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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_z
_database_code_depnum_ccdc_archive 'CCDC 1027723'
_audit_update_record             
;
2014-11-24 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H22 Co N6 O9'
_chemical_formula_weight         717.51

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   P2(1)/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                   11.8287(14)
_cell_length_b                   16.996(2)
_cell_length_c                   15.0618(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.133(2)
_cell_angle_gamma                90.00
_cell_volume                     2980.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2231
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.04

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1468
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9263
_exptl_absorpt_correction_T_max  0.9500
_exptl_absorpt_process_details   'SADABS,(Sheldrick, 2001)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14469
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5245
_reflns_number_gt                3659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON

_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)+(0.0807P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5245
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1309
_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
C1 C 0.8632(3) 0.1319(2) 0.4097(3) 0.0325(9) Uani 1 1 d . . .
C2 C 0.7698(3) 0.1832(2) 0.4320(3) 0.0302(9) Uani 1 1 d . . .
C3 C 0.6713(3) 0.1964(2) 0.3691(3) 0.0339(9) Uani 1 1 d . . .
H3 H 0.6627 0.1727 0.3126 0.041 Uiso 1 1 calc R . .
C4 C 0.5848(3) 0.2452(2) 0.3906(3) 0.0362(10) Uani 1 1 d . B .
C5 C 0.6004(3) 0.2828(2) 0.4732(3) 0.0407(11) Uani 1 1 d . . .
H5 H 0.5449 0.3177 0.4861 0.049 Uiso 1 1 calc R . .
C6 C 0.6978(4) 0.2690(2) 0.5369(3) 0.0369(10) Uani 1 1 d . . .
C7 C 0.7824(3) 0.2181(2) 0.5172(3) 0.0351(10) Uani 1 1 d . . .
H7 H 0.8468 0.2073 0.5605 0.042 Uiso 1 1 calc R . .
C8 C 0.7128(4) 0.3121(3) 0.6244(3) 0.0469(11) Uani 1 1 d . . .
C9 C 0.3489(3) 0.2440(2) 0.2038(3) 0.0355(10) Uani 1 1 d . . .
C10 C 0.2729(3) 0.2977(2) 0.2299(3) 0.0334(9) Uani 1 1 d . . .
H10 H 0.2861 0.3180 0.2882 0.040 Uiso 1 1 calc R . .
C11 C 0.1779(3) 0.3209(2) 0.1693(3) 0.0298(9) Uani 1 1 d . . .
C12 C 0.1579(3) 0.2902(2) 0.0823(3) 0.0312(9) Uani 1 1 d . . .
H12 H 0.0954 0.3074 0.0406 0.037 Uiso 1 1 calc R . .
C13 C 0.2322(3) 0.2334(2) 0.0579(3) 0.0344(9) Uani 1 1 d . . .
C14 C 0.3277(4) 0.2102(2) 0.1193(3) 0.0422(11) Uani 1 1 d . . .
H14 H 0.3772 0.1722 0.1037 0.051 Uiso 1 1 calc R . .
C15 C 0.2108(4) 0.1955(3) -0.0327(3) 0.0449(11) Uani 1 1 d . . .
C16 C 0.1009(3) 0.3816(2) 0.2000(3) 0.0328(9) Uani 1 1 d . . .
C17 C 1.0210(3) 0.1136(2) 0.1362(3) 0.0418(11) Uani 1 1 d . . .
H17 H 1.0823 0.1440 0.1645 0.050 Uiso 1 1 calc R . .
C18 C 0.9695(3) 0.1217(3) 0.0497(3) 0.0429(11) Uani 1 1 d . . .
H18 H 0.9875 0.1579 0.0081 0.052 Uiso 1 1 calc R . .
C19 C 0.8887(3) 0.0264(2) 0.1133(3) 0.0359(10) Uani 1 1 d . . .
H19 H 0.8400 -0.0149 0.1214 0.043 Uiso 1 1 calc R . .
C20 C 0.7998(3) 0.0590(2) -0.0453(3) 0.0330(9) Uani 1 1 d . . .
C21 C 0.6929(4) 0.0276(2) -0.0430(3) 0.0436(11) Uani 1 1 d . . .
H21 H 0.6768 0.0063 0.0102 0.052 Uiso 1 1 calc R . .
C22 C 0.6100(4) 0.0278(2) -0.1196(3) 0.0452(11) Uani 1 1 d . . .
H22 H 0.5386 0.0057 -0.1173 0.054 Uiso 1 1 calc R . .
C23 C 0.6299(3) 0.0601(2) -0.2003(3) 0.0370(10) Uani 1 1 d . . .
C24 C 0.7397(4) 0.0881(3) -0.2011(3) 0.0458(11) Uani 1 1 d . . .
H24 H 0.7572 0.1077 -0.2547 0.055 Uiso 1 1 calc R . .
C25 C 0.8240(4) 0.0880(3) -0.1250(3) 0.0431(11) Uani 1 1 d . . .
H25 H 0.8968 0.1074 -0.1278 0.052 Uiso 1 1 calc R . .
C26 C 0.5532(4) 0.1132(3) -0.3531(3) 0.0533(13) Uani 1 1 d . . .
H26 H 0.6160 0.1469 -0.3469 0.064 Uiso 1 1 calc R . .
C27 C 0.4744(4) 0.1137(3) -0.4321(3) 0.0517(13) Uani 1 1 d . . .
H27 H 0.4859 0.1471 -0.4786 0.062 Uiso 1 1 calc R . .
C28 C 0.3800(3) 0.0665(2) -0.4436(3) 0.0324(9) Uani 1 1 d . . .
C29 C 0.3618(3) 0.0189(2) -0.3729(3) 0.0403(10) Uani 1 1 d . . .
H29 H 0.2963 -0.0123 -0.3787 0.048 Uiso 1 1 calc R . .
C30 C 0.4407(3) 0.0179(2) -0.2940(3) 0.0419(11) Uani 1 1 d . . .
H30 H 0.4270 -0.0140 -0.2469 0.050 Uiso 1 1 calc R . .
C31 C 0.5408(4) 0.0632(2) -0.2826(3) 0.0383(10) Uani 1 1 d . . .
C32 C 0.3338(4) 0.0806(3) -0.6092(3) 0.0463(11) Uani 1 1 d . . .
H32 H 0.4072 0.0924 -0.6195 0.056 Uiso 1 1 calc R . .
C33 C 0.2383(3) 0.0747(3) -0.6717(3) 0.0422(11) Uani 1 1 d . . .
H33 H 0.2345 0.0817 -0.7334 0.051 Uiso 1 1 calc R . .
C34 C 0.1893(3) 0.0519(2) -0.5434(3) 0.0319(9) Uani 1 1 d . . .
H34 H 0.1463 0.0402 -0.4991 0.038 Uiso 1 1 calc R . .
Co1 Co 0.98298(4) 0.03956(3) 0.31252(3) 0.02433(17) Uani 1 1 d . . .
N1 N 0.4813(3) 0.2635(2) 0.3304(3) 0.0459(9) Uani 1 1 d . . .
N2 N 0.4529(3) 0.2229(2) 0.2639(3) 0.0464(9) Uani 1 1 d . A .
N3 N 0.9701(3) 0.05378(18) 0.1770(2) 0.0340(8) Uani 1 1 d . . .
N4 N 0.8844(3) 0.06527(19) 0.0353(2) 0.0323(8) Uani 1 1 d . . .
N5 N 0.3033(3) 0.06616(19) -0.5276(2) 0.0325(8) Uani 1 1 d . . .
N6 N 0.1471(3) 0.05679(18) -0.6302(2) 0.0324(8) Uani 1 1 d . . .
O1 O 0.8653(2) 0.12092(16) 0.32483(19) 0.0399(7) Uani 1 1 d . . .
O2 O 0.9330(2) 0.10106(17) 0.4690(2) 0.0464(8) Uani 1 1 d . . .
O3 O 0.7996(3) 0.28430(19) 0.6847(2) 0.0567(9) Uani 1 1 d . . .
H3A H 0.8094 0.3126 0.7295 0.085 Uiso 1 1 calc R . .
O4 O 0.6533(3) 0.3667(2) 0.6384(2) 0.0724(11) Uani 1 1 d . . .
O5 O 0.4806(7) 0.1496(5) 0.2475(6) 0.174(3) Uiso 0.80 1 d P A 1
O5A O 0.434(3) 0.318(2) 0.374(2) 0.177(13) Uiso 0.20 1 d P B 2
O6 O 0.2721(3) 0.1445(2) -0.0541(2) 0.0740(11) Uani 1 1 d . . .
O7 O 0.1176(3) 0.22128(18) -0.0871(2) 0.0520(8) Uani 1 1 d . . .
H7A H 0.1018 0.1914 -0.1303 0.078 Uiso 1 1 calc R . .
O8 O 0.0822(2) 0.44230(15) 0.15109(18) 0.0377(7) Uani 1 1 d . . .
O9 O 0.0642(3) 0.37127(17) 0.2711(2) 0.0537(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
C1 O2 1.223(4) . ?
C1 O1 1.296(5) . ?
C1 C2 1.492(5) . ?
C2 C3 1.385(5) . ?
C2 C7 1.397(5) . ?
C3 C4 1.400(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(6) . ?
C4 N1 1.424(5) . ?
C5 C6 1.384(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.394(5) . ?
C6 C8 1.491(6) . ?
C7 H7 0.9300 . ?
C8 O4 1.206(5) . ?
C8 O3 1.332(5) . ?
C9 C14 1.378(6) . ?
C9 C10 1.385(5) . ?
C9 N2 1.440(5) . ?
C10 C11 1.375(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.391(5) . ?
C11 C16 1.502(5) . ?
C12 C13 1.397(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.386(6) . ?
C13 C15 1.489(6) . ?
C14 H14 0.9300 . ?
C15 O6 1.209(5) . ?
C15 O7 1.327(5) . ?
C16 O9 1.236(5) . ?
C16 O8 1.265(4) . ?
C17 C18 1.345(5) . ?
C17 N3 1.380(5) . ?
C17 H17 0.9300 . ?
C18 N4 1.379(5) . ?
C18 H18 0.9300 . ?
C19 N3 1.319(5) . ?
C19 N4 1.340(5) . ?
C19 H19 0.9300 . ?
C20 C25 1.374(6) . ?
C20 C21 1.379(6) . ?
C20 N4 1.435(5) . ?
C21 C22 1.376(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(6) . ?
C23 C31 1.480(5) . ?
C24 C25 1.380(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.376(6) . ?
C26 C31 1.387(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.361(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.385(6) . ?
C28 N5 1.421(5) . ?
C29 C30 1.376(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.398(6) . ?
C30 H30 0.9300 . ?
C32 C33 1.342(6) . ?
C32 N5 1.362(5) . ?
C32 H32 0.9300 . ?
C33 N6 1.373(5) . ?
C33 H33 0.9300 . ?
C34 N6 1.316(5) . ?
C34 N5 1.350(5) . ?
C34 H34 0.9300 . ?
Co1 O8 1.943(3) 2_645 ?
Co1 O1 1.993(3) . ?
Co1 N6 2.003(3) 1_656 ?
Co1 N3 2.035(3) . ?
N1 N2 1.213(5) . ?
N1 O5A 1.32(4) . ?
N2 O5 1.322(9) . ?
N6 Co1 2.003(3) 1_454 ?
O3 H3A 0.8200 . ?
O7 H7A 0.8200 . ?
O8 Co1 1.943(3) 2_655 ?

