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

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#
#                 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
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H54 Cd2 N8 O15'
_chemical_formula_weight         1568.09

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                   25.6565(6)
_cell_length_b                   12.4636(3)
_cell_length_c                   21.2198(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.910(2)
_cell_angle_gamma                90.00
_cell_volume                     6525.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    277(2)
_cell_measurement_reflns_used    2620
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      20.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3176
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      277(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.0855
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24648
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6227
_reflns_number_gt                4126
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1996)'
_computing_cell_refinement       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          SQUEEZE

_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)+(0.0406P)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         6227
_refine_ls_number_parameters     439
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      1.008
_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
Cd1 Cd 0.189085(11) 0.60933(2) 0.488314(14) 0.03741(11) Uani 1 1 d . . .
O1 O 0.24001(10) 0.7182(2) 0.56719(12) 0.0396(7) Uani 1 1 d . . .
O2 O 0.24877(11) 0.8959(2) 0.56838(14) 0.0532(8) Uani 1 1 d . . .
O3 O -0.00624(12) 0.8943(3) 0.63554(17) 0.0656(9) Uani 1 1 d . . .
O4 O 0.03966(12) 0.8229(3) 0.72921(16) 0.0844(12) Uani 1 1 d . . .
H4A H 0.0205 0.7732 0.7388 0.101 Uiso 0.50 1 d PR . .
O5 O 0.40782(18) 0.6511(5) 0.8012(3) 0.160(2) Uani 1 1 d U . .
O6 O 0.37605(16) 0.8050(5) 0.7561(2) 0.1155(16) Uani 1 1 d U . .
H6A H 0.4084 0.8197 0.7671 0.139 Uiso 0.50 1 calc PR . .
N1 N 0.22351(13) 0.4587(3) 0.55114(16) 0.0396(8) Uani 1 1 d . . .
N2 N 0.15296(13) 0.4541(3) 0.42858(16) 0.0430(9) Uani 1 1 d . . .
N3 N 0.12259(13) 0.7290(3) 0.43786(16) 0.0460(9) Uani 1 1 d . . .
N4 N 0.11251(13) 0.5902(3) 0.53423(17) 0.0487(9) Uani 1 1 d . . .
C1 C 0.17843(14) 0.8240(3) 0.60700(17) 0.0333(9) Uani 1 1 d . . .
C2 C 0.13610(15) 0.8897(3) 0.57371(18) 0.0403(10) Uani 1 1 d . . .
H2A H 0.1392 0.9277 0.5372 0.048 Uiso 1 1 calc R . .
C3 C 0.08957(15) 0.8997(3) 0.59380(19) 0.0415(10) Uani 1 1 d . . .
H3A H 0.0612 0.9426 0.5703 0.050 Uiso 1 1 calc R . .
C4 C 0.08515(14) 0.8459(3) 0.64869(19) 0.0389(10) Uani 1 1 d . . .
C5 C 0.12792(15) 0.7830(3) 0.68309(19) 0.0415(10) Uani 1 1 d . . .
H5A H 0.1253 0.7490 0.7211 0.050 Uiso 1 1 calc R . .
C6 C 0.17449(15) 0.7688(3) 0.66301(18) 0.0354(9) Uani 1 1 d . . .
C7 C 0.21906(9) 0.7009(2) 0.70369(11) 0.0351(9) Uani 1 1 d G . .
C8 C 0.20638(11) 0.6046(2) 0.72908(14) 0.0560(12) Uani 1 1 d G . .
H8A H 0.1705 0.5817 0.7193 0.067 Uiso 1 1 calc R . .
C9 C 0.24725(17) 0.5425(2) 0.76912(15) 0.0817(17) Uani 1 1 d G . .
H9A H 0.2388 0.4781 0.7861 0.098 Uiso 1 1 calc R . .
C10 C 0.30081(14) 0.5767(3) 0.78378(13) 0.0799(18) Uani 1 1 d G . .
H10A H 0.3282 0.5352 0.8106 0.096 Uiso 1 1 calc R . .
C11 C 0.31349(9) 0.6730(3) 0.75840(15) 0.0655(14) Uani 1 1 d G . .
C12 C 0.27262(11) 0.7351(2) 0.71835(13) 0.0494(11) Uani 1 1 d G . .
H12A H 0.2811 0.7995 0.7014 0.059 Uiso 1 1 calc R . .
C13 C 0.22571(15) 0.8111(4) 0.57893(18) 0.0371(10) Uani 1 1 d . . .
C14 C 0.03485(17) 0.8577(4) 0.6715(2) 0.0490(12) Uani 1 1 d . . .
C15 C 0.3690(3) 0.7070(8) 0.7751(3) 0.101(2) Uani 1 1 d U . .
C16 C 0.25889(17) 0.4602(4) 0.6102(2) 0.0483(11) Uani 1 1 d . . .
H16A H 0.2739 0.5256 0.6271 0.058 Uiso 1 1 calc R . .
C17 C 0.27427(19) 0.3686(4) 0.6476(2) 0.0554(13) Uani 1 1 d . . .
H17A H 0.2990 0.3728 0.6887 0.067 Uiso 1 1 calc R . .
C18 C 0.25316(19) 0.2737(4) 0.6238(2) 0.0573(13) Uani 1 1 d . . .
H18A H 0.2640 0.2116 0.6482 0.069 Uiso 1 1 calc R . .
C19 C 0.21475(18) 0.2672(4) 0.5622(2) 0.0491(12) Uani 1 1 d . . .
C20 C 0.20172(16) 0.3635(3) 0.5263(2) 0.0399(11) Uani 1 1 d . . .
C21 C 0.16402(16) 0.3611(3) 0.4619(2) 0.0390(10) Uani 1 1 d . . .
C22 C 0.14067(17) 0.2629(4) 0.4365(2) 0.0491(12) Uani 1 1 d . . .
C23 C 0.10520(18) 0.2651(5) 0.3736(3) 0.0633(15) Uani 1 1 d . . .
H23A H 0.0886 0.2020 0.3548 0.076 Uiso 1 1 calc R . .
C24 C 0.09465(19) 0.3579(5) 0.3397(3) 0.0653(15) Uani 1 1 d . . .
H24A H 0.0715 0.3592 0.2975 0.078 Uiso 1 1 calc R . .
C25 C 0.11914(17) 0.4513(4) 0.3692(2) 0.0545(12) Uani 1 1 d . . .
H25A H 0.1113 0.5153 0.3459 0.065 Uiso 1 1 calc R . .
C26 C 0.1894(2) 0.1697(4) 0.5336(3) 0.0603(13) Uani 1 1 d . . .
H26A H 0.1976 0.1059 0.5569 0.072 Uiso 1 1 calc R . .
C27 C 0.1540(2) 0.1684(4) 0.4739(3) 0.0630(14) Uani 1 1 d . . .
H27A H 0.1379 0.1039 0.4569 0.076 Uiso 1 1 calc R . .
C28 C 0.12843(19) 0.7997(4) 0.3938(2) 0.0600(13) Uani 1 1 d . . .
H28A H 0.1613 0.8026 0.3832 0.072 Uiso 1 1 calc R . .
C29 C 0.0872(2) 0.8701(4) 0.3626(3) 0.0777(16) Uani 1 1 d . . .
H29A H 0.0923 0.9187 0.3316 0.093 Uiso 1 1 calc R . .
C30 C 0.0393(2) 0.8661(5) 0.3786(3) 0.0817(18) Uani 1 1 d . . .
H30A H 0.0109 0.9112 0.3576 0.098 Uiso 1 1 calc R . .
C31 C 0.03249(18) 0.7958(5) 0.4259(3) 0.0647(14) Uani 1 1 d . . .
C32 C 0.07546(15) 0.7265(4) 0.4551(2) 0.0487(11) Uani 1 1 d . . .
C33 C 0.07053(16) 0.6539(4) 0.5059(2) 0.0479(12) Uani 1 1 d . . .
C34 C 0.02210(18) 0.6541(5) 0.5254(3) 0.0653(15) Uani 1 1 d . . .
C35 C 0.0198(2) 0.5830(5) 0.5751(3) 0.0849(19) Uani 1 1 d . . .
H35A H -0.0115 0.5800 0.5891 0.102 Uiso 1 1 calc R . .
C36 C 0.0613(2) 0.5192(5) 0.6031(3) 0.0772(17) Uani 1 1 d . . .
