9) . . . . ?
N1 C1 C6 C5 177.2(5) . . . . ?
C2 C1 C6 C5 -2.1(7) . . . . ?
C11 C9 C10 C11 -2.7(7) . . . 5_575 ?
C8 C9 C10 C11 177.6(4) . . . 5_575 ?
C11 C9 C10 C12 176.5(5) . . . . ?
C8 C9 C10 C12 -3.2(6) . . . . ?
Co1 O1 N3 O3 -176.4(5) . . . . ?
Co1 O1 N3 O2 3.5(5) . . . . ?
Co1 O2 N3 O3 176.3(5) . . . . ?
Co1 O2 N3 O1 -3.6(5) . . . . ?
C6 C5 C4 C3 0.5(11) . . . . ?
C5 C4 C3 C2 -1.1(10) . . . . ?
N2 C2 C3 C4 -178.4(6) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
N1 Co1 O4 C14 139.5(8) 2 . . . ?
N1 Co1 O4 C14 -39.5(8) . . . . ?
O4 Co1 O4 C14 20.5(7) 2 . . . ?
O2 Co1 O4 C14 -127.0(7) 2 . . . ?
O2 Co1 O4 C14 71.8(9) . . . . ?
O1 Co1 O4 C14 -125.8(8) 2 . . . ?
O1 Co1 O4 C14 52.7(8) . . . . ?
Co1 O4 C14 N4 -161.0(9) . . . . ?
C16 N4 C14 O4 -0.9(19) . . . . ?
C15 N4 C14 O4 -176.4(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.808
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.072
_database_code_depnum_ccdc_archive 'CCDC 923231'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110510a
#TrackingRef 'complex 5. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H33 Cd N7 O7'
_chemical_formula_weight         704.02

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   16.651(5)
_cell_length_b                   9.660(3)
_cell_length_c                   19.921(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.878(5)
_cell_angle_gamma                90.00
_cell_volume                     3082.0(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2753
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      26.15

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8938
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7444
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2721
_reflns_number_gt                2296
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.0279P)²+0.0000P] 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         2721
_refine_ls_number_parameters     226
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.88638(3) 0.2500 0.04601(14) Uani 1 2 d S . .
N1 N 0.09132(16) 0.8673(2) 0.18523(13) 0.0475(6) Uani 1 1 d . A .
N2 N 0.13005(15) 0.7871(2) 0.09456(13) 0.0456(6) Uani 1 1 d . A .
N3 N -0.1100(2) 0.9913(5) 0.1264(2) 0.0781(10) Uani 1 1 d . . .
O1 O -0.10681(17) 0.8638(3) 0.13569(15) 0.0860(9) Uani 1 1 d . A .
O2 O -0.0676(2) 1.0648(3) 0.17500(17) 0.0844(8) Uani 1 1 d . A .
O3 O -0.1518(2) 1.0423(5) 0.07223(19) 0.1428(17) Uani 1 1 d . A .
C1 C 0.15823(18) 0.9447(3) 0.17836(16) 0.0421(7) Uani 1 1 d . . .
C2 C 0.18263(18) 0.8961(3) 0.12143(16) 0.0449(7) Uani 1 1 d . A .
C3 C 0.2466(2) 0.9562(4) 0.0998(2) 0.0684(10) Uani 1 1 d . . .
H3 H 0.2630 0.9221 0.0608 0.082 Uiso 1 1 calc R A .
C4 C 0.2849(2) 1.0670(5) 0.1374(2) 0.0869(14) Uani 1 1 d . A .
H4 H 0.3283 1.1125 0.1236 0.104 Uiso 1 1 calc R . .
C5 C 0.2628(2) 1.1157(4) 0.1950(2) 0.0795(12) Uani 1 1 d . . .
H5 H 0.2922 1.1919 0.2203 0.095 Uiso 1 1 calc R A .
C6 C 0.1991(2) 1.0564(4) 0.21652(19) 0.0589(9) Uani 1 1 d . A .