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 C1 O1 122.1(4) . . ?
O2 C1 C2 121.1(4) . . ?
O1 C1 C2 116.8(3) . . ?
C3 C2 C7 120.1(3) . . ?
C3 C2 C1 120.5(4) . . ?
C7 C2 C1 119.5(3) . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 N1 115.9(4) . . ?
C3 C4 N1 124.3(4) . . ?
C4 C5 C6 120.6(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.9(4) . . ?
C5 C6 C8 119.0(4) . . ?
C7 C6 C8 121.0(4) . . ?
C6 C7 C2 119.7(4) . . ?
C6 C7 H7 120.2 . . ?
C2 C7 H7 120.2 . . ?
O4 C8 O3 123.9(4) . . ?
O4 C8 C6 123.4(5) . . ?
O3 C8 C6 112.7(4) . . ?
C14 C9 C10 121.0(4) . . ?
C14 C9 N2 118.2(4) . . ?
C10 C9 N2 120.7(4) . . ?
C11 C10 C9 119.7(4) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 C16 117.5(3) . . ?
C12 C11 C16 122.4(3) . . ?
C11 C12 C13 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 119.8(4) . . ?
C14 C13 C15 118.4(4) . . ?
C12 C13 C15 121.8(4) . . ?
C9 C14 C13 119.5(4) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
O6 C15 O7 122.9(4) . . ?
O6 C15 C13 122.8(4) . . ?
O7 C15 C13 114.3(4) . . ?
O9 C16 O8 124.6(4) . . ?
O9 C16 C11 119.6(4) . . ?
O8 C16 C11 115.7(4) . . ?
C18 C17 N3 110.3(4) . . ?
C18 C17 H17 124.8 . . ?
N3 C17 H17 124.8 . . ?
C17 C18 N4 105.9(4) . . ?
C17 C18 H18 127.0 . . ?
N4 C18 H18 127.0 . . ?
N3 C19 N4 111.9(3) . . ?
N3 C19 H19 124.0 . . ?
N4 C19 H19 124.0 . . ?
C25 C20 C21 119.5(4) . . ?
C25 C20 N4 119.5(4) . . ?
C21 C20 N4 120.9(4) . . ?
C22 C21 C20 120.0(4) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 121.8(4) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C24 C23 C22 116.5(4) . . ?
C24 C23 C31 120.8(4) . . ?
C22 C23 C31 122.7(4) . . ?
C25 C24 C23 122.3(4) . . ?
C25 C24 H24 118.9 . . ?
C23 C24 H24 118.9 . . ?
C20 C25 C24 119.7(4) . . ?
C20 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C27 C26 C31 121.3(4) . . ?
C27 C26 H26 119.4 . . ?
C31 C26 H26 119.4 . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 118.8(4) . . ?
C27 C28 N5 119.8(4) . . ?
C29 C28 N5 121.4(4) . . ?
C30 C29 C28 119.8(4) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 122.1(4) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 H30 119.0 . . ?
C26 C31 C30 116.4(4) . . ?
C26 C31 C23 120.5(4) . . ?
C30 C31 C23 123.1(4) . . ?
C33 C32 N5 107.2(4) . . ?
C33 C32 H32 126.4 . . ?
N5 C32 H32 126.4 . . ?
C32 C33 N6 109.2(4) . . ?
C32 C33 H33 125.4 . . ?
N6 C33 H33 125.4 . . ?
N6 C34 N5 110.9(3) . . ?
N6 C34 H34 124.6 . . ?
N5 C34 H34 124.6 . . ?
O8 Co1 O1 104.22(12) 2_645 . ?
O8 Co1 N6 113.94(12) 2_645 1_656 ?
O1 Co1 N6 119.88(12) . 1_656 ?
O8 Co1 N3 114.87(12) 2_645 . ?
O1 Co1 N3 94.62(12) . . ?
N6 Co1 N3 108.11(13) 1_656 . ?
N2 N1 O5A 137.4(15) . . ?
N2 N1 C4 118.9(4) . . ?
O5A N1 C4 102.9(15) . . ?
N1 N2 O5 130.4(5) . . ?
N1 N2 C9 117.3(3) . . ?
O5 N2 C9 109.2(5) . . ?
C19 N3 C17 104.8(3) . . ?
C19 N3 Co1 127.2(3) . . ?
C17 N3 Co1 124.9(3) . . ?
C19 N4 C18 106.9(3) . . ?
C19 N4 C20 128.2(3) . . ?
C18 N4 C20 124.4(3) . . ?
C34 N5 C32 106.7(3) . . ?
C34 N5 C28 128.3(3) . . ?
C32 N5 C28 125.0(3) . . ?
C34 N6 C33 106.0(3) . . ?
C34 N6 Co1 126.0(3) . 1_454 ?
C33 N6 Co1 128.0(3) . 1_454 ?
C1 O1 Co1 109.1(2) . . ?
C8 O3 H3A 109.5 . . ?
C15 O7 H7A 109.5 . . ?
C16 O8 Co1 124.6(3) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p
_database_code_depnum_ccdc_archive 'CCDC 1027724'
_audit_update_record             
;
2014-11-24 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H42 Mn3 N8 O24'
_chemical_formula_weight         1279.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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                   9.7766(17)
_cell_length_b                   12.204(2)
_cell_length_c                   12.262(2)
_cell_angle_alpha                72.090(3)
_cell_angle_beta                 85.517(3)
_cell_angle_gamma                73.131(3)
_cell_volume                     1332.1(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1672
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      23.03