H36A H 0.0596 0.4723 0.6366 0.093 Uiso 1 1 calc R . .
C37 C 0.10724(19) 0.5251(4) 0.5807(2) 0.0624(14) Uani 1 1 d . . .
H37A H 0.1361 0.4800 0.5999 0.075 Uiso 1 1 calc R . .
C38 C -0.0162(2) 0.7898(5) 0.4465(3) 0.0847(19) Uani 1 1 d . . .
H38A H -0.0456 0.8329 0.4260 0.102 Uiso 1 1 calc R . .
C39 C -0.0204(2) 0.7254(6) 0.4933(3) 0.089(2) Uani 1 1 d . . .
H39A H -0.0522 0.7259 0.5063 0.107 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
Cd1 O2 2.246(2) 7_566 ?
Cd1 O1 2.270(3) . ?
Cd1 N3 2.298(3) . ?
Cd1 N1 2.331(3) . ?
Cd1 N2 2.359(4) . ?
Cd1 N4 2.432(3) . ?
O1 C13 1.260(5) . ?
O2 C13 1.260(4) . ?
O2 Cd1 2.246(2) 7_566 ?
O3 C14 1.208(5) . ?
O4 C14 1.273(5) . ?
O4 H4A 0.8499 . ?
O5 C15 1.217(7) . ?
O6 C15 1.315(8) . ?
O6 H6A 0.8200 . ?
N1 C16 1.331(5) . ?
N1 C20 1.355(5) . ?
N2 C25 1.320(5) . ?
N2 C21 1.347(5) . ?
N3 C28 1.323(5) . ?
N3 C32 1.356(5) . ?
N4 C37 1.312(5) . ?
N4 C33 1.341(5) . ?
C1 C2 1.389(5) . ?
C1 C6 1.401(5) . ?
C1 C13 1.499(5) . ?
C2 C3 1.379(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.375(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(5) . ?
C4 C14 1.505(5) . ?
C5 C6 1.386(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.493(4) . ?
C7 C8 1.3900 . ?
C7 C12 1.3900 . ?
C8 C9 1.3900 . ?
C8 H8A 0.9300 . ?
C9 C10 1.3900 . ?
C9 H9A 0.9300 . ?
C10 C11 1.3900 . ?
C10 H10A 0.9300 . ?
C11 C12 1.3900 . ?
C11 C15 1.435(7) . ?
C12 H12A 0.9300 . ?
C16 C17 1.385(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.341(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.406(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.411(6) . ?
C19 C26 1.434(6) . ?
C20 C21 1.442(6) . ?
C21 C22 1.403(5) . ?
C22 C23 1.395(6) . ?
C22 C27 1.409(6) . ?
C23 C24 1.350(7) . ?
C23 H23A 0.9300 . ?
C24 C25 1.388(7) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.340(7) . ?
C26 H26A 0.9300 . ?
C27 H27A 0.9300 . ?
C28 C29 1.393(6) . ?
C28 H28A 0.9300 . ?
C29 C30 1.364(7) . ?
C29 H29A 0.9300 . ?
C30 C31 1.377(7) . ?
C30 H30A 0.9300 . ?
C31 C32 1.404(6) . ?
C31 C38 1.435(7) . ?
C32 C33 1.439(6) . ?
C33 C34 1.413(6) . ?
C34 C35 1.391(8) . ?
C34 C39 1.426(8) . ?
C35 C36 1.332(7) . ?
C35 H35A 0.9300 . ?
C36 C37 1.388(6) . ?
C36 H36A 0.9300 . ?
C37 H37A 0.9300 . ?
C38 C39 1.305(8) . ?
C38 H38A 0.9300 . ?
C39 H39A 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
O2 Cd1 O1 93.58(10) 7_566 . ?
O2 Cd1 N3 108.32(12) 7_566 . ?
O1 Cd1 N3 99.15(11) . . ?
O2 Cd1 N1 94.01(11) 7_566 . ?
O1 Cd1 N1 90.50(11) . . ?
N3 Cd1 N1 154.90(12) . . ?
O2 Cd1 N2 85.45(10) 7_566 . ?
O1 Cd1 N2 161.56(11) . . ?
N3 Cd1 N2 98.63(12) . . ?
N1 Cd1 N2 71.24(12) . . ?
O2 Cd1 N4 169.01(11) 7_566 . ?
O1 Cd1 N4 97.37(10) . . ?
N3 Cd1 N4 70.87(12) . . ?
N1 Cd1 N4 85.00(12) . . ?
N2 Cd1 N4 83.87(11) . . ?
C13 O1 Cd1 123.7(2) . . ?
C13 O2 Cd1 120.5(3) . 7_566 ?
C14 O4 H4A 124.7 . . ?
C15 O6 H6A 109.5 . . ?
C16 N1 C20 118.7(4) . . ?
C16 N1 Cd1 125.5(3) . . ?
C20 N1 Cd1 115.6(3) . . ?
C25 N2 C21 117.9(4) . . ?
C25 N2 Cd1 126.4(3) . . ?
C21 N2 Cd1 115.4(3) . . ?
C28 N3 C32 119.2(4) . . ?
C28 N3 Cd1 123.3(3) . . ?
C32 N3 Cd1 117.5(3) . . ?
C37 N4 C33 117.9(4) . . ?
C37 N4 Cd1 128.5(3) . . ?
C33 N4 Cd1 113.6(3) . . ?
C2 C1 C6 119.5(3) . . ?
C2 C1 C13 117.8(3) . . ?
C6 C1 C13 122.6(3) . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 C14 120.1(4) . . ?
C5 C4 C14 120.8(4) . . ?
C4 C5 C6 122.5(4) . . ?
C4 C5 H5A 118.8 . . ?
C6 C5 H5A 118.8 . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 C7 118.9(3) . . ?
C1 C6 C7 123.2(3) . . ?
C8 C7 C12 120.0 . . ?
C8 C7 C6 119.4(2) . . ?
C12 C7 C6 120.6(2) . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 C15 118.8(4) . . ?
C12 C11 C15 121.2(4) . . ?
C11 C12 C7 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C7 C12 H12A 120.0 . . ?
O2 C13 O1 124.0(3) . . ?
O2 C13 C1 116.8(4) . . ?
O1 C13 C1 119.3(4) . . ?
O3 C14 O4 125.0(4) . . ?
O3 C14 C4 120.7(4) . . ?
O4 C14 C4 114.3(4) . . ?
O5 C15 O6 120.5(7) . . ?
O5 C15 C11 125.2(8) . . ?
O6 C15 C11 114.2(6) . . ?
N1 C16 C17 122.7(4) . . ?
N1 C16 H16A 118.6 . . ?
C17 C16 H16A 118.6 . . ?
C18 C17 C16 119.4(5) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C17 C18 C19 120.5(5) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C18 C19 C20 117.1(4) . . ?
C18 C19 C26 124.3(5) . . ?
C20 C19 C26 118.6(4) . . ?
N1 C20 C19 121.5(4) . . ?
N1 C20 C21 119.0(4) . . ?
C19 C20 C21 119.5(4) . . ?
N2 C21 C22 122.8(4) . . ?
N2 C21 C20 118.0(4) . . ?
C22 C21 C20 119.1(4) . . ?
C23 C22 C21 116.6(5) . . ?
C23 C22 C27 123.3(5) . . ?
C21 C22 C27 120.0(4) . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 118.6(5) . . ?
C23 C24 H24A 120.7 . . ?
C25 C24 H24A 120.7 . . ?
N2 C25 C24 123.3(5) . . ?
N2 C25 H25A 118.3 . . ?
C24 C25 H25A 118.3 . . ?
C27 C26 C19 121.5(5) . . ?
C27 C26 H26A 119.3 . . ?
C19 C26 H26A 119.3 . . ?
C26 C27 C22 121.3(5) . . ?
C26 C27 H27A 119.4 . . ?
C22 C27 H27A 119.4 . . ?
N3 C28 C29 122.4(5) . . ?
N3 C28 H28A 118.8 . . ?
C29 C28 H28A 118.8 . . ?
C30 C29 C28 118.5(5) . . ?
C30 C29 H29A 120.7 . . ?
C28 C29 H29A 120.7 . . ?
C29 C30 C31 120.4(5) . . ?
C29 C30 H30A 119.8 . . ?
C31 C30 H30A 119.8 . . ?
C30 C31 C32 118.2(5) . . ?
C30 C31 C38 123.3(5) . . ?
C32 C31 C38 118.5(5) . . ?
N3 C32 C31 121.1(4) . . ?
N3 C32 C33 119.0(4) . . ?
C31 C32 C33 119.9(4) . . ?
N4 C33 C34 122.1(5) . . ?
N4 C33 C32 118.9(4) . . ?
C34 C33 C32 118.9(4) . . ?
C35 C34 C33 116.4(5) . . ?
C35 C34 C39 124.9(5) . . ?
C33 C34 C39 118.6(5) . . ?
C36 C35 C34 121.5(5) . . ?
C36 C35 H35A 119.2 . . ?
C34 C35 H35A 119.2 . . ?
C35 C36 C37 117.8(5) . . ?
C35 C36 H36A 121.1 . . ?
C37 C36 H36A 121.1 . . ?
N4 C37 C36 124.2(5) . . ?
N4 C37 H37A 117.9 . . ?
C36 C37 H37A 117.9 . . ?
C39 C38 C31 121.6(5) . . ?
C39 C38 H38A 119.2 . . ?
C31 C38 H38A 119.2 . . ?
C38 C39 C34 122.4(5) . . ?
C38 C39 H39A 118.8 . . ?
C34 C39 H39A 118.8 . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.077