H6 H 0.1838 1.0906 0.2560 0.071 Uiso 1 1 calc R . .
C7 C 0.0773(2) 0.7770(3) 0.13422(17) 0.0530(8) Uani 1 1 d . . .
H7 H 0.0337 0.7106 0.1262 0.064 Uiso 1 1 calc R A .
C8 C 0.1320(2) 0.7039(3) 0.03374(17) 0.0534(9) Uani 1 1 d . . .
H8A H 0.1867 0.6568 0.0428 0.064 Uiso 1 1 calc R A .
H8B H 0.1260 0.7656 -0.0070 0.064 Uiso 1 1 calc R . .
C9 C 0.06324(19) 0.5968(3) 0.01683(16) 0.0447(7) Uani 1 1 d . A .
C10 C -0.0169(2) 0.6386(3) -0.01965(16) 0.0479(8) Uani 1 1 d . . .
C11 C 0.08061(19) 0.4602(3) 0.03718(17) 0.0503(8) Uani 1 1 d . . .
C12 C -0.0364(2) 0.7888(3) -0.0381(2) 0.0714(11) Uani 1 1 d . A .
H12A H 0.0103 0.8466 -0.0126 0.107 Uiso 1 1 calc R . .
H12B H -0.0871 0.8155 -0.0253 0.107 Uiso 1 1 calc R . .
H12C H -0.0453 0.8017 -0.0884 0.107 Uiso 1 1 calc R . .
C13 C 0.1668(2) 0.4166(4) 0.0790(2) 0.0823(12) Uani 1 1 d . A .
H13A H 0.2013 0.3975 0.0473 0.123 Uiso 1 1 calc R . .
H13B H 0.1628 0.3330 0.1057 0.123 Uiso 1 1 calc R . .
H13C H 0.1924 0.4912 0.1112 0.123 Uiso 1 1 calc R . .
O4 O -0.0148(4) 0.6488(4) 0.2507(6) 0.0603(18) Uani 0.50 1 d PD A -1
N4 N 0.0266(3) 0.4246(5) 0.2558(4) 0.0595(18) Uani 0.50 1 d PD A -1
C14 C 0.0316(3) 0.5575(5) 0.2401(4) 0.0571(18) Uani 0.50 1 d PD A -1
H14 H 0.0742 0.5837 0.2191 0.069 Uiso 0.50 1 calc PR A -1
C15 C 0.0833(8) 0.3191(11) 0.2422(8) 0.163(8) Uani 0.50 1 d PD A -1
H15A H 0.0514 0.2515 0.2087 0.244 Uiso 0.50 1 calc PR A -1
H15B H 0.1113 0.2719 0.2859 0.244 Uiso 0.50 1 calc PR A -1
H15C H 0.1251 0.3632 0.2229 0.244 Uiso 0.50 1 calc PR A -1
C16 C -0.0363(8) 0.3750(11) 0.2880(8) 0.171(9) Uani 0.50 1 d PD A -1
H16A H -0.0515 0.4496 0.3156 0.257 Uiso 0.50 1 calc PR A -1
H16B H -0.0141 0.2965 0.3186 0.257 Uiso 0.50 1 calc PR A -1
H16C H -0.0859 0.3456 0.2516 0.257 Uiso 0.50 1 calc PR A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.255(2) . ?
Cd1 N1 2.255(2) 2 ?
Cd1 O4 2.309(4) . ?
Cd1 O4 2.309(4) 2 ?
Cd1 O2 2.356(3) . ?
Cd1 O2 2.356(3) 2 ?
Cd1 O1 2.486(3) . ?
Cd1 O1 2.486(3) 2 ?
N1 C7 1.311(4) . ?
N1 C1 1.379(4) . ?
N2 C7 1.335(4) . ?
N2 C2 1.380(4) . ?
N2 C8 1.461(4) . ?
N3 O3 1.217(4) . ?
N3 O1 1.245(4) . ?