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             653
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9108
_exptl_absorpt_correction_T_max  0.9392
_exptl_absorpt_process_details   'SADABS,(Sheldrick, 2001)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6592
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4641
_reflns_number_gt                3347
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON

_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 commands DFIX and DANG were
 used to bind the hydrogen atoms from water molecules. The SADI restraints was
 applied to O4 and O8 atoms, to make the bond length of O4-N2 and O8-N2 equal.
;

_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)+(0.0710P)²+2.4585P] 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         4641
_refine_ls_number_parameters     396
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1644
_refine_ls_wR_factor_gt          0.1444
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
C1 C 0.9569(7) 0.3579(5) 1.3403(4) 0.0510(15) Uani 1 1 d . . .
C2 C 0.9138(6) 0.4064(4) 1.2159(4) 0.0374(12) Uani 1 1 d . . .
C3 C 0.9399(5) 0.3302(4) 1.1489(4) 0.0338(11) Uani 1 1 d . . .
H3 H 0.9915 0.2504 1.1801 0.041 Uiso 1 1 calc R . .
C4 C 0.8915(5) 0.3691(4) 1.0367(4) 0.0318(11) Uani 1 1 d . . .
C5 C 0.9205(5) 0.2825(4) 0.9683(4) 0.0310(11) Uani 1 1 d . . .
C6 C 0.8199(6) 0.4895(4) 0.9894(5) 0.0434(13) Uani 1 1 d . . .
H6 H 0.7855 0.5180 0.9143 0.052 Uiso 1 1 calc R . .
C7 C 0.8000(6) 0.5673(4) 1.0561(5) 0.0468(14) Uani 1 1 d . . .
C8 C 0.8465(7) 0.5257(5) 1.1685(5) 0.0480(14) Uani 1 1 d . . .
H8 H 0.8324 0.5785 1.2119 0.058 Uiso 1 1 calc R . .
C9 C 0.5916(5) 0.8666(4) 0.9071(5) 0.0399(13) Uani 1 1 d . A .
C10 C 0.4467(5) 0.9171(4) 0.8870(5) 0.0392(12) Uani 1 1 d . . .
H10 H 0.3845 0.8692 0.9054 0.047 Uiso 1 1 calc R . .
C11 C 0.3952(5) 1.0392(4) 0.8393(4) 0.0319(11) Uani 1 1 d . . .
C12 C 0.4885(5) 1.1098(4) 0.8103(4) 0.0292(10) Uani 1 1 d . . .
H12 H 0.4534 1.1922 0.7770 0.035 Uiso 1 1 calc R . .
C13 C 0.6348(5) 1.0579(4) 0.8309(4) 0.0292(10) Uani 1 1 d . . .
C14 C 0.6861(5) 0.9350(4) 0.8800(4) 0.0349(11) Uani 1 1 d . . .
H14 H 0.7834 0.8991 0.8944 0.042 Uiso 1 1 calc R . .
C15 C 0.7356(5) 1.1340(4) 0.8005(4) 0.0297(10) Uani 1 1 d . . .
C16 C 0.2381(5) 1.0953(5) 0.8225(4) 0.0365(12) Uani 1 1 d . . .
C17 C 0.6259(9) 0.9878(7) 0.5480(8) 0.090(3) Uani 1 1 d . . .
H17 H 0.7117 0.9771 0.5831 0.108 Uiso 1 1 calc R . .
C18 C 0.5767(9) 0.8885(7) 0.5601(8) 0.098(3) Uani 1 1 d . . .
H18 H 0.6322 0.8127 0.6004 0.118 Uiso 1 1 calc R . .
C19 C 0.4483(7) 0.9002(6) 0.5138(6) 0.0615(17) Uani 1 1 d . . .
C20 C 0.3891(8) 0.7982(6) 0.5241(7) 0.077(2) Uani 1 1 d . . .
H20A H 0.2917 0.8176 0.5511 0.092 Uiso 1 1 calc R . .
H20B H 0.3857 0.7892 0.4485 0.092 Uiso 1 1 calc R . .
C21 C 0.4446(8) 0.6364(8) 0.7161(7) 0.084(2) Uani 1 1 d . . .
H21 H 0.3725 0.6729 0.7582 0.101 Uiso 1 1 calc R . .
C22 C 0.5400(9) 0.5311(7) 0.7555(7) 0.086(3) Uani 1 1 d . . .
H22 H 0.5478 0.4798 0.8301 0.103 Uiso 1 1 calc R . .
C23 C 0.5784(8) 0.6025(7) 0.5738(7) 0.085(3) Uani 1 1 d . . .
C24 C 0.6433(12) 0.6181(12) 0.4576(9) 0.178(7) Uani 1 1 d . . .
H24A H 0.7168 0.6573 0.4519 0.267 Uiso 1 1 calc R . .
H24B H 0.5709 0.6661 0.4003 0.267 Uiso 1 1 calc R . .
H24C H 0.6839 0.5410 0.4459 0.267 Uiso 1 1 calc R . .
Mn1 Mn -0.03571(7) 1.22460(6) 0.74348(6) 0.0281(2) Uani 1 1 d . . .
Mn2 Mn 0.0000 1.0000 1.0000 0.0234(3) Uani 1 2 d S . .
N1 N 0.7499(6) 0.6968(5) 1.0072(5) 0.0639(15) Uani 1 1 d . A .
N2 N 0.6424(6) 0.7342(5) 0.9582(6) 0.0681(16) Uani 1 1 d D . .
N3 N 0.4710(5) 0.6822(4) 0.6021(5) 0.0598(14) Uani 1 1 d . . .
N4 N 0.6239(8) 0.5124(5) 0.6666(6) 0.091(2) Uani 1 1 d . . .
O2 O 0.1569(4) 1.0299(4) 0.8700(3) 0.0519(10) Uani 1 1 d . . .
O3 O 0.1916(4) 1.2016(3) 0.7624(4) 0.0513(10) Uani 1 1 d . . .
O4 O 0.5447(11) 0.6733(9) 0.9585(10) 0.119(3) Uiso 0.70 1 d PD A 1
O6 O 0.6990(4) 1.2374(3) 0.7335(3) 0.0443(9) Uani 1 1 d . . .
O7 O 0.8615(3) 1.0866(3) 0.8434(3) 0.0347(8) Uani 1 1 d . . .
O8 O 0.545(3) 0.685(2) 1.037(2) 0.140(9) Uiso 0.30 1 d PD A 2
O9 O 0.9587(6) 0.4288(4) 1.3944(3) 0.0647(13) Uani 1 1 d . . .
O10 O 0.9833(7) 0.2448(4) 1.3834(4) 0.0891(19) Uani 1 1 d . . .
O11 O 0.9650(4) 0.1716(3) 1.0231(3) 0.0404(9) Uani 1 1 d . . .
O12 O 0.8975(4) 0.3242(3) 0.8627(3) 0.0395(8) Uani 1 1 d . . .
O1W O -0.0057(6) 1.1453(4) 0.6077(4) 0.0658(13) Uani 1 1 d D . .
H1WA H -0.012(6) 1.173(4) 0.5367(11) 0.056(19) Uiso 1 1 d D . .
H1WB H 0.024(8) 1.0707(10) 0.625(4) 0.084 Uiso 1 1 d D . .
O2W O -0.0766(4) 1.3958(3) 0.6145(3) 0.0379(8) Uani 1 1 d D . .
H2WA H -0.1636(14) 1.419(5) 0.605(5) 0.057 Uiso 1 1 d D . .
H2WB H -0.043(6) 1.448(4) 0.622(8) 0.12(4) Uiso 1 1 d D . .
O3W O 0.1330(7) 0.9081(5) 0.6901(5) 0.0889(17) Uani 1 1 d D . .
H3WA H 0.056(5) 0.898(9) 0.676(8) 0.133 Uiso 1 1 d D . .
H3WB H 0.125(9) 0.932(8) 0.748(5) 0.133 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
C1 O9 1.246(6) . ?
C1 O10 1.271(7) . ?
C1 C2 1.502(7) . ?
C2 C8 1.369(7) . ?
C2 C3 1.380(7) . ?
C3 C4 1.383(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.388(7) . ?
C4 C5 1.495(7) . ?
C5 O12 1.249(6) . ?