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.107 0.250 60 29 ' '
2 0.500 -0.107 0.750 60 29 ' '
3 0.000 0.393 0.750 60 29 ' '
4 0.000 0.607 0.250 60 29 ' '
_platon_squeeze_details          
; 
 Electron density contributions from three disordered water molecules were 
 removed by using the SQUEEZE procedure from the PLATON software.
 
 Because of the hydrophobic effect, the disordered water molecules
 can be easily lost above room temperature, which is why only one water molecule
 shown in the Elemental and TG analysis results.
;

# start Validation Reply Form

_vrf_PLAT420_a                   
;

PROBLEM: ALERT: D-H Without Acceptor       O6     -   *H6A
RESPONSE: This is possible that there could have been an O6-H6AO 
hydrogen bond with one of squeezed-out water oxygen atoms.
;

# end Validation Reply Form 
_exptl_crystal_preparation       Luminescent
_database_code_depnum_ccdc_archive 'CCDC 996435'
#######################################################################
#
#                 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_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H40 Cu2 N4 O16'
_chemical_formula_weight         1079.94

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.46830(10)
_cell_length_b                   9.9602(2)
_cell_length_c                   15.8627(3)
_cell_angle_alpha                81.1100(10)
_cell_angle_beta                 88.0780(10)
_cell_angle_gamma                69.0990(10)
_cell_volume                     1088.78(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle-like
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             554
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8570
_exptl_absorpt_correction_T_max  0.9013
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'

_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 Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17461
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4928
_reflns_number_gt                4242
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1996)'
_computing_cell_refinement       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of 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.

 The hydrogen atoms of the water and carboxylate group were located from 
 difference maps and refined with isotropic temperature factors.
 To restrains the bond length and bond angles, 
 the instrucitons are used as follows: 
 DFIX 0.85 0.01 O1W H1WA O1W H1WB O2W H2WA O2W H2WB
 DFIX 1.39 0.01 H1WA H1WB H2WA H2WB
 DFIX 0.85 0.01 O5 H5O
;