N3 O2 1.251(4) . ?
C1 C2 1.387(4) . ?
C1 C6 1.387(4) . ?
C2 C3 1.382(4) . ?
C3 C4 1.361(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.511(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.388(4) . ?
C9 C10 1.393(4) . ?
C10 C11 1.399(4) 5_565 ?
C10 C12 1.510(4) . ?
C11 C10 1.399(4) 5_565 ?
C11 C13 1.509(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O4 C14 1.2295(11) . ?
N4 C14 1.330(6) . ?
N4 C16 1.451(8) . ?
N4 C15 1.465(7) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N1 170.64(12) . 2 ?
N1 Cd1 O4 90.71(18) . . ?
N1 Cd1 O4 79.95(18) 2 . ?
N1 Cd1 O4 79.95(18) . 2 ?
N1 Cd1 O4 90.70(18) 2 2 ?
O4 Cd1 O4 12.5(2) . 2 ?
N1 Cd1 O2 88.67(10) . . ?
N1 Cd1 O2 98.20(10) 2 . ?
O4 Cd1 O2 134.3(3) . . ?
O4 Cd1 O2 139.2(3) 2 . ?
N1 Cd1 O2 98.20(10) . 2 ?
N1 Cd1 O2 88.67(10) 2 2 ?
O4 Cd1 O2 139.2(3) . 2 ?
O4 Cd1 O2 134.3(3) 2 2 ?
O2 Cd1 O2 85.95(17) . 2 ?
N1 Cd1 O1 83.93(10) . . ?
N1 Cd1 O1 95.25(10) 2 . ?
O4 Cd1 O1 82.4(3) . . ?
O4 Cd1 O1 87.6(3) 2 . ?
O2 Cd1 O1 52.08(10) . . ?
O2 Cd1 O1 138.00(12) 2 . ?
N1 Cd1 O1 95.25(10) . 2 ?
N1 Cd1 O1 83.93(10) 2 2 ?
O4 Cd1 O1 87.6(3) . 2 ?
O4 Cd1 O1 82.4(3) 2 2 ?
O2 Cd1 O1 138.00(12) . 2 ?
O2 Cd1 O1 52.08(10) 2 2 ?
O1 Cd1 O1 169.92(15) . 2 ?
C7 N1 C1 105.1(2) . . ?
C7 N1 Cd1 119.56(19) . . ?
C1 N1 Cd1 134.6(2) . . ?
C7 N2 C2 106.0(3) . . ?
C7 N2 C8 128.1(2) . . ?
C2 N2 C8 125.8(2) . . ?
O3 N3 O1 121.5(5) . . ?
O3 N3 O2 121.5(5) . . ?
O1 N3 O2 117.1(4) . . ?
N3 O1 Cd1 92.3(2) . . ?
N3 O2 Cd1 98.4(2) . . ?
N1 C1 C2 108.9(2) . . ?
N1 C1 C6 131.0(3) . . ?
C2 C1 C6 120.1(3) . . ?
N2 C2 C3 131.4(3) . . ?
N2 C2 C1 106.2(3) . . ?
C3 C2 C1 122.4(3) . . ?
C4 C3 C2 116.3(3) . . ?
C4 C3 H3 121.8 . . ?
C2 C3 H3 121.8 . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 117.3(3) . . ?
C5 C6 H6 121.4 . . ?
C1 C6 H6 121.4 . . ?
N1 C7 N2 113.8(3) . . ?
N1 C7 H7 123.1 . . ?
N2 C7 H7 123.1 . . ?
N2 C8 C9 112.0(2) . . ?
N2 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C11 C9 C10 121.4(3) . . ?
C11 C9 C8 120.1(3) . . ?
C10 C9 C8 118.5(3) . . ?
C9 C10 C11 119.0(3) . 5_565 ?
C9 C10 C12 121.2(3) . . ?
C11 C10 C12 119.8(3) 5_565 . ?