C5 O11 1.272(5) . ?
C6 C7 1.398(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(8) . ?
C7 N1 1.453(7) . ?
C8 H8 0.9300 . ?
C9 C14 1.375(7) . ?
C9 C10 1.379(7) . ?
C9 N2 1.487(7) . ?
C10 C11 1.374(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(6) . ?
C11 C16 1.491(6) . ?
C12 C13 1.394(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.385(6) . ?
C13 C15 1.495(6) . ?
C14 H14 0.9300 . ?
C15 O6 1.241(5) . ?
C15 O7 1.276(5) . ?
C16 O3 1.248(6) . ?
C16 O2 1.271(6) . ?
C17 C19 1.357(9) 2_676 ?
C17 C18 1.392(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.370(10) . ?
C18 H18 0.9300 . ?
C19 C17 1.357(9) 2_676 ?
C19 C20 1.486(10) . ?
C20 N3 1.480(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.322(10) . ?
C21 N3 1.371(9) . ?
C21 H21 0.9300 . ?
C22 N4 1.348(10) . ?
C22 H22 0.9300 . ?
C23 N4 1.314(9) . ?
C23 N3 1.314(8) . ?
C23 C24 1.493(12) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
Mn1 O12 2.127(3) 1_465 ?
Mn1 O1W 2.132(4) . ?
Mn1 O2W 2.147(3) . ?
Mn1 O3 2.179(3) . ?
Mn1 O7 2.206(3) 1_455 ?
Mn2 O11 2.126(3) 1_465 ?
Mn2 O11 2.126(3) 2_667 ?
Mn2 O2 2.147(3) . ?
Mn2 O2 2.147(3) 2_577 ?
Mn2 O7 2.228(3) 2_677 ?
Mn2 O7 2.228(3) 1_455 ?
N1 N2 1.152(7) . ?
N2 O4 1.369(10) . ?
N2 O8 1.429(17) . ?
O7 Mn1 2.206(3) 1_655 ?
O7 Mn2 2.228(3) 1_655 ?
O11 Mn2 2.126(3) 1_645 ?
O12 Mn1 2.127(3) 1_645 ?
O1W H1WA 0.831(10) . ?
O1W H1WB 0.833(10) . ?
O2W H2WA 0.821(10) . ?
O2W H2WB 0.829(10) . ?
O3W H3WA 0.836(10) . ?
O3W H3WB 0.834(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 C1 O10 125.0(5) . . ?
O9 C1 C2 119.4(5) . . ?
O10 C1 C2 115.5(5) . . ?
C8 C2 C3 119.5(5) . . ?
C8 C2 C1 120.5(5) . . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C4 121.9(4) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C6 118.6(5) . . ?
C3 C4 C5 119.8(4) . . ?
C6 C4 C5 121.6(4) . . ?
O12 C5 O11 125.2(5) . . ?
O12 C5 C4 117.8(4) . . ?
O11 C5 C4 117.0(4) . . ?
C4 C6 C7 119.1(5) . . ?
C4 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C8 C7 C6 121.1(5) . . ?
C8 C7 N1 116.1(5) . . ?
C6 C7 N1 122.2(5) . . ?
C2 C8 C7 119.7(5) . . ?
C2 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C14 C9 C10 121.7(4) . . ?
C14 C9 N2 121.0(5) . . ?
C10 C9 N2 117.3(5) . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 120.1(4) . . ?
C10 C11 C16 119.6(4) . . ?
C12 C11 C16 120.3(4) . . ?
C11 C12 C13 120.3(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 119.4(4) . . ?
C14 C13 C15 120.2(4) . . ?
C12 C13 C15 120.4(4) . . ?
C9 C14 C13 119.3(4) . . ?
C9 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
O6 C15 O7 121.9(4) . . ?
O6 C15 C13 121.0(4) . . ?
O7 C15 C13 117.0(4) . . ?
O3 C16 O2 122.8(5) . . ?
O3 C16 C11 119.9(4) . . ?
O2 C16 C11 117.2(5) . . ?
C19 C17 C18 121.6(7) 2_676 . ?
C19 C17 H17 119.2 2_676 . ?
C18 C17 H17 119.2 . . ?
C19 C18 C17 121.4(7) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C17 C19 C18 116.9(7) 2_676 . ?
C17 C19 C20 118.9(7) 2_676 . ?
C18 C19 C20 124.2(6) . . ?
N3 C20 C19 114.5(6) . . ?
N3 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
N3 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C22 C21 N3 107.8(7) . . ?
C22 C21 H21 126.1 . . ?
N3 C21 H21 126.1 . . ?
C21 C22 N4 106.7(7) . . ?
C21 C22 H22 126.7 . . ?
N4 C22 H22 126.7 . . ?
N4 C23 N3 108.2(7) . . ?
N4 C23 C24 126.7(7) . . ?
N3 C23 C24 125.0(8) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O12 Mn1 O1W 169.22(17) 1_465 . ?
O12 Mn1 O2W 85.79(14) 1_465 . ?
O1W Mn1 O2W 87.50(16) . . ?
O12 Mn1 O3 95.11(15) 1_465 . ?
O1W Mn1 O3 93.94(19) . . ?
O2W Mn1 O3 95.62(15) . . ?
O12 Mn1 O7 91.37(13) 1_465 1_455 ?
O1W Mn1 O7 88.90(16) . 1_455 ?
O2W Mn1 O7 142.88(13) . 1_455 ?
O3 Mn1 O7 121.49(13) . 1_455 ?
O11 Mn2 O11 180.000(1) 1_465 2_667 ?
O11 Mn2 O2 92.94(15) 1_465 . ?
O11 Mn2 O2 87.06(15) 2_667 . ?
O11 Mn2 O2 87.06(15) 1_465 2_577 ?
O11 Mn2 O2 92.94(15) 2_667 2_577 ?
O2 Mn2 O2 180.000(1) . 2_577 ?
O11 Mn2 O7 90.98(13) 1_465 2_677 ?
O11 Mn2 O7 89.02(13) 2_667 2_677 ?
O2 Mn2 O7 100.87(13) . 2_677 ?
O2 Mn2 O7 79.13(13) 2_577 2_677 ?
O11 Mn2 O7 89.02(13) 1_465 1_455 ?
O11 Mn2 O7 90.98(13) 2_667 1_455 ?
O2 Mn2 O7 79.13(13) . 1_455 ?
O2 Mn2 O7 100.87(13) 2_577 1_455 ?
O7 Mn2 O7 180.000(1) 2_677 1_455 ?
N2 N1 C7 116.4(6) . . ?
N1 N2 O4 126.9(7) . . ?
N1 N2 O8 104.8(13) . . ?
O4 N2 O8 42.3(11) . . ?
N1 N2 C9 116.5(5) . . ?
O4 N2 C9 115.5(6) . . ?
O8 N2 C9 113.9(12) . . ?
C23 N3 C21 107.7(6) . . ?
C23 N3 C20 126.3(6) . . ?
C21 N3 C20 126.0(6) . . ?
C23 N4 C22 109.6(6) . . ?
C16 O2 Mn2 145.5(4) . . ?
C16 O3 Mn1 103.9(3) . . ?
C15 O7 Mn1 99.5(3) . 1_655 ?
C15 O7 Mn2 148.0(3) . 1_655 ?
Mn1 O7 Mn2 101.80(12) 1_655 1_655 ?
C5 O11 Mn2 140.6(3) . 1_645 ?
C5 O12 Mn1 124.9(3) . 1_645 ?
Mn1 O1W H1WA 134(4) . . ?
Mn1 O1W H1WB 117(4) . . ?
H1WA O1W H1WB 109(3) . . ?
Mn1 O2W H2WA 105(4) . . ?
Mn1 O2W H2WB 120(6) . . ?
H2WA O2W H2WB 113(3) . . ?
H3WA O3W H3WB 110(3) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.088
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p
_database_code_depnum_ccdc_archive 'CCDC 1027725'
_audit_update_record             
;
2014-11-24 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H36 Cd3 N8 O20'
_chemical_formula_weight         1382.05