_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)+(0.0466P)²+0.4174P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4928
_refine_ls_number_parameters     345
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0835
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.63519(3) 0.57262(2) 0.746974(14) 0.02727(9) Uani 1 1 d . . .
O1 O 0.7580(2) 0.31546(15) 0.62914(9) 0.0343(3) Uani 1 1 d . . .
O2 O 0.6521(2) 0.55583(15) 0.62830(8) 0.0315(3) Uani 1 1 d . . .
O3 O 0.7861(2) 0.65370(19) 0.19339(9) 0.0420(4) Uani 1 1 d . . .
O4 O 1.09402(19) 0.54984(16) 0.22029(8) 0.0311(3) Uani 1 1 d . . .
O5 O 1.0147(3) 0.2217(2) 0.08348(11) 0.0525(5) Uani 1 1 d D . .
H5O H 1.026(5) 0.212(4) 0.0310(9) 0.097(13) Uiso 1 1 d D . .
O6 O 1.2216(3) -0.0043(2) 0.10056(13) 0.0712(6) Uani 1 1 d . . .
O1W O 0.5758(2) 0.36848(17) 0.78260(10) 0.0352(3) Uani 1 1 d D . .
O2W O 1.0061(4) 0.8059(2) 1.07828(12) 0.0673(6) Uani 1 1 d D . .
N1 N 0.4168(2) 0.76330(18) 0.72002(10) 0.0267(3) Uani 1 1 d . . .
N2 N 0.5984(2) 0.63325(19) 0.86222(10) 0.0305(4) Uani 1 1 d . . .
C1 C 0.7711(3) 0.4710(2) 0.50117(11) 0.0228(4) Uani 1 1 d . . .
C2 C 0.6984(3) 0.6107(2) 0.45601(12) 0.0267(4) Uani 1 1 d . . .
H2A H 0.6166 0.6862 0.4823 0.032 Uiso 1 1 calc R . .
C3 C 0.7473(3) 0.6376(2) 0.37226(12) 0.0259(4) Uani 1 1 d . . .
H3A H 0.6944 0.7310 0.3419 0.031 Uiso 1 1 calc R . .
C4 C 0.8748(3) 0.5274(2) 0.33209(11) 0.0224(4) Uani 1 1 d . . .
C5 C 0.9473(3) 0.3854(2) 0.37616(11) 0.0231(4) Uani 1 1 d . . .
C6 C 0.8908(3) 0.3602(2) 0.46007(12) 0.0238(4) Uani 1 1 d . . .
H6A H 0.9350 0.2657 0.4895 0.029 Uiso 1 1 calc R . .
C7 C 1.0745(3) 0.2591(2) 0.33713(12) 0.0254(4) Uani 1 1 d . . .
C8 C 1.0503(3) 0.2466(2) 0.25249(13) 0.0281(4) Uani 1 1 d . . .
H8A H 0.9579 0.3215 0.2179 0.034 Uiso 1 1 calc R . .
C9 C 1.1634(3) 0.1227(2) 0.21889(14) 0.0322(4) Uani 1 1 d . . .
C10 C 1.2985(3) 0.0096(2) 0.27034(16) 0.0393(5) Uani 1 1 d . . .
H10A H 1.3721 -0.0738 0.2483 0.047 Uiso 1 1 calc R . .
C11 C 1.3236(3) 0.0208(2) 0.35414(16) 0.0386(5) Uani 1 1 d . . .
H11A H 1.4141 -0.0553 0.3888 0.046 Uiso 1 1 calc R . .
C12 C 1.2147(3) 0.1450(2) 0.38713(14) 0.0318(4) Uani 1 1 d . . .
H12A H 1.2354 0.1525 0.4434 0.038 Uiso 1 1 calc R . .
C13 C 0.7243(3) 0.4410(2) 0.59365(11) 0.0244(4) Uani 1 1 d . . .
C14 C 0.9231(3) 0.5776(2) 0.24238(11) 0.0245(4) Uani 1 1 d . . .
C15 C 1.1370(4) 0.1065(3) 0.12907(15) 0.0406(5) Uani 1 1 d . . .
C16 C 0.6972(3) 0.5563(3) 0.93329(14) 0.0430(6) Uani 1 1 d . . .
H16A H 0.7873 0.4643 0.9306 0.052 Uiso 1 1 calc R . .
C17 C 0.6712(4) 0.6073(3) 1.00990(14) 0.0487(6) Uani 1 1 d . . .
H17A H 0.7423 0.5511 1.0582 0.058 Uiso 1 1 calc R . .
C18 C 0.5385(4) 0.7426(3) 1.01395(15) 0.0485(6) Uani 1 1 d . . .
H18A H 0.5194 0.7801 1.0651 0.058 Uiso 1 1 calc R . .
C19 C 0.4337(4) 0.8226(3) 0.94178(15) 0.0423(5) Uani 1 1 d . . .
H19A H 0.3415 0.9141 0.9438 0.051 Uiso 1 1 calc R . .
C20 C 0.4666(3) 0.7659(2) 0.86660(13) 0.0294(4) Uani 1 1 d . . .
C21 C 0.3653(3) 0.8414(2) 0.78447(13) 0.0287(4) Uani 1 1 d . . .
C22 C 0.2294(3) 0.9804(2) 0.77349(16) 0.0382(5) Uani 1 1 d . . .
H22A H 0.1982 1.0337 0.8186 0.046 Uiso 1 1 calc R . .
C23 C 0.1408(3) 1.0388(2) 0.69423(17) 0.0429(6) Uani 1 1 d . . .
H23A H 0.0468 1.1312 0.6855 0.051 Uiso 1 1 calc R . .
C24 C 0.1936(3) 0.9584(3) 0.62854(16) 0.0411(5) Uani 1 1 d . . .
H24A H 0.1361 0.9961 0.5747 0.049 Uiso 1 1 calc R . .
C25 C 0.3323(3) 0.8217(2) 0.64307(14) 0.0340(5) Uani 1 1 d . . .
H25A H 0.3684 0.7682 0.5982 0.041 Uiso 1 1 calc R . .
H2WA H 1.088(4) 0.841(3) 1.089(2) 0.080(13) Uiso 1 1 d D . .
H2WB H 0.995(5) 0.744(3) 1.1181(16) 0.106(15) Uiso 1 1 d D . .
H1WA H 0.624(3) 0.341(3) 0.7363(11) 0.055(8) Uiso 1 1 d D . .
H1WB H 0.4650(19) 0.362(3) 0.7866(15) 0.049(8) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.9115(13) . ?
Cu1 O4 1.9904(13) 2_766 ?
Cu1 N2 1.9929(16) . ?
Cu1 N1 2.0089(16) . ?
Cu1 O1W 2.2187(15) . ?
O1 C13 1.229(2) . ?
O2 C13 1.279(2) . ?
O3 C14 1.242(2) . ?
O4 C14 1.256(2) . ?
O4 Cu1 1.9904(13) 2_766 ?
O5 C15 1.309(3) . ?
O5 H5O 0.851(10) . ?
O6 C15 1.208(3) . ?
O1W H1WA 0.848(9) . ?
O1W H1WB 0.851(9) . ?
O2W H2WA 0.838(10) . ?
O2W H2WB 0.834(10) . ?
N1 C25 1.341(3) . ?
N1 C21 1.343(3) . ?
N2 C16 1.337(3) . ?
N2 C20 1.347(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.386(3) . ?
C1 C13 1.506(2) . ?
C2 C3 1.377(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.399(3) . ?
C4 C14 1.510(2) . ?
C5 C6 1.395(3) . ?
C5 C7 1.489(2) . ?
C6 H6A 0.9300 . ?
C7 C8 1.391(3) . ?
C7 C12 1.394(3) . ?
C8 C9 1.396(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.383(3) . ?
C9 C15 1.486(3) . ?
C10 C11 1.376(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.385(3) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C16 C17 1.370(3) . ?
C16 H16A 0.9300 . ?
C17 C18 1.368(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.375(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.375(3) . ?
C19 H19A 0.9300 . ?
C20 C21 1.480(3) . ?
C21 C22 1.383(3) . ?
C22 C23 1.383(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.374(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.376(3) . ?
C24 H24A 0.9300 . ?
C25 H25A 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
O2 Cu1 O4 97.21(6) . 2_766 ?
O2 Cu1 N2 168.38(6) . . ?
O4 Cu1 N2 89.50(6) 2_766 . ?
O2 Cu1 N1 89.64(6) . . ?
O4 Cu1 N1 153.60(6) 2_766 . ?
N2 Cu1 N1 80.27(7) . . ?
O2 Cu1 O1W 93.21(6) . . ?
O4 Cu1 O1W 85.29(6) 2_766 . ?
N2 Cu1 O1W 96.79(7) . . ?
N1 Cu1 O1W 119.89(6) . . ?
C13 O2 Cu1 128.47(12) . . ?
C14 O4 Cu1 144.08(13) . 2_766 ?
C15 O5 H5O 109(3) . . ?
Cu1 O1W H1WA 89.4(18) . . ?
Cu1 O1W H1WB 125.5(18) . . ?
H1WA O1W H1WB 108.7(15) . . ?
H2WA O2W H2WB 112.9(17) . . ?
C25 N1 C21 118.86(18) . . ?
C25 N1 Cu1 125.63(15) . . ?
C21 N1 Cu1 115.27(13) . . ?
C16 N2 C20 118.42(18) . . ?
C16 N2 Cu1 125.64(15) . . ?
C20 N2 Cu1 115.89(13) . . ?
C2 C1 C6 118.73(17) . . ?
C2 C1 C13 120.60(17) . . ?
C6 C1 C13 120.65(16) . . ?
C3 C2 C1 120.06(17) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 121.21(17) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 C5 119.54(16) . . ?
C3 C4 C14 114.38(16) . . ?
C5 C4 C14 126.08(16) . . ?
C6 C5 C4 118.03(16) . . ?
C6 C5 C7 118.41(16) . . ?
C4 C5 C7 123.51(16) . . ?
C1 C6 C5 122.33(17) . . ?
C1 C6 H6A 118.8 . . ?
C5 C6 H6A 118.8 . . ?
C8 C7 C12 118.26(18) . . ?
C8 C7 C5 121.72(17) . . ?
C12 C7 C5 119.90(17) . . ?
C7 C8 C9 120.63(19) . . ?
C7 C8 H8A 119.7 . . ?
C9 C8 H8A 119.7 . . ?
C10 C9 C8 120.0(2) . . ?
C10 C9 C15 118.61(19) . . ?
C8 C9 C15 121.3(2) . . ?
C11 C10 C9 119.79(19) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 120.3(2) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C11 C12 C7 120.9(2) . . ?
C11 C12 H12A 119.5 . . ?
C7 C12 H12A 119.5 . . ?
O1 C13 O2 126.07(17) . . ?
O1 C13 C1 120.42(17) . . ?
O2 C13 C1 113.50(16) . . ?
O3 C14 O4 121.98(17) . . ?
O3 C14 C4 116.72(16) . . ?
O4 C14 C4 121.18(16) . . ?
O6 C15 O5 122.8(2) . . ?
O6 C15 C9 122.6(2) . . ?
O5 C15 C9 114.63(19) . . ?
N2 C16 C17 122.8(2) . . ?
N2 C16 H16A 118.6 . . ?
C17 C16 H16A 118.6 . . ?
C18 C17 C16 118.7(2) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C17 C18 C19 119.4(2) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
C20 C19 C18 119.3(2) . . ?
C20 C19 H19A 120.4 . . ?
C18 C19 H19A 120.4 . . ?
N2 C20 C19 121.44(19) . . ?
N2 C20 C21 113.95(17) . . ?
C19 C20 C21 124.61(19) . . ?
N1 C21 C22 121.95(19) . . ?
N1 C21 C20 114.26(17) . . ?
C22 C21 C20 123.79(19) . . ?
C23 C22 C21 118.8(2) . . ?
C23 C22 H22A 120.6 . . ?
C21 C22 H22A 120.6 . . ?
C24 C23 C22 119.0(2) . . ?
C24 C23 H23A 120.5 . . ?
C22 C23 H23A 120.5 . . ?
C23 C24 C25 119.4(2) . . ?
C23 C24 H24A 120.3 . . ?
C25 C24 H24A 120.3 . . ?
N1 C25 C24 121.9(2) . . ?
N1 C25 H25A 119.0 . . ?
C24 C25 H25A 119.0 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 996436'
#######################################################################
#
#                 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_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H26 N3 Ni O9'
_chemical_formula_weight         631.25

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'
O O 0.0106 0.0060 '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'
Ni Ni 0.3393 1.1124 '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                   9.5251(6)
_cell_length_b                   9.8837(6)
_cell_length_c                   16.3942(11)
_cell_angle_alpha                72.834(4)
_cell_angle_beta                 87.431(4)
_cell_angle_gamma                71.093(4)
_cell_volume                     1392.88(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             654
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9145
_exptl_absorpt_correction_T_max  0.9349
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'

_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 Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22494
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6329
_reflns_number_gt                4924
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1996)'
_computing_cell_refinement       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of 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.