C9 C11 C10 119.5(3) . 5_565 ?
C9 C11 C13 121.1(3) . . ?
C10 C11 C13 119.3(3) 5_565 . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 O4 Cd1 129.7(4) . . ?
C14 N4 C16 121.5(5) . . ?
C14 N4 C15 122.8(6) . . ?
C16 N4 C15 115.7(6) . . ?
O4 C14 N4 124.7(5) . . ?
O4 C14 H14 117.7 . . ?
N4 C14 H14 117.7 . . ?

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
N1 Cd1 N1 C7 43.9(2) 2 . . . ?
O4 Cd1 N1 C7 40.7(4) . . . . ?
O4 Cd1 N1 C7 47.1(4) 2 . . . ?
O2 Cd1 N1 C7 -93.6(2) . . . . ?
O2 Cd1 N1 C7 -179.3(2) 2 . . . ?
O1 Cd1 N1 C7 -41.6(2) . . . . ?
O1 Cd1 N1 C7 128.3(2) 2 . . . ?
N1 Cd1 N1 C1 -147.6(3) 2 . . . ?
O4 Cd1 N1 C1 -150.7(4) . . . . ?
O4 Cd1 N1 C1 -144.4(4) 2 . . . ?
O2 Cd1 N1 C1 75.0(3) . . . . ?
O2 Cd1 N1 C1 -10.7(3) 2 . . . ?
O1 Cd1 N1 C1 127.0(3) . . . . ?
O1 Cd1 N1 C1 -63.1(3) 2 . . . ?
O3 N3 O1 Cd1 175.0(3) . . . . ?
O2 N3 O1 Cd1 -4.3(3) . . . . ?
N1 Cd1 O1 N3 -90.5(2) . . . . ?
N1 Cd1 O1 N3 98.9(2) 2 . . . ?
O4 Cd1 O1 N3 178.0(3) . . . . ?
O4 Cd1 O1 N3 -170.6(3) 2 . . . ?
O2 Cd1 O1 N3 2.6(2) . . . . ?
O2 Cd1 O1 N3 5.1(3) 2 . . . ?
O1 Cd1 O1 N3 -176.3(2) 2 . . . ?
O3 N3 O2 Cd1 -174.7(3) . . . . ?
O1 N3 O2 Cd1 4.6(4) . . . . ?
N1 Cd1 O2 N3 80.7(2) . . . . ?
N1 Cd1 O2 N3 -92.9(2) 2 . . . ?
O4 Cd1 O2 N3 -9.0(4) . . . . ?
O4 Cd1 O2 N3 7.8(3) 2 . . . ?
O2 Cd1 O2 N3 179.0(3) 2 . . . ?
O1 Cd1 O2 N3 -2.6(2) . . . . ?
O1 Cd1 O2 N3 177.1(2) 2 . . . ?
C7 N1 C1 C2 0.0(3) . . . . ?
Cd1 N1 C1 C2 -169.7(2) . . . . ?
C7 N1 C1 C6 178.4(3) . . . . ?
Cd1 N1 C1 C6 8.7(5) . . . . ?
C7 N2 C2 C3 -177.1(4) . . . . ?
C8 N2 C2 C3 1.4(6) . . . . ?
C7 N2 C2 C1 1.1(3) . . . . ?
C8 N2 C2 C1 179.7(3) . . . . ?
N1 C1 C2 N2 -0.7(3) . . . . ?
C6 C1 C2 N2 -179.3(3) . . . . ?
N1 C1 C2 C3 177.7(3) . . . . ?
C6 C1 C2 C3 -0.9(5) . . . . ?
N2 C2 C3 C4 177.9(4) . . . . ?
C1 C2 C3 C4 -0.2(6) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 C6 -1.6(7) . . . . ?
C4 C5 C6 C1 0.5(6) . . . . ?
N1 C1 C6 C5 -177.6(3) . . . . ?
C2 C1 C6 C5 0.7(5) . . . . ?