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.973(2)
_cell_length_b                   10.452(2)
_cell_length_c                   12.671(3)
_cell_angle_alpha                111.595(3)
_cell_angle_beta                 104.229(3)
_cell_angle_gamma                92.999(3)
_cell_volume                     1175.4(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2573
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      27.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_process_details   'SADABS,(Sheldrick, 2001)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5844
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4083
_reflns_number_gt                3410
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON

_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)+(0.0503P)²+0.6115P] 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         4083
_refine_ls_number_parameters     359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 0.5000 0.5000 0.5000 0.01912(12) Uani 1 2 d S . .
Cd2 Cd 0.54407(3) -0.17579(3) -0.26441(3) 0.02206(11) Uani 1 1 d . . .
O1 O 0.6391(3) 0.7190(3) 0.5884(3) 0.0264(7) Uani 1 1 d . . .
O4 O 1.3179(3) 0.6197(4) 0.5127(3) 0.0393(8) Uani 1 1 d . . .
O2 O 0.8206(3) 0.8432(4) 0.7402(3) 0.0424(9) Uani 1 1 d . . .
O3 O 1.3088(3) 0.7834(4) 0.6813(3) 0.0434(9) Uani 1 1 d . . .
O7 O 0.5300(4) 0.4936(3) -0.3218(3) 0.0392(8) Uani 1 1 d . . .
O6 O 0.5825(4) 0.0366(3) -0.1074(3) 0.0445(9) Uani 1 1 d . . .
O5 O 0.5440(5) 0.0451(3) -0.2811(3) 0.0503(10) Uani 1 1 d . . .
O8 O 0.5838(4) 0.6929(3) -0.1621(3) 0.0411(9) Uani 1 1 d . . .
N1 N 0.8290(4) 0.4984(4) 0.2389(3) 0.0270(8) Uani 1 1 d . . .
N2 N 0.7518(4) 0.5555(4) 0.1821(3) 0.0257(8) Uani 1 1 d . A .
C11 C 1.0949(4) 0.6728(4) 0.5315(4) 0.0224(9) Uani 1 1 d . A .
C12 C 0.6581(5) 0.3296(5) 0.0072(4) 0.0275(10) Uani 1 1 d . A .
H12 H 0.6785 0.2793 0.0547 0.033 Uiso 1 1 calc R . .
C13 C 1.0092(4) 0.7280(4) 0.6047(4) 0.0224(9) Uani 1 1 d . . .
H13 H 1.0491 0.7774 0.6856 0.027 Uiso 1 1 calc R . .
C14 C 0.5675(4) 0.5627(5) -0.2126(4) 0.0259(10) Uani 1 1 d . . .
C15 C 0.7716(4) 0.7613(4) 0.6353(4) 0.0245(9) Uani 1 1 d . . .
C16 C 0.5976(5) 0.2619(4) -0.1133(4) 0.0266(10) Uani 1 1 d . . .
C17 C 0.5966(5) 0.4823(4) -0.1336(4) 0.0241(9) Uani 1 1 d . . .
C18 C 0.5681(5) 0.3371(4) -0.1838(4) 0.0280(10) Uani 1 1 d . . .
H18 H 0.5291 0.2904 -0.2652 0.034 Uiso 1 1 calc R . .
C19 C 0.8055(4) 0.6401(4) 0.4346(4) 0.0221(9) Uani 1 1 d . . .
H19 H 0.7097 0.6325 0.4014 0.026 Uiso 1 1 calc R A .
C20 C 1.2526(5) 0.6921(5) 0.5791(4) 0.0268(10) Uani 1 1 d . . .
C21 C 1.0330(5) 0.5953(4) 0.4112(4) 0.0243(9) Uani 1 1 d . . .
H21 H 1.0876 0.5518 0.3627 0.029 Uiso 1 1 calc R A .
C22 C 0.6562(4) 0.5505(4) -0.0119(4) 0.0245(9) Uani 1 1 d . A .
H22 H 0.6743 0.6473 0.0228 0.029 Uiso 1 1 calc R . .
N3 N 0.9487(5) 0.8719(5) 0.1141(4) 0.0480(12) Uani 1 1 d . . .
C24 C 0.8649(4) 0.7091(4) 0.5565(4) 0.0227(9) Uani 1 1 d . A .
C25 C 0.8894(4) 0.5833(4) 0.3638(3) 0.0205(9) Uani 1 1 d . A .
C26 C 0.6883(4) 0.4752(4) 0.0569(4) 0.0228(9) Uani 1 1 d . . .
C27 C 0.5713(5) 0.1042(5) -0.1708(4) 0.0288(10) Uani 1 1 d . . .
N4 N 0.8012(5) 0.9684(5) 0.2035(5) 0.0615(15) Uani 1 1 d . . .
H4 H 0.7593 1.0008 0.2573 0.074 Uiso 1 1 calc R . .
C29 C 0.9180(7) 0.9126(6) 0.2158(5) 0.0534(16) Uani 1 1 d . . .
C30 C 0.9553(6) 0.5688(7) -0.0727(6) 0.0578(16) Uani 1 1 d . . .
H30 H 0.9238 0.6149 -0.1223 0.069 Uiso 1 1 calc R . .
C31 C 1.0315(6) 0.6462(6) 0.0448(6) 0.0537(16) Uani 1 1 d . . .
C32 C 0.8482(7) 0.9054(6) 0.0345(6) 0.0570(16) Uani 1 1 d . . .
H32 H 0.8448 0.8884 -0.0435 0.068 Uiso 1 1 calc R . .
C33 C 1.0647(7) 0.8014(6) 0.0899(7) 0.0688(19) Uani 1 1 d . . .
H33A H 1.1420 0.8346 0.1620 0.083 Uiso 1 1 calc R . .
H33B H 1.0954 0.8258 0.0318 0.083 Uiso 1 1 calc R . .
C34 C 0.7584(7) 0.9661(6) 0.0912(6) 0.0615(18) Uani 1 1 d . . .
H34 H 0.6809 1.0007 0.0604 0.074 Uiso 1 1 calc R . .
C35 C 0.9975(10) 0.9037(8) 0.3273(6) 0.094(3) Uani 1 1 d . . .
H35A H 1.0364 0.8187 0.3096 0.141 Uiso 1 1 calc R . .
H35B H 0.9360 0.9050 0.3751 0.141 Uiso 1 1 calc R . .
H35C H 1.0719 0.9818 0.3697 0.141 Uiso 1 1 calc R . .
C36 C 0.9256(6) 0.4240(6) -0.1176(6) 0.0551(16) Uani 1 1 d . . .
H36 H 0.8766 0.3743 -0.1968 0.066 Uiso 1 1 calc R . .
O9 O 0.8656(11) 0.3762(11) 0.2027(9) 0.076(4) Uiso 0.480(10) 1 d P A 1
O10 O 0.7461(12) 0.6830(12) 0.2187(9) 0.092(4) Uiso 0.520(10) 1 d P A 2
O11 O 0.6782(11) 0.1602(11) -0.4097(9) 0.083(3) Uiso 0.50 1 d PG . .
H11A H 0.5986 0.1397 -0.4006 0.125 Uiso 0.50 1 d PG . .
H11B H 0.7136 0.0857 -0.4353 0.125 Uiso 0.50 1 d PG . .
O12 O 0.7372(11) 0.9672(11) 0.4177(8) 0.080(3) Uiso 0.50 1 d PG . .
H12A H 0.8100 1.0290 0.4595 0.121 Uiso 0.50 1 d PG . .
H12B H 0.6692 0.9885 0.4478 0.121 Uiso 0.50 1 d PG . .