 The hydrogen atoms of the water and carboxylate group were located from 
 difference maps and refined with isotropic temperature factors.
 To restrains the bond length and bond angles, 
 the instrucitons are used as follows:
 DFIX 0.85 0.01 O5 H5O
 DFIX 0.85 0.01 O1W H1WA O1W H1WB O2W H2WA O2W H2WB O3W H3WA O3W H3WB
 DFIX 1.39 0.01 H1WA H1WB H2WA H2WB H3WA H3WB 
;

_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)+(0.0511P)²+0.4020P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6329
_refine_ls_number_parameters     408
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1062
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003

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
Ni1 Ni 0.36970(3) 0.31396(3) 1.321319(18) 0.02647(10) Uani 1 1 d . . .
O1 O 0.2120(2) 0.5235(2) 1.45130(10) 0.0467(5) Uani 1 1 d . . .
O2 O 0.21274(17) 0.51666(17) 1.31725(10) 0.0314(4) Uani 1 1 d . . .
O3 O -0.45537(17) 1.12293(17) 1.32429(10) 0.0342(4) Uani 1 1 d . . .
O4 O -0.35890(19) 1.20049(18) 1.19949(11) 0.0429(4) Uani 1 1 d . . .
O5 O 0.3701(3) 0.8503(3) 0.95050(15) 0.0757(7) Uani 1 1 d D . .
H5O H 0.354(5) 0.830(5) 0.9055(16) 0.095(14) Uiso 1 1 d D . .
O6 O 0.1362(2) 0.8548(2) 0.96580(12) 0.0561(5) Uani 1 1 d . . .
N1 N 0.2751(2) 0.3339(2) 1.20367(12) 0.0319(4) Uani 1 1 d . . .
N2 N 0.1699(3) 0.4571(3) 0.76013(15) 0.0495(6) Uani 1 1 d . . .
N3 N 0.2405(2) 0.1910(2) 1.38748(12) 0.0297(4) Uani 1 1 d . . .
C1 C 0.0365(2) 0.7210(2) 1.34896(14) 0.0262(4) Uani 1 1 d . . .
C2 C -0.0911(3) 0.7287(3) 1.39441(14) 0.0311(5) Uani 1 1 d . . .
H2A H -0.0907 0.6498 1.4425 0.037 Uiso 1 1 calc R . .
C3 C -0.2185(2) 0.8510(2) 1.36957(15) 0.0312(5) Uani 1 1 d . . .
H3A H -0.3034 0.8535 1.4002 0.037 Uiso 1 1 calc R . .
C4 C -0.2197(2) 0.9709(2) 1.29853(14) 0.0285(5) Uani 1 1 d . . .
C5 C -0.0920(2) 0.9639(2) 1.25353(15) 0.0301(5) Uani 1 1 d . . .
H5A H -0.0923 1.0442 1.2064 0.036 Uiso 1 1 calc R . .
C6 C 0.0361(2) 0.8407(2) 1.27675(14) 0.0268(5) Uani 1 1 d . . .
C7 C 0.1678(2) 0.8369(2) 1.22372(15) 0.0295(5) Uani 1 1 d . . .
C8 C 0.3065(3) 0.8151(3) 1.25815(17) 0.0372(6) Uani 1 1 d . . .
H8A H 0.3189 0.8033 1.3161 0.045 Uiso 1 1 calc R . .
C9 C 0.4270(3) 0.8107(3) 1.20700(19) 0.0456(7) Uani 1 1 d . . .
H9A H 0.5189 0.7983 1.2307 0.055 Uiso 1 1 calc R . .
C10 C 0.4120(3) 0.8245(3) 1.12164(18) 0.0441(6) Uani 1 1 d . . .
H10A H 0.4938 0.8191 1.0881 0.053 Uiso 1 1 calc R . .
C11 C 0.2736(3) 0.8467(3) 1.08578(16) 0.0362(5) Uani 1 1 d . . .
C12 C 0.1528(3) 0.8552(2) 1.13683(15) 0.0337(5) Uani 1 1 d . . .
H12A H 0.0597 0.8736 1.1124 0.040 Uiso 1 1 calc R . .
C13 C 0.1655(2) 0.5766(2) 1.37497(14) 0.0279(5) Uani 1 1 d . . .
C14 C -0.3548(3) 1.1074(2) 1.27176(15) 0.0304(5) Uani 1 1 d . . .
C15 C 0.2515(3) 0.8519(3) 0.99536(17) 0.0432(6) Uani 1 1 d . . .
C16 C 0.1835(3) 0.5426(3) 0.88051(16) 0.0431(6) Uani 1 1 d . . .
H16A H 0.1854 0.6211 0.9003 0.052 Uiso 1 1 calc R . .
C17 C 0.1713(3) 0.5628(3) 0.79434(17) 0.0491(7) Uani 1 1 d . . .
H17A H 0.1635 0.6569 0.7574 0.059 Uiso 1 1 calc R . .
C18 C 0.1759(3) 0.3262(4) 0.81544(18) 0.0488(7) Uani 1 1 d . . .
H18A H 0.1730 0.2504 0.7935 0.059 Uiso 1 1 calc R . .
C19 C 0.1863(3) 0.2951(3) 0.90283(17) 0.0420(6) Uani 1 1 d . . .
H19A H 0.1887 0.2014 0.9382 0.050 Uiso 1 1 calc R . .
C20 C 0.1930(3) 0.4050(3) 0.93768(15) 0.0340(5) Uani 1 1 d . . .
C21 C 0.2130(3) 0.3779(3) 1.03068(15) 0.0324(5) Uani 1 1 d . . .
C22 C 0.1798(3) 0.4966(3) 1.06496(16) 0.0402(6) Uani 1 1 d . . .
H22A H 0.1355 0.5941 1.0302 0.048 Uiso 1 1 calc R . .
C23 C 0.2121(3) 0.4702(3) 1.14971(16) 0.0394(6) Uani 1 1 d . . .
H23A H 0.1889 0.5519 1.1710 0.047 Uiso 1 1 calc R . .
C24 C 0.2981(3) 0.2193(3) 1.17218(17) 0.0431(6) Uani 1 1 d . . .
H24A H 0.3359 0.1227 1.2093 0.052 Uiso 1 1 calc R . .
C25 C 0.2689(3) 0.2360(3) 1.08820(17) 0.0438(6) Uani 1 1 d . . .
H25A H 0.2867 0.1519 1.0696 0.053 Uiso 1 1 calc R . .
C26 C 0.0936(3) 0.2543(3) 1.38139(17) 0.0424(6) Uani 1 1 d . . .
H26A H 0.0539 0.3525 1.3467 0.051 Uiso 1 1 calc R . .
C27 C -0.0023(3) 0.1838(3) 1.42304(17) 0.0434(6) Uani 1 1 d . . .
H27A H -0.1042 0.2339 1.4157 0.052 Uiso 1 1 calc R . .
C28 C 0.0511(2) 0.0385(3) 1.47598(14) 0.0307(5) Uani 1 1 d . . .
C29 C 0.2037(3) -0.0281(3) 1.48173(18) 0.0432(6) Uani 1 1 d . . .
H29A H 0.2461 -0.1265 1.5157 0.052 Uiso 1 1 calc R . .
C30 C 0.2931(3) 0.0500(3) 1.43763(16) 0.0389(6) Uani 1 1 d . . .
H30A H 0.3954 0.0022 1.4430 0.047 Uiso 1 1 calc R . .
O1W O 0.4647(2) 0.3108(2) 1.43477(12) 0.0426(4) Uani 1 1 d D . .