C1 N1 C7 N2 0.7(4) . . . . ?
Cd1 N1 C7 N2 172.3(2) . . . . ?
C2 N2 C7 N1 -1.2(4) . . . . ?
C8 N2 C7 N1 -179.7(3) . . . . ?
C7 N2 C8 C9 0.7(5) . . . . ?
C2 N2 C8 C9 -177.6(3) . . . . ?
N2 C8 C9 C11 -100.3(3) . . . . ?
N2 C8 C9 C10 80.1(4) . . . . ?
C11 C9 C10 C11 -1.3(5) . . . 5_565 ?
C8 C9 C10 C11 178.4(3) . . . 5_565 ?
C11 C9 C10 C12 176.5(3) . . . . ?
C8 C9 C10 C12 -3.8(4) . . . . ?
C10 C9 C11 C10 1.3(5) . . . 5_565 ?
C8 C9 C11 C10 -178.4(3) . . . 5_565 ?
C10 C9 C11 C13 -177.7(3) . . . . ?
C8 C9 C11 C13 2.7(5) . . . . ?
N1 Cd1 O4 C14 20.6(9) . . . . ?
N1 Cd1 O4 C14 -158.9(9) 2 . . . ?
O4 Cd1 O4 C14 -10(2) 2 . . . ?
O2 Cd1 O4 C14 109.5(8) . . . . ?
O2 Cd1 O4 C14 -82.8(9) 2 . . . ?
O1 Cd1 O4 C14 104.4(9) . . . . ?
O1 Cd1 O4 C14 -74.6(8) 2 . . . ?
Cd1 O4 C14 N4 165.1(8) . . . . ?
C16 N4 C14 O4 0.00(3) . . . . ?
C15 N4 C14 O4 180.00(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 923232'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_n110419a
#TrackingRef 'complex 6. cif.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H33 Cu N7 O7'
_chemical_formula_weight         655.16

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   16.271(3)
_cell_length_b                   9.664(3)
_cell_length_c                   19.485(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.811(6)
_cell_angle_gamma                90.00
_cell_volume                     2975.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1791
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      24.88

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1364
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7307
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2630
_reflns_number_gt                1888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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)+(0.0570P)²+6.0986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     patterson
_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         2630
_refine_ls_number_parameters     226
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.067
_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 0.0000 0.11424(6) 0.7500 0.0355(3) Uani 1 2 d S . .
O1 O 0.0965(2) 0.1177(3) 0.83702(15) 0.0536(9) Uani 1 1 d . . .
O2 O 0.0653(2) -0.0994(3) 0.8395(2) 0.0673(10) Uani 1 1 d . . .
O3 O 0.1404(3) 0.0001(5) 0.9327(2) 0.112(2) Uani 1 1 d . . .
N1 N 0.0788(2) 0.1193(3) 0.68584(15) 0.0350(8) Uani 1 1 d . . .
N2 N 0.1235(2) 0.1989(3) 0.59399(15) 0.0363(8) Uani 1 1 d . A .
N3 N 0.1016(3) 0.0034(5) 0.8705(2) 0.0604(12) Uani 1 1 d . . .
C1 C 0.1508(3) 0.0453(4) 0.68111(18) 0.0290(9) Uani 1 1 d . . .
C2 C 0.1787(3) 0.0933(4) 0.62275(19) 0.0307(9) Uani 1 1 d . A .
C3 C 0.2471(3) 0.0348(5) 0.6017(2) 0.0490(12) Uani 1 1 d . . .
H3A H 0.2648 0.0683 0.5618 0.059 Uiso 1 1 calc R A .
C4 C 0.2875(3) -0.0736(6) 0.6415(3) 0.0648(16) Uani 1 1 d . . .
H4 H 0.3341 -0.1169 0.6287 0.078 Uiso 1 1 calc R . .
C5 C 0.2611(3) -0.1214(6) 0.7009(3) 0.0639(16) Uani 1 1 d . . .