_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 O7 2.230(3) 2_665 ?
Cd1 O7 2.230(3) 1_556 ?
Cd1 O4 2.263(3) 1_455 ?
Cd1 O4 2.263(3) 2_766 ?
Cd1 O1 2.332(3) . ?
Cd1 O1 2.332(3) 2_666 ?
Cd2 O8 2.199(3) 1_545 ?
Cd2 O3 2.247(3) 1_444 ?
Cd2 O1 2.248(3) 1_544 ?
Cd2 O6 2.306(3) . ?
Cd2 O5 2.395(3) . ?
Cd2 C27 2.692(4) . ?
O1 C15 1.285(5) . ?
O1 Cd2 2.248(3) 1_566 ?
O4 C20 1.248(5) . ?
O4 Cd1 2.263(3) 1_655 ?
O2 C15 1.240(5) . ?
O3 C20 1.256(6) . ?
O3 Cd2 2.247(3) 1_666 ?
O7 C14 1.248(5) . ?
O7 Cd1 2.230(3) 1_554 ?
O6 C27 1.241(6) . ?
O5 C27 1.252(6) . ?
O8 C14 1.254(5) . ?
O8 Cd2 2.199(3) 1_565 ?
N1 N2 1.248(5) . ?
N1 O9 1.295(11) . ?
N1 C25 1.448(5) . ?
N2 O10 1.250(11) . ?
N2 C26 1.447(5) . ?
C11 C21 1.391(6) . ?
C11 C13 1.404(6) . ?
C11 C20 1.513(6) . ?
C12 C16 1.380(6) . ?
C12 C26 1.398(6) . ?
C12 H12 0.9300 . ?
C13 C24 1.390(6) . ?
C13 H13 0.9300 . ?
C14 C17 1.514(6) . ?
C15 C24 1.507(6) . ?
C16 C18 1.384(6) . ?
C16 C27 1.514(6) . ?
C17 C22 1.392(6) . ?
C17 C18 1.395(6) . ?
C18 H18 0.9300 . ?
C19 C25 1.374(6) . ?
C19 C24 1.394(6) . ?
C19 H19 0.9300 . ?
C21 C25 1.389(6) . ?
C21 H21 0.9300 . ?
C22 C26 1.370(6) . ?
C22 H22 0.9300 . ?
N3 C29 1.318(7) . ?
N3 C32 1.394(7) . ?
N3 C33 1.441(8) . ?
N4 C29 1.330(8) . ?
N4 C34 1.373(8) . ?
N4 H4 0.8600 . ?
C29 C35 1.480(9) . ?
C30 C36 1.393(9) . ?
C30 C31 1.394(9) . ?
C30 H30 0.9300 . ?
C31 C36 1.380(9) 2_765 ?
C31 C33 1.496(8) . ?
C32 C34 1.326(9) . ?
C32 H32 0.9300 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C31 1.380(9) 2_765 ?
C36 H36 0.9300 . ?
O11 H11A 0.8575 . ?
O11 H11B 0.8575 . ?
O12 H12A 0.8577 . ?
O12 H12B 0.8576 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Cd1 O7 180.000(1) 2_665 1_556 ?
O7 Cd1 O4 86.27(13) 2_665 1_455 ?
O7 Cd1 O4 93.73(13) 1_556 1_455 ?
O7 Cd1 O4 93.73(13) 2_665 2_766 ?
O7 Cd1 O4 86.27(13) 1_556 2_766 ?
O4 Cd1 O4 180.000(1) 1_455 2_766 ?
O7 Cd1 O1 90.38(11) 2_665 . ?
O7 Cd1 O1 89.62(11) 1_556 . ?
O4 Cd1 O1 85.17(12) 1_455 . ?
O4 Cd1 O1 94.83(12) 2_766 . ?
O7 Cd1 O1 89.62(11) 2_665 2_666 ?
O7 Cd1 O1 90.38(11) 1_556 2_666 ?
O4 Cd1 O1 94.83(12) 1_455 2_666 ?
O4 Cd1 O1 85.17(12) 2_766 2_666 ?
O1 Cd1 O1 180.000(1) . 2_666 ?
O8 Cd2 O3 98.42(14) 1_545 1_444 ?
O8 Cd2 O1 101.44(12) 1_545 1_544 ?
O3 Cd2 O1 114.23(11) 1_444 1_544 ?
O8 Cd2 O6 97.99(12) 1_545 . ?
O3 Cd2 O6 99.43(13) 1_444 . ?
O1 Cd2 O6 137.69(12) 1_544 . ?
O8 Cd2 O5 152.69(12) 1_545 . ?
O3 Cd2 O5 91.33(14) 1_444 . ?
O1 Cd2 O5 97.59(12) 1_544 . ?
O6 Cd2 O5 55.09(12) . . ?
O8 Cd2 C27 125.19(13) 1_545 . ?
O3 Cd2 C27 96.46(13) 1_444 . ?
O1 Cd2 C27 119.33(13) 1_544 . ?
O6 Cd2 C27 27.37(13) . . ?
O5 Cd2 C27 27.72(13) . . ?
C15 O1 Cd2 104.5(3) . 1_566 ?
C15 O1 Cd1 133.7(3) . . ?
Cd2 O1 Cd1 100.16(11) 1_566 . ?
C20 O4 Cd1 146.2(3) . 1_655 ?
C20 O3 Cd2 115.1(3) . 1_666 ?
C14 O7 Cd1 145.8(3) . 1_554 ?
C27 O6 Cd2 93.9(3) . . ?
C27 O5 Cd2 89.5(3) . . ?
C14 O8 Cd2 121.3(3) . 1_565 ?
N2 N1 O9 129.8(6) . . ?
N2 N1 C25 115.0(4) . . ?
O9 N1 C25 115.1(6) . . ?
N1 N2 O10 124.8(6) . . ?
N1 N2 C26 117.3(4) . . ?
O10 N2 C26 116.5(6) . . ?
C21 C11 C13 119.1(4) . . ?
C21 C11 C20 118.6(4) . . ?
C13 C11 C20 122.3(4) . . ?
C16 C12 C26 119.0(4) . . ?
C16 C12 H12 120.5 . . ?
C26 C12 H12 120.5 . . ?
C24 C13 C11 120.2(4) . . ?
C24 C13 H13 119.9 . . ?
C11 C13 H13 119.9 . . ?
O7 C14 O8 125.9(4) . . ?
O7 C14 C17 117.2(4) . . ?
O8 C14 C17 116.9(4) . . ?
O2 C15 O1 121.6(4) . . ?
O2 C15 C24 121.3(4) . . ?
O1 C15 C24 117.1(4) . . ?
C12 C16 C18 120.4(4) . . ?
C12 C16 C27 120.3(4) . . ?
C18 C16 C27 119.2(4) . . ?
C22 C17 C18 119.1(4) . . ?
C22 C17 C14 121.2(4) . . ?
C18 C17 C14 119.7(4) . . ?
C16 C18 C17 120.4(4) . . ?
C16 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C25 C19 C24 119.5(4) . . ?
C25 C19 H19 120.3 . . ?
C24 C19 H19 120.3 . . ?
O4 C20 O3 124.7(4) . . ?
O4 C20 C11 117.7(4) . . ?
O3 C20 C11 117.5(4) . . ?
C25 C21 C11 119.7(4) . . ?
C25 C21 H21 120.1 . . ?
C11 C21 H21 120.1 . . ?
C26 C22 C17 120.1(4) . . ?
C26 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C29 N3 C32 108.5(5) . . ?
C29 N3 C33 125.1(6) . . ?
C32 N3 C33 126.3(6) . . ?
C13 C24 C19 120.0(4) . . ?
C13 C24 C15 120.5(4) . . ?
C19 C24 C15 119.5(4) . . ?
C19 C25 C21 121.2(4) . . ?
C19 C25 N1 120.7(4) . . ?
C21 C25 N1 117.9(4) . . ?
C22 C26 C12 121.0(4) . . ?
C22 C26 N2 115.9(4) . . ?
C12 C26 N2 123.1(4) . . ?
O6 C27 O5 121.5(4) . . ?
O6 C27 C16 119.3(4) . . ?
O5 C27 C16 119.2(4) . . ?
O6 C27 Cd2 58.7(2) . . ?
O5 C27 Cd2 62.8(2) . . ?
C16 C27 Cd2 175.8(3) . . ?
C29 N4 C34 109.0(5) . . ?
C29 N4 H4 125.5 . . ?
C34 N4 H4 125.5 . . ?
N3 C29 N4 108.1(5) . . ?
N3 C29 C35 127.9(7) . . ?
N4 C29 C35 124.0(7) . . ?
C36 C30 C31 121.3(6) . . ?
C36 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C36 C31 C30 118.4(6) 2_765 . ?
C36 C31 C33 121.4(6) 2_765 . ?
C30 C31 C33 120.2(7) . . ?
C34 C32 N3 107.1(6) . . ?
C34 C32 H32 126.5 . . ?
N3 C32 H32 126.5 . . ?
N3 C33 C31 113.9(5) . . ?
N3 C33 H33A 108.8 . . ?
C31 C33 H33A 108.8 . . ?
N3 C33 H33B 108.8 . . ?
C31 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C32 C34 N4 107.3(6) . . ?
C32 C34 H34 126.4 . . ?
N4 C34 H34 126.4 . . ?
C29 C35 H35A 109.5 . . ?
C29 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C29 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C31 C36 C30 120.3(6) 2_765 . ?
C31 C36 H36 119.9 2_765 . ?
C30 C36 H36 119.9 . . ?
H11A O11 H11B 109.5 . . ?
H12A O12 H12B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.105
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p
_database_code_depnum_ccdc_archive 'CCDC 1027726'
_audit_update_record             
;
2014-11-24 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H18 Cd N5 O6.50'
_chemical_formula_weight         616.85