H1WA H 0.529(2) 0.355(3) 1.420(2) 0.062(10) Uiso 1 1 d D . .
H1WB H 0.391(2) 0.366(3) 1.454(2) 0.081(12) Uiso 1 1 d D . .
O2W O 0.49720(19) 0.44004(19) 1.25068(12) 0.0436(4) Uani 1 1 d D . .
H2WA H 0.5544 0.3864 1.2227 0.052 Uiso 1 1 d RD . .
H2WB H 0.5477 0.4602 1.2842 0.052 Uiso 1 1 d RD . .
O3W O 0.6721(3) 0.4681(3) 0.39921(17) 0.0716(7) Uani 1 1 d D . .
H3WA H 0.717(3) 0.463(4) 0.4443(11) 0.080(12) Uiso 1 1 d D . .
H3WB H 0.721(4) 0.495(5) 0.3563(12) 0.095(15) Uiso 1 1 d 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
Ni1 N3 2.0596(18) . ?
Ni1 O2 2.0597(15) . ?
Ni1 O3 2.0634(15) 1_645 ?
Ni1 O2W 2.0908(17) . ?
Ni1 O1W 2.0921(18) . ?
Ni1 N1 2.0943(19) . ?
O1 C13 1.244(3) . ?
O2 C13 1.253(3) . ?
O3 C14 1.262(3) . ?
O3 Ni1 2.0635(15) 1_465 ?
O4 C14 1.261(3) . ?
O5 C15 1.318(3) . ?
O6 C15 1.209(3) . ?
N1 C24 1.332(3) . ?
N1 C23 1.333(3) . ?
N2 C17 1.327(4) . ?
N2 C18 1.328(4) . ?
N3 C26 1.329(3) . ?
N3 C30 1.333(3) . ?
C1 C2 1.390(3) . ?
C1 C6 1.405(3) . ?
C1 C13 1.510(3) . ?
C2 C3 1.380(3) . ?
C3 C4 1.392(3) . ?
C4 C5 1.387(3) . ?
C4 C14 1.498(3) . ?
C5 C6 1.386(3) . ?
C6 C7 1.490(3) . ?
C7 C8 1.386(3) . ?
C7 C12 1.390(3) . ?
C8 C9 1.388(3) . ?
C9 C10 1.375(4) . ?
C10 C11 1.392(4) . ?
C11 C12 1.386(3) . ?
C11 C15 1.490(4) . ?
C16 C17 1.372(4) . ?
C16 C20 1.383(3) . ?
C18 C19 1.375(4) . ?
C19 C20 1.388(3) . ?
C20 C21 1.478(3) . ?
C21 C22 1.387(3) . ?
C21 C25 1.386(3) . ?
C22 C23 1.366(3) . ?
C24 C25 1.368(4) . ?
C26 C27 1.365(3) . ?
C27 C28 1.380(3) . ?
C28 C29 1.383(3) . ?
C28 C28 1.485(4) 2_558 ?
C29 C30 1.372(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 O2 93.80(7) . . ?
N3 Ni1 O3 92.02(7) . 1_645 ?
O2 Ni1 O3 173.53(6) . 1_645 ?
N3 Ni1 O2W 178.23(7) . . ?
O2 Ni1 O2W 85.91(7) . . ?
O3 Ni1 O2W 88.36(7) 1_645 . ?
N3 Ni1 O1W 91.84(8) . . ?
O2 Ni1 O1W 89.52(7) . . ?
O3 Ni1 O1W 87.47(7) 1_645 . ?
O2W Ni1 O1W 89.90(8) . . ?
N3 Ni1 N1 91.71(7) . . ?
O2 Ni1 N1 87.64(7) . . ?
O3 Ni1 N1 95.02(7) 1_645 . ?
O2W Ni1 N1 86.53(7) . . ?
O1W Ni1 N1 175.59(7) . . ?
C13 O2 Ni1 131.31(14) . . ?
C14 O3 Ni1 127.67(14) . 1_465 ?
C24 N1 C23 116.4(2) . . ?
C24 N1 Ni1 123.44(16) . . ?
C23 N1 Ni1 118.92(16) . . ?
C17 N2 C18 115.6(2) . . ?
C26 N3 C30 116.2(2) . . ?
C26 N3 Ni1 119.01(15) . . ?
C30 N3 Ni1 124.75(15) . . ?
C2 C1 C6 119.3(2) . . ?
C2 C1 C13 117.82(19) . . ?
C6 C1 C13 122.61(19) . . ?
C3 C2 C1 121.3(2) . . ?
C2 C3 C4 119.8(2) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 C14 120.1(2) . . ?
C3 C4 C14 121.0(2) . . ?
C4 C5 C6 122.0(2) . . ?
C5 C6 C1 118.6(2) . . ?
C5 C6 C7 119.51(19) . . ?
C1 C6 C7 121.83(19) . . ?
C8 C7 C12 118.2(2) . . ?
C8 C7 C6 122.2(2) . . ?
C12 C7 C6 119.6(2) . . ?
C7 C8 C9 120.6(2) . . ?
C10 C9 C8 120.7(2) . . ?
C9 C10 C11 119.6(2) . . ?
C12 C11 C10 119.3(2) . . ?
C12 C11 C15 118.2(2) . . ?
C10 C11 C15 122.4(2) . . ?
C11 C12 C7 121.5(2) . . ?
O1 C13 O2 125.3(2) . . ?
O1 C13 C1 118.5(2) . . ?
O2 C13 C1 116.07(19) . . ?
O4 C14 O3 124.4(2) . . ?
O4 C14 C4 118.1(2) . . ?
O3 C14 C4 117.5(2) . . ?
O6 C15 O5 122.7(3) . . ?
O6 C15 C11 123.3(2) . . ?
O5 C15 C11 114.0(3) . . ?
C17 C16 C20 119.6(3) . . ?
N2 C17 C16 124.5(3) . . ?
N2 C18 C19 124.5(3) . . ?
C18 C19 C20 119.3(3) . . ?
C16 C20 C19 116.5(2) . . ?
C16 C20 C21 120.8(2) . . ?
C19 C20 C21 122.7(2) . . ?
C22 C21 C25 116.0(2) . . ?
C22 C21 C20 120.8(2) . . ?
C25 C21 C20 123.2(2) . . ?
C23 C22 C21 120.0(2) . . ?
N1 C23 C22 123.6(2) . . ?
N1 C24 C25 123.5(2) . . ?
C24 C25 C21 120.1(2) . . ?
N3 C26 C27 123.9(2) . . ?
C26 C27 C28 120.3(2) . . ?
C27 C28 C29 115.9(2) . . ?
C27 C28 C28 121.2(3) . 2_558 ?
C29 C28 C28 123.0(3) . 2_558 ?
C30 C29 C28 120.5(2) . . ?
N3 C30 C29 123.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 996437'
#######################################################################
#
#                 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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H42 Mn3 N6 O14'
_chemical_formula_weight         1235.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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/n

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

_cell_length_a                   9.3553(2)
_cell_length_b                   24.7637(4)
_cell_length_c                   11.6174(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4110(10)
_cell_angle_gamma                90.00
_cell_volume                     2469.86(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1262
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'