H5 H 0.2906 -0.1961 0.7276 0.077 Uiso 1 1 calc R A .
C6 C 0.1936(3) -0.0630(4) 0.7217(2) 0.0417(11) Uani 1 1 d . . .
H6 H 0.1767 -0.0956 0.7622 0.050 Uiso 1 1 calc R . .
C7 C 0.0662(3) 0.2085(4) 0.6328(2) 0.0448(12) Uani 1 1 d . . .
H7 H 0.0208 0.2729 0.6232 0.054 Uiso 1 1 calc R A .
C8 C 0.1279(3) 0.2835(4) 0.5310(2) 0.0446(12) Uani 1 1 d . . .
H8A H 0.1206 0.2223 0.4893 0.054 Uiso 1 1 calc R A .
H8B H 0.1844 0.3271 0.5390 0.054 Uiso 1 1 calc R . .
C9 C 0.0599(3) 0.3961(4) 0.51605(18) 0.0350(10) Uani 1 1 d . . .
C10 C 0.0828(3) 0.5316(4) 0.53875(19) 0.0366(10) Uani 1 1 d . . .
C11 C 0.0215(3) 0.6382(4) 0.52095(19) 0.0382(11) Uani 1 1 d . . .
C12 C 0.1706(3) 0.5665(5) 0.5819(2) 0.0529(13) Uani 1 1 d . . .
H12A H 0.1950 0.4856 0.6098 0.079 Uiso 1 1 calc R . .
H12B H 0.1672 0.6437 0.6138 0.079 Uiso 1 1 calc R . .
H12C H 0.2065 0.5930 0.5502 0.079 Uiso 1 1 calc R . .
C13 C 0.0477(4) 0.7866(4) 0.5417(2) 0.0580(14) Uani 1 1 d . . .
H13A H 0.0034 0.8501 0.5172 0.087 Uiso 1 1 calc R A .
H13B H 0.1008 0.8077 0.5284 0.087 Uiso 1 1 calc R . .
H13C H 0.0559 0.7976 0.5929 0.087 Uiso 1 1 calc R . .
N4 N -0.0257(3) 0.5685(5) 0.7412(2) 0.029(2) Uani 0.50 1 d PD A -1
O4 O 0.0230(3) 0.3461(5) 0.7575(5) 0.035(2) Uani 0.50 1 d PD A -1
C14 C -0.0285(4) 0.4322(6) 0.7636(3) 0.0299(18) Uani 0.50 1 d PD A -1
H14 H -0.0731 0.4056 0.7846 0.036 Uiso 0.50 1 calc PR A -1
C15 C 0.0391(6) 0.6165(7) 0.7093(5) 0.055(3) Uani 0.50 1 d PD A -1
H15A H 0.0856 0.5495 0.7178 0.082 Uiso 0.50 1 calc PR A -1
H15B H 0.0602 0.7061 0.7298 0.082 Uiso 0.50 1 calc PR A -1
H15C H 0.0161 0.6271 0.6583 0.082 Uiso 0.50 1 calc PR A -1
C16 C -0.0897(5) 0.6665(7) 0.7502(4) 0.039(2) Uani 0.50 1 d PD A -1
H16A H -0.1304 0.6200 0.7723 0.059 Uiso 0.50 1 calc PR A -1
H16B H -0.1194 0.7028 0.7039 0.059 Uiso 0.50 1 calc PR A -1
H16C H -0.0628 0.7429 0.7804 0.059 Uiso 0.50 1 calc PR A -1


_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 1.994(3) . ?
Cu1 N1 1.994(3) 2_556 ?
Cu1 O1 2.017(3) 2_556 ?
Cu1 O1 2.018(3) . ?
Cu1 O4 2.271(5) 2_556 ?
Cu1 O4 2.271(5) . ?
O1 N3 1.276(5) . ?
O2 N3 1.238(5) . ?
O3 N3 1.226(5) . ?
N1 C7 1.324(5) . ?