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'
Cd Cd -0.8075 1.2024 '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'

_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                   14.256(3)
_cell_length_b                   15.256(3)
_cell_length_c                   23.920(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.486(3)
_cell_angle_gamma                90.00
_cell_volume                     5098.3(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2878
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      22.15

_exptl_crystal_description       blcok
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2472
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8986
_exptl_absorpt_correction_T_max  0.9308
_exptl_absorpt_process_details   'SADABS,(Sheldrick, 2001)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12062
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4479
_reflns_number_gt                3084
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON

_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)+(0.0833P)²+6.9265P] 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         4479
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1549
_refine_ls_wR_factor_gt          0.1356
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.49973(3) 0.04534(3) 0.426425(19) 0.04084(19) Uani 1 1 d . . .
O2 O 0.3940(3) 0.0074(3) 0.47962(19) 0.0487(11) Uani 1 1 d . . .
O3 O 0.3738(3) -0.0825(3) 0.4059(2) 0.0511(12) Uani 1 1 d . . .
N5 N 0.4179(4) 0.9584(3) 0.1186(2) 0.0379(12) Uani 1 1 d . . .
N6 N 0.4083(4) 0.1088(3) 0.3468(2) 0.0424(13) Uani 1 1 d . . .
O5 O 0.0216(6) -0.0587(6) 0.5737(3) 0.132(4) Uani 1 1 d . . .
N7 N 0.3867(4) 0.2229(3) 0.2897(2) 0.0364(12) Uani 1 1 d . . .
O4 O 0.1088(6) 0.0510(5) 0.5653(3) 0.103(2) Uani 1 1 d . . .
N8 N 0.3774(4) 0.8429(3) 0.1636(2) 0.0435(13) Uani 1 1 d . . .
C6 C 0.2585(4) -0.0875(4) 0.4648(2) 0.0369(14) Uani 1 1 d . . .
C7 C 0.2201(4) -0.1673(4) 0.4431(2) 0.0345(13) Uani 1 1 d . . .
H7 H 0.2489 -0.1978 0.4174 0.041 Uiso 1 1 calc R . .
C8 C 0.3203(5) 0.4227(4) 0.2023(3) 0.0424(15) Uani 1 1 d . . .
H8 H 0.2849 0.4378 0.1667 0.051 Uiso 1 1 calc R . .
C9 C 0.4345(5) 0.8747(4) 0.1297(3) 0.0461(16) Uani 1 1 d . . .
H9 H 0.4799 0.8417 0.1160 0.055 Uiso 1 1 calc R . .
C10 C 0.3265(5) 0.3356(4) 0.2184(3) 0.0414(15) Uani 1 1 d . . .
H10 H 0.2955 0.2926 0.1939 0.050 Uiso 1 1 calc R . .
C11 C 0.3481(4) -0.0527(4) 0.4490(3) 0.0416(15) Uani 1 1 d . . .
C12 C 0.3463(5) 0.9807(4) 0.1459(3) 0.0430(16) Uani 1 1 d . . .
H12 H 0.3196 1.0364 0.1456 0.052 Uiso 1 1 calc R . .
C13 C 0.3655(4) 0.4883(4) 0.2381(3) 0.0369(14) Uani 1 1 d . . .
N9 N 0.0837(5) -0.0231(6) 0.5554(3) 0.073(2) Uani 1 1 d . . .
C16 C 0.3795(4) 0.3134(4) 0.2715(3) 0.0364(14) Uani 1 1 d . . .
C17 C 0.3674(5) 0.6515(4) 0.2568(3) 0.0460(16) Uani 1 1 d . . .
H17 H 0.3655 0.6402 0.2948 0.055 Uiso 1 1 calc R . .
C18 C 0.1395(4) -0.2021(4) 0.4592(3) 0.0398(15) Uani 1 1 d . . .
C19 C 0.4162(5) 0.4643(4) 0.2919(3) 0.0399(15) Uani 1 1 d . . .
H19 H 0.4454 0.5073 0.3171 0.048 Uiso 1 1 calc R . .
C20 C 0.2143(5) -0.0407(4) 0.5019(3) 0.0432(15) Uani 1 1 d . . .
H20 H 0.2389 0.0127 0.5168 0.052 Uiso 1 1 calc R . .
C21 C 0.4235(4) 0.3778(4) 0.3083(2) 0.0382(14) Uani 1 1 d . . .
H21 H 0.4581 0.3626 0.3442 0.046 Uiso 1 1 calc R . .
C22 C 0.3656(4) 0.5808(4) 0.2186(3) 0.0391(14) Uani 1 1 d . . .
C23 C 0.3994(5) 0.1940(4) 0.3436(3) 0.0444(16) Uani 1 1 d . . .
H23 H 0.4016 0.2303 0.3750 0.053 Uiso 1 1 calc R . .
C24 C 0.3195(5) 0.9111(4) 0.1732(3) 0.0517(18) Uani 1 1 d . . .
H24 H 0.2714 0.9093 0.1944 0.062 Uiso 1 1 calc R . .
C25 C 0.3741(4) 0.7539(4) 0.1825(3) 0.0414(15) Uani 1 1 d . . .
C26 C 0.3717(5) 0.6862(4) 0.1439(3) 0.0515(18) Uani 1 1 d . . .
H26 H 0.3730 0.6981 0.1059 0.062 Uiso 1 1 calc R . .
C29 C 0.3673(5) 0.6003(4) 0.1622(3) 0.0457(16) Uani 1 1 d . . .
H29 H 0.3655 0.5548 0.1361 0.055 Uiso 1 1 calc R . .
C30 C 0.3720(5) 0.7365(4) 0.2391(3) 0.0490(17) Uani 1 1 d . . .
H30 H 0.3736 0.7823 0.2649 0.059 Uiso 1 1 calc R . .
C31 C 0.3839(5) 0.1499(4) 0.2557(3) 0.0474(16) Uani 1 1 d . . .
H31 H 0.3739 0.1484 0.2160 0.057 Uiso 1 1 calc R . .
C32 C 0.3985(5) 0.0810(4) 0.2915(3) 0.0479(16) Uani 1 1 d . . .
H32 H 0.4015 0.0229 0.2803 0.057 Uiso 1 1 calc R . .
C33 C 0.1331(5) -0.0751(5) 0.5163(3) 0.0475(16) Uani 1 1 d . . .
C36 C 0.0950(5) -0.1545(5) 0.4968(3) 0.0484(17) Uani 1 1 d . . .
H36 H 0.0408 -0.1762 0.5082 0.058 Uiso 1 1 calc R . .
C37 C 0.1030(5) -0.2918(4) 0.4376(3) 0.0480(17) Uani 1 1 d . . .
O6 O 0.1341(4) -0.3272(3) 0.3998(3) 0.0687(15) Uani 1 1 d . . .
O7 O 0.0395(3) -0.3242(3) 0.4623(2) 0.0623(14) Uani 1 1 d . . .
O1W O 0.3438(3) 0.7758(3) 0.0014(2) 0.184(9) Uani 0.50 1 d PR . .
H1WA H 0.3512 0.7254 0.0168 0.276 Uiso 0.50 1 d PR . .
H1WB H 0.3637 0.7751 -0.0298 0.276 Uiso 0.50 1 d PR . .