_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 Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39660
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.60
_reflns_number_total             5717
_reflns_number_gt                4463
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1996)'
_computing_cell_refinement       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of 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)+(0.0406P)²+0.8956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5717
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0881
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Mn1 Mn 0.18429(4) 0.185777(12) 0.14440(2) 0.02322(9) Uani 1 1 d . . .
Mn2 Mn 0.0000 0.0000 0.0000 0.01983(10) Uani 1 2 d S . .
N1 N 0.1876(2) 0.18419(7) 0.34074(14) 0.0274(4) Uani 1 1 d . . .
N2 N 0.1941(2) 0.18392(7) 0.95198(15) 0.0284(4) Uani 1 1 d . . .
N3 N -0.0015(2) 0.00725(7) -0.19527(14) 0.0266(4) Uani 1 1 d . . .
O1 O 0.26504(16) 0.10310(5) 0.18073(12) 0.0285(3) Uani 1 1 d . . .
O2 O 0.23247(16) 0.03130(5) 0.05698(12) 0.0276(3) Uani 1 1 d . . .
O3 O 0.6167(2) 0.18263(7) -0.53277(14) 0.0495(5) Uani 1 1 d . . .
O4 O 0.6438(2) 0.22909(6) -0.36118(14) 0.0425(4) Uani 1 1 d . . .
O5 O 0.90483(16) 0.08251(5) -0.01781(12) 0.0270(3) Uani 1 1 d . . .
O6 O 0.94139(16) 0.16331(6) 0.07413(13) 0.0293(3) Uani 1 1 d . . .
O1W O 0.4320(2) 0.21810(8) 0.23615(16) 0.0383(4) Uani 1 1 d . . .
C1 C 0.4458(2) 0.08849(7) 0.08739(17) 0.0220(4) Uani 1 1 d . . .
C2 C 0.4491(2) 0.07982(7) -0.02973(17) 0.0234(4) Uani 1 1 d . . .
H2A H 0.3640 0.0635 -0.0921 0.028 Uiso 1 1 calc R . .
C3 C 0.5764(2) 0.09490(7) -0.05646(17) 0.0228(4) Uani 1 1 d . . .
C4 C 0.7068(2) 0.11651(7) 0.04039(17) 0.0224(4) Uani 1 1 d . . .
C5 C 0.7008(2) 0.12717(8) 0.15601(17) 0.0257(4) Uani 1 1 d . . .
H5A H 0.7852 0.1438 0.2186 0.031 Uiso 1 1 calc R . .
C6 C 0.5715(2) 0.11355(8) 0.17966(17) 0.0261(4) Uani 1 1 d . . .
H6A H 0.5691 0.1212 0.2572 0.031 Uiso 1 1 calc R . .
C7 C 0.5619(2) 0.09201(8) -0.18833(17) 0.0240(4) Uani 1 1 d . . .
C8 C 0.4982(2) 0.04726(8) -0.26353(19) 0.0300(5) Uani 1 1 d . . .
H8A H 0.4710 0.0170 -0.2293 0.036 Uiso 1 1 calc R . .
C9 C 0.4750(3) 0.04736(9) -0.38880(19) 0.0348(5) Uani 1 1 d . . .
H9A H 0.4324 0.0171 -0.4379 0.042 Uiso 1 1 calc R . .
C10 C 0.5144(3) 0.09197(9) -0.44214(18) 0.0317(5) Uani 1 1 d . . .
H10A H 0.4982 0.0916 -0.5265 0.038 Uiso 1 1 calc R . .
C11 C 0.5778(2) 0.13698(8) -0.36927(17) 0.0261(4) Uani 1 1 d . . .
C12 C 0.6006(2) 0.13640(8) -0.24343(17) 0.0258(4) Uani 1 1 d . . .
H12A H 0.6432 0.1667 -0.1945 0.031 Uiso 1 1 calc R . .
C13 C 0.3026(2) 0.07305(8) 0.11011(16) 0.0217(4) Uani 1 1 d . . .
C14 C 0.6159(3) 0.18698(8) -0.42651(18) 0.0304(5) Uani 1 1 d . . .
C15 C 0.8629(2) 0.12138(7) 0.03011(16) 0.0212(4) Uani 1 1 d . . .
C16 C 0.1367(3) 0.14190(9) 0.38437(19) 0.0343(5) Uani 1 1 d . . .
H16A H 0.1000 0.1120 0.3324 0.041 Uiso 1 1 calc R . .
C17 C 0.2424(3) 0.22586(8) 0.41895(18) 0.0303(5) Uani 1 1 d . . .
H17A H 0.2803 0.2555 0.3909 0.036 Uiso 1 1 calc R . .
C18 C 0.2461(3) 0.22758(8) 0.53856(18) 0.0297(5) Uani 1 1 d . . .
H18A H 0.2852 0.2577 0.5891 0.036 Uiso 1 1 calc R . .
C19 C 0.1905(2) 0.18362(8) 0.58255(17) 0.0262(4) Uani 1 1 d . . .
C20 C 0.1357(3) 0.14015(8) 0.50216(19) 0.0352(5) Uani 1 1 d . . .
H20A H 0.0980 0.1097 0.5279 0.042 Uiso 1 1 calc R . .
C21 C 0.1935(3) 0.18364(8) 0.71094(17) 0.0277(4) Uani 1 1 d . . .
C22 C 0.3038(3) 0.21230(9) 0.80788(18) 0.0320(5) Uani 1 1 d . . .
H22A H 0.3803 0.2320 0.7941 0.038 Uiso 1 1 calc R . .
C23 C 0.2995(3) 0.21146(9) 0.92529(18) 0.0330(5) Uani 1 1 d . . .
H23A H 0.3741 0.2312 0.9892 0.040 Uiso 1 1 calc R . .
C24 C 0.0889(3) 0.15584(9) 0.85863(19) 0.0350(5) Uani 1 1 d . . .
H24A H 0.0151 0.1360 0.8756 0.042 Uiso 1 1 calc R . .
C25 C 0.0838(3) 0.15476(9) 0.73870(19) 0.0350(5) Uani 1 1 d . . .
H25A H 0.0074 0.1348 0.6766 0.042 Uiso 1 1 calc R . .
C26 C -0.1212(3) 0.02509(10) -0.29521(19) 0.0375(5) Uani 1 1 d . . .
H26A H -0.2075 0.0388 -0.2841 0.045 Uiso 1 1 calc R . .
C27 C -0.1237(3) 0.02427(10) -0.41483(19) 0.0355(5) Uani 1 1 d . . .
H27A H -0.2085 0.0386 -0.4814 0.043 Uiso 1 1 calc R . .
C28 C 0.0001(2) 0.00216(8) -0.43597(16) 0.0245(4) Uani 1 1 d . . .
C29 C 0.1258(2) -0.01491(9) -0.33097(17) 0.0292(4) Uani 1 1 d . . .
H29A H 0.2133 -0.0292 -0.3392 0.035 Uiso 1 1 calc R . .
C30 C 0.1217(3) -0.01084(8) -0.21398(18) 0.0279(4) Uani 1 1 d . . .
H30A H 0.2094 -0.0213 -0.1445 0.033 Uiso 1 1 calc R . .
H1WA H 0.503(4) 0.2090(15) 0.315(3) 0.097(12) Uiso 1 1 d . . .
H1WB H 0.429(4) 0.2512(15) 0.240(3) 0.086(12) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O4 2.1383(15) 4_566 ?
Mn1 O6 2.1600(14) 1_455 ?
Mn1 O1 2.1651(14) . ?
Mn1 N1 2.2691(15) . ?
Mn1 N2 2.2740(15) 1_554 ?
Mn1 O1W 2.2767(17) . ?
Mn2 O2 2.1505(13) . ?
Mn2 O2 2.1505(13) 3 ?
Mn2 O5 2.2055(13) 1_455 ?
Mn2 O5 2.2055(13) 3_655 ?
Mn2 N3 2.2701(14) . ?
Mn2 N3 2.2701(14) 3 ?
N1 C16 1.331(2) . ?
N1 C17 1.335(2) . ?
N2 C23 1.332(3) . ?
N2 C24 1.334(3) . ?
N2 Mn1 2.2740(15) 1_556 ?
N3 C26 1.328(3) . ?
N3 C30 1.332(2) . ?
O1 C13 1.257(2) . ?
O2 C13 1.248(2) . ?