N1 C1 1.394(5) . ?
N2 C7 1.336(5) . ?
N2 C2 1.386(5) . ?
N2 C8 1.490(5) . ?
C1 C6 1.394(5) . ?
C1 C2 1.400(5) . ?
C2 C3 1.394(6) . ?
C3 C4 1.375(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.405(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.530(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.389(6) 5_566 ?
C9 C10 1.404(5) . ?
C10 C11 1.418(6) . ?
C10 C12 1.513(7) . ?
C11 C9 1.389(6) 5_566 ?
C11 C13 1.523(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N4 C14 1.392(7) . ?
N4 C15 1.425(8) . ?
N4 C16 1.449(7) . ?
O4 C14 1.206(6) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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 177.18(18) . 2_556 ?
N1 Cu1 O1 87.74(13) . 2_556 ?
N1 Cu1 O1 92.22(13) 2_556 2_556 ?
N1 Cu1 O1 92.21(13) . . ?
N1 Cu1 O1 87.74(13) 2_556 . ?
O1 Cu1 O1 178.08(18) 2_556 . ?
N1 Cu1 O4 93.2(2) . 2_556 ?
N1 Cu1 O4 84.0(2) 2_556 2_556 ?
O1 Cu1 O4 81.14(19) 2_556 2_556 ?
O1 Cu1 O4 96.94(19) . 2_556 ?
N1 Cu1 O4 84.0(2) . . ?
N1 Cu1 O4 93.2(2) 2_556 . ?
O1 Cu1 O4 96.94(19) 2_556 . ?
O1 Cu1 O4 81.14(19) . . ?
O4 Cu1 O4 18.6(3) 2_556 . ?
N3 O1 Cu1 111.0(3) . . ?
C7 N1 C1 104.9(3) . . ?
C7 N1 Cu1 120.2(3) . . ?
C1 N1 Cu1 134.8(2) . . ?
C7 N2 C2 107.1(3) . . ?
C7 N2 C8 127.2(3) . . ?
C2 N2 C8 125.7(3) . . ?
O3 N3 O2 122.3(4) . . ?
O3 N3 O1 118.9(4) . . ?
O2 N3 O1 118.7(4) . . ?
C6 C1 N1 131.4(4) . . ?
C6 C1 C2 119.6(4) . . ?
N1 C1 C2 108.9(3) . . ?
N2 C2 C3 131.7(4) . . ?
N2 C2 C1 105.5(3) . . ?
C3 C2 C1 122.7(4) . . ?
C4 C3 C2 116.9(4) . . ?
C4 C3 H3A 121.6 . . ?
C2 C3 H3A 121.6 . . ?
C3 C4 C5 121.0(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 121.9(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 H6 121.1 . . ?
C1 C6 H6 121.1 . . ?
N1 C7 N2 113.5(4) . . ?
N1 C7 H7 123.3 . . ?
N2 C7 H7 123.3 . . ?
N2 C8 C9 111.9(3) . . ?
N2 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C11 C9 C10 122.4(4) 5_566 . ?
C11 C9 C8 119.1(4) 5_566 . ?
C10 C9 C8 118.5(4) . . ?
C9 C10 C11 118.8(4) . . ?
C9 C10 C12 121.9(4) . . ?
C11 C10 C12 119.3(4) . . ?
C9 C11 C10 118.8(4) 5_566 . ?
C9 C11 C13 122.3(4) 5_566 . ?
C10 C11 C13 118.9(4) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 N4 C15 121.9(4) . . ?
C14 N4 C16 120.2(4) . . ?
C15 N4 C16 117.9(4) . . ?
C14 O4 Cu1 125.4(5) . . ?
O4 C14 N4 123.1(6) . . ?
O4 C14 H14 118.4 . . ?
N4 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
N1 Cu1 O1 N3 -112.4(3) . . . . ?
N1 Cu1 O1 N3 70.4(3) 2_556 . . . ?
O1 Cu1 O1 N3 159.1(3) 2_556 . . . ?