_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 N5 2.192(5) 2_645 ?
Cd1 O7 2.197(5) 3 ?
Cd1 O2 2.233(4) . ?
Cd1 N6 2.297(5) . ?
Cd1 O2 2.576(5) 5_656 ?
Cd1 O3 2.631(4) . ?
O2 C11 1.272(7) . ?
O2 Cd1 2.576(5) 5_656 ?
O3 C11 1.247(8) . ?
N5 C9 1.316(7) . ?
N5 C12 1.360(8) . ?
N5 Cd1 2.192(5) 2_665 ?
N6 C23 1.306(7) . ?
N6 C32 1.369(8) . ?
O5 N9 1.194(9) . ?
N7 C23 1.340(7) . ?
N7 C31 1.376(8) . ?
N7 C16 1.445(7) . ?
O4 N9 1.195(9) . ?
N8 C9 1.346(7) . ?
N8 C24 1.376(8) . ?
N8 C25 1.436(8) . ?
C6 C20 1.384(8) . ?
C6 C7 1.392(8) . ?
C6 C11 1.500(8) . ?
C7 C18 1.388(8) . ?
C7 H7 0.9300 . ?
C8 C10 1.381(8) . ?
C8 C13 1.390(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C16 1.386(8) . ?
C10 H10 0.9300 . ?
C12 C24 1.342(9) . ?
C12 H12 0.9300 . ?
C13 C19 1.394(8) . ?
C13 C22 1.486(9) . ?
N9 C33 1.505(9) . ?
C16 C21 1.383(8) . ?
C17 C30 1.369(9) . ?
C17 C22 1.412(9) . ?
C17 H17 0.9300 . ?
C18 C36 1.402(9) . ?
C18 C37 1.517(9) . ?
C19 C21 1.374(8) . ?
C19 H19 0.9300 . ?
C20 C33 1.374(9) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C29 1.386(8) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.381(9) . ?
C25 C30 1.386(9) . ?
C26 C29 1.387(8) . ?
C26 H26 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.346(9) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C36 1.370(9) . ?
C36 H36 0.9300 . ?
C37 O6 1.211(8) . ?
C37 O7 1.275(8) . ?
O7 Cd1 2.197(5) 3_445 ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?

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
N5 Cd1 O7 128.20(18) 2_645 3 ?
N5 Cd1 O2 127.72(17) 2_645 . ?
O7 Cd1 O2 99.40(17) 3 . ?
N5 Cd1 N6 96.80(19) 2_645 . ?
O7 Cd1 N6 90.07(18) 3 . ?
O2 Cd1 N6 104.25(17) . . ?
N5 Cd1 O2 87.73(17) 2_645 5_656 ?
O7 Cd1 O2 83.19(16) 3 5_656 ?
O2 Cd1 O2 76.59(17) . 5_656 ?
N6 Cd1 O2 173.25(16) . 5_656 ?
N5 Cd1 O3 82.66(16) 2_645 . ?
O7 Cd1 O3 149.13(17) 3 . ?
O2 Cd1 O3 53.24(15) . . ?
N6 Cd1 O3 84.51(17) . . ?
O2 Cd1 O3 101.08(14) 5_656 . ?
C11 O2 Cd1 100.8(4) . . ?
C11 O2 Cd1 115.1(4) . 5_656 ?
Cd1 O2 Cd1 103.41(17) . 5_656 ?
C11 O3 Cd1 82.9(4) . . ?
C9 N5 C12 105.6(5) . . ?
C9 N5 Cd1 126.4(4) . 2_665 ?
C12 N5 Cd1 127.7(4) . 2_665 ?
C23 N6 C32 105.2(5) . . ?
C23 N6 Cd1 120.0(4) . . ?
C32 N6 Cd1 127.1(4) . . ?
C23 N7 C31 106.6(5) . . ?
C23 N7 C16 126.3(5) . . ?
C31 N7 C16 127.1(5) . . ?
C9 N8 C24 106.5(5) . . ?
C9 N8 C25 126.3(5) . . ?
C24 N8 C25 127.1(5) . . ?
C20 C6 C7 119.7(5) . . ?
C20 C6 C11 120.0(6) . . ?
C7 C6 C11 120.4(5) . . ?
C18 C7 C6 121.1(5) . . ?
C18 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C10 C8 C13 121.8(6) . . ?
C10 C8 H8 119.1 . . ?
C13 C8 H8 119.1 . . ?
N5 C9 N8 111.4(5) . . ?
N5 C9 H9 124.3 . . ?
N8 C9 H9 124.3 . . ?
C8 C10 C16 118.9(6) . . ?
C8 C10 H10 120.5 . . ?
C16 C10 H10 120.5 . . ?
O3 C11 O2 122.5(6) . . ?
O3 C11 C6 119.0(6) . . ?
O2 C11 C6 118.4(6) . . ?
C24 C12 N5 110.4(5) . . ?
C24 C12 H12 124.8 . . ?
N5 C12 H12 124.8 . . ?
C8 C13 C19 118.1(6) . . ?
C8 C13 C22 121.3(6) . . ?
C19 C13 C22 120.5(6) . . ?
O5 N9 O4 125.0(8) . . ?
O5 N9 C33 117.5(8) . . ?
O4 N9 C33 117.6(7) . . ?
C21 C16 C10 120.3(5) . . ?
C21 C16 N7 119.5(5) . . ?
C10 C16 N7 120.2(5) . . ?
C30 C17 C22 121.2(6) . . ?
C30 C17 H17 119.4 . . ?
C22 C17 H17 119.4 . . ?
C7 C18 C36 119.0(5) . . ?
C7 C18 C37 119.8(6) . . ?
C36 C18 C37 121.1(6) . . ?
C21 C19 C13 120.7(6) . . ?
C21 C19 H19 119.6 . . ?
C13 C19 H19 119.6 . . ?
C33 C20 C6 118.5(6) . . ?
C33 C20 H20 120.8 . . ?
C6 C20 H20 120.8 . . ?
C19 C21 C16 120.2(6) . . ?
C19 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?
C29 C22 C17 117.7(6) . . ?
C29 C22 C13 120.8(6) . . ?
C17 C22 C13 121.5(5) . . ?
N6 C23 N7 112.1(6) . . ?
N6 C23 H23 124.0 . . ?
N7 C23 H23 124.0 . . ?
C12 C24 N8 106.1(6) . . ?
C12 C24 H24 126.9 . . ?
N8 C24 H24 126.9 . . ?
C26 C25 C30 120.5(6) . . ?
C26 C25 N8 119.7(6) . . ?
C30 C25 N8 119.9(6) . . ?
C25 C26 C29 119.5(6) . . ?
C25 C26 H26 120.2 . . ?
C29 C26 H26 120.2 . . ?
C22 C29 C26 121.4(6) . . ?
C22 C29 H29 119.3 . . ?
C26 C29 H29 119.3 . . ?
C17 C30 C25 119.7(6) . . ?
C17 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?
C32 C31 N7 105.8(6) . . ?
C32 C31 H31 127.1 . . ?
N7 C31 H31 127.1 . . ?
C31 C32 N6 110.3(6) . . ?
C31 C32 H32 124.8 . . ?
N6 C32 H32 124.8 . . ?
C36 C33 C20 123.3(6) . . ?
C36 C33 N9 118.3(6) . . ?
C20 C33 N9 118.4(7) . . ?
C33 C36 C18 118.5(6) . . ?
C33 C36 H36 120.8 . . ?
C18 C36 H36 120.8 . . ?
O6 C37 O7 124.9(6) . . ?
O6 C37 C18 120.4(6) . . ?
O7 C37 C18 114.8(7) . . ?
C37 O7 Cd1 108.8(5) . 3_445 ?
H1WA O1W H1WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.111
_exptl_crystal_preparation       Luminescent