O3 C14 1.242(2) . ?
O4 C14 1.255(2) . ?
O4 Mn1 2.1383(15) 4_665 ?
O5 C15 1.251(2) . ?
O5 Mn2 2.2055(13) 1_655 ?
O6 C15 1.257(2) . ?
O6 Mn1 2.1600(14) 1_655 ?
O1W H1WA 0.92(4) . ?
O1W H1WB 0.82(4) . ?
C1 C6 1.384(3) . ?
C1 C2 1.390(2) . ?
C1 C13 1.514(2) . ?
C2 C3 1.395(2) . ?
C2 H2A 0.9300 . ?
C3 C4 1.397(3) . ?
C3 C7 1.485(2) . ?
C4 C5 1.392(2) . ?
C4 C15 1.516(2) . ?
C5 C6 1.385(3) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.390(3) . ?
C7 C12 1.391(3) . ?
C8 C9 1.383(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.386(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.383(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.391(3) . ?
C11 C14 1.514(3) . ?
C12 H12A 0.9300 . ?
C16 C20 1.373(3) . ?
C16 H16A 0.9300 . ?
C17 C18 1.377(2) . ?
C17 H17A 0.9300 . ?
C18 C19 1.388(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.383(3) . ?
C19 C21 1.481(2) . ?
C20 H20A 0.9300 . ?
C21 C22 1.383(3) . ?
C21 C25 1.390(3) . ?
C22 C23 1.381(3) . ?
C22 H22A 0.9300 . ?
C23 H23A 0.9300 . ?
C24 C25 1.375(3) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.381(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.389(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.382(3) . ?
C28 C28 1.491(3) 3_554 ?
C29 C30 1.379(2) . ?
C29 H29A 0.9300 . ?
C30 H30A 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
O4 Mn1 O6 95.47(6) 4_566 1_455 ?
O4 Mn1 O1 169.15(6) 4_566 . ?
O6 Mn1 O1 93.63(5) 1_455 . ?
O4 Mn1 N1 88.80(6) 4_566 . ?
O6 Mn1 N1 88.14(6) 1_455 . ?
O1 Mn1 N1 85.60(5) . . ?
O4 Mn1 N2 93.79(6) 4_566 1_554 ?
O6 Mn1 N2 94.05(6) 1_455 1_554 ?
O1 Mn1 N2 91.45(5) . 1_554 ?
N1 Mn1 N2 176.43(6) . 1_554 ?
O4 Mn1 O1W 78.62(7) 4_566 . ?
O6 Mn1 O1W 171.77(6) 1_455 . ?
O1 Mn1 O1W 91.71(6) . . ?
N1 Mn1 O1W 86.02(6) . . ?
N2 Mn1 O1W 92.07(6) 1_554 . ?
O2 Mn2 O2 180 . 3 ?
O2 Mn2 O5 90.93(5) . 1_455 ?
O2 Mn2 O5 89.07(5) 3 1_455 ?
O2 Mn2 O5 89.07(5) . 3_655 ?
O2 Mn2 O5 90.93(5) 3 3_655 ?
O5 Mn2 O5 180. 1_455 3_655 ?
O2 Mn2 N3 83.28(5) . . ?
O2 Mn2 N3 96.72(5) 3 . ?
O5 Mn2 N3 89.49(5) 1_455 . ?
O5 Mn2 N3 90.51(5) 3_655 . ?
O2 Mn2 N3 96.72(5) . 3 ?
O2 Mn2 N3 83.28(5) 3 3 ?
O5 Mn2 N3 90.51(5) 1_455 3 ?
O5 Mn2 N3 89.49(5) 3_655 3 ?
N3 Mn2 N3 180 . 3 ?
C16 N1 C17 116.58(16) . . ?
C16 N1 Mn1 122.16(13) . . ?
C17 N1 Mn1 121.26(12) . . ?
C23 N2 C24 116.92(17) . . ?
C23 N2 Mn1 122.75(13) . 1_556 ?
C24 N2 Mn1 120.29(13) . 1_556 ?
C26 N3 C30 116.93(16) . . ?
C26 N3 Mn2 124.60(13) . . ?
C30 N3 Mn2 118.31(13) . . ?
C13 O1 Mn1 126.81(12) . . ?
C13 O2 Mn2 135.98(12) . . ?
C14 O4 Mn1 146.04(13) . 4_665 ?
C15 O5 Mn2 149.06(12) . 1_655 ?
C15 O6 Mn1 136.33(13) . 1_655 ?
Mn1 O1W H1WA 125(2) . . ?
Mn1 O1W H1WB 109(2) . . ?
H1WA O1W H1WB 103(3) . . ?
C6 C1 C2 119.00(17) . . ?
C6 C1 C13 121.11(16) . . ?
C2 C1 C13 119.82(17) . . ?
C1 C2 C3 121.97(18) . . ?
C1 C2 H2A 119.0 . . ?
C3 C2 H2A 119.0 . . ?
C2 C3 C4 118.23(16) . . ?
C2 C3 C7 118.71(17) . . ?
C4 C3 C7 122.81(16) . . ?
C5 C4 C3 119.50(17) . . ?
C5 C4 C15 118.07(17) . . ?
C3 C4 C15 121.85(15) . . ?
C6 C5 C4 121.27(18) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C1 C6 C5 119.74(17) . . ?
C1 C6 H6A 120.1 . . ?
C5 C6 H6A 120.1 . . ?
C8 C7 C12 117.76(17) . . ?
C8 C7 C3 121.83(17) . . ?
C12 C7 C3 120.20(17) . . ?
C9 C8 C7 120.58(18) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C8 C9 C10 120.87(19) . . ?
C8 C9 H9A 119.6 . . ?
C10 C9 H9A 119.6 . . ?
C11 C10 C9 119.62(18) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C10 C11 C12 118.99(18) . . ?
C10 C11 C14 120.61(17) . . ?
C12 C11 C14 120.36(18) . . ?
C7 C12 C11 122.18(18) . . ?
C7 C12 H12A 118.9 . . ?
C11 C12 H12A 118.9 . . ?
O2 C13 O1 125.80(17) . . ?
O2 C13 C1 116.78(15) . . ?
O1 C13 C1 117.42(17) . . ?
O3 C14 O4 126.27(19) . . ?
O3 C14 C11 117.46(19) . . ?
O4 C14 C11 116.27(17) . . ?
O5 C15 O6 125.50(17) . . ?
O5 C15 C4 117.14(16) . . ?
O6 C15 C4 117.32(16) . . ?
N1 C16 C20 123.35(19) . . ?
N1 C16 H16A 118.3 . . ?
C20 C16 H16A 118.3 . . ?
N1 C17 C18 124.04(18) . . ?
N1 C17 H17A 118.0 . . ?
C18 C17 H17A 118.0 . . ?
C17 C18 C19 118.96(18) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 117.03(17) . . ?
C20 C19 C21 122.26(17) . . ?
C18 C19 C21 120.71(17) . . ?
C16 C20 C19 120.03(19) . . ?
C16 C20 H20A 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C22 C21 C25 117.14(17) . . ?
C22 C21 C19 121.95(18) . . ?
C25 C21 C19 120.90(19) . . ?
C23 C22 C21 119.39(19) . . ?
C23 C22 H22A 120.3 . . ?
C21 C22 H22A 120.3 . . ?
N2 C23 C22 123.5(2) . . ?
N2 C23 H23A 118.2 . . ?
C22 C23 H23A 118.2 . . ?
N2 C24 C25 123.42(19) . . ?
N2 C24 H24A 118.3 . . ?
C25 C24 H24A 118.3 . . ?
C24 C25 C21 119.6(2) . . ?
C24 C25 H25A 120.2 . . ?
C21 C25 H25A 120.2 . . ?
N3 C26 C27 123.1(2) . . ?
N3 C26 H26A 118.5 . . ?
C27 C26 H26A 118.5 . . ?
C26 C27 C28 120.1(2) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C29 C28 C27 116.22(16) . . ?
C29 C28 C28 121.5(2) . 3_554 ?
C27 C28 C28 122.3(2) . 3_554 ?
C30 C29 C28 120.01(19) . . ?
C30 C29 H29A 120.0 . . ?
C28 C29 H29A 120.0 . . ?
N3 C30 C29 123.40(19) . . ?
N3 C30 H30A 118.3 . . ?
C29 C30 H30A 118.3 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 996438'