O4 Cu1 O1 N3 154.1(4) 2_556 . . . ?
O4 Cu1 O1 N3 164.0(4) . . . . ?
N1 Cu1 N1 C7 -42.4(3) 2_556 . . . ?
O1 Cu1 N1 C7 46.7(3) 2_556 . . . ?
O1 Cu1 N1 C7 -131.3(3) . . . . ?
O4 Cu1 N1 C7 -34.3(4) 2_556 . . . ?
O4 Cu1 N1 C7 -50.5(4) . . . . ?
N1 Cu1 N1 C1 138.4(4) 2_556 . . . ?
O1 Cu1 N1 C1 -132.5(4) 2_556 . . . ?
O1 Cu1 N1 C1 49.4(4) . . . . ?
O4 Cu1 N1 C1 146.5(4) 2_556 . . . ?
O4 Cu1 N1 C1 130.3(4) . . . . ?
Cu1 O1 N3 O3 -160.7(4) . . . . ?
Cu1 O1 N3 O2 17.6(5) . . . . ?
C7 N1 C1 C6 -178.9(4) . . . . ?
Cu1 N1 C1 C6 0.4(7) . . . . ?
C7 N1 C1 C2 -0.9(4) . . . . ?
Cu1 N1 C1 C2 178.4(3) . . . . ?
C7 N2 C2 C3 176.4(4) . . . . ?
C8 N2 C2 C3 -2.9(7) . . . . ?
C7 N2 C2 C1 -1.3(4) . . . . ?
C8 N2 C2 C1 179.3(4) . . . . ?
C6 C1 C2 N2 179.6(3) . . . . ?
N1 C1 C2 N2 1.4(4) . . . . ?
C6 C1 C2 C3 1.7(6) . . . . ?
N1 C1 C2 C3 -176.6(4) . . . . ?
N2 C2 C3 C4 -177.9(5) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C2 C3 C4 C5 -0.6(8) . . . . ?
C3 C4 C5 C6 0.5(9) . . . . ?
C4 C5 C6 C1 0.7(8) . . . . ?
N1 C1 C6 C5 176.0(4) . . . . ?
C2 C1 C6 C5 -1.7(6) . . . . ?
C1 N1 C7 N2 0.0(5) . . . . ?
Cu1 N1 C7 N2 -179.4(3) . . . . ?
C2 N2 C7 N1 0.8(5) . . . . ?
C8 N2 C7 N1 -179.9(4) . . . . ?
C7 N2 C8 C9 3.8(6) . . . . ?
C2 N2 C8 C9 -177.0(4) . . . . ?
N2 C8 C9 C11 -82.1(4) . . . 5_566 ?
N2 C8 C9 C10 99.6(4) . . . . ?
C11 C9 C10 C11 -2.5(6) 5_566 . . . ?
C8 C9 C10 C11 175.8(3) . . . . ?
C11 C9 C10 C12 177.1(4) 5_566 . . . ?
C8 C9 C10 C12 -4.6(5) . . . . ?
C9 C10 C11 C9 2.4(6) . . . 5_566 ?
C12 C10 C11 C9 -177.2(4) . . . 5_566 ?
C9 C10 C11 C13 -176.4(3) . . . . ?
C12 C10 C11 C13 4.0(5) . . . . ?
N1 Cu1 O4 C14 145.8(6) . . . . ?
N1 Cu1 O4 C14 -33.8(5) 2_556 . . . ?
O1 Cu1 O4 C14 58.8(6) 2_556 . . . ?
O1 Cu1 O4 C14 -121.0(6) . . . . ?
O4 Cu1 O4 C14 26.7(10) 2_556 . . . ?
Cu1 O4 C14 N4 -154.2(5) . . . . ?
C15 N4 C14 O4 0.00(2) . . . . ?
C16 N4 C14 O4 179.999(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.069


_database_code_depnum_ccdc_archive 'CCDC 923233'
