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


data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C30 H18 Cd2 N10 O10'
_chemical_formula_sum            'C30 H18 Cd2 N10 O10'
_chemical_formula_weight         903.34

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   'P2(1)/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                   10.130(2)
_cell_length_b                   10.646(2)
_cell_length_c                   28.531(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.23(3)
_cell_angle_gamma                90.00
_cell_volume                     3068.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6976
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            29299
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.46
_reflns_number_total             6976
_reflns_number_gt                5780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0178P)²+12.0278P] 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         6976
_refine_ls_number_parameters     481
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.50546(3) 0.66820(3) 0.989841(10) 0.01160(8) Uani 1 1 d . . .
Cd2 Cd 1.21354(3) 0.50827(3) 0.928619(10) 0.01240(8) Uani 1 1 d . . .
O1 O 1.2556(3) 0.6395(3) 0.98885(9) 0.0141(6) Uani 1 1 d . . .
O2 O 1.3628(3) 0.8010(3) 1.02222(10) 0.0165(6) Uani 1 1 d . . .
O3 O 0.6626(3) 0.8244(3) 1.00213(11) 0.0212(7) Uani 1 1 d . . .
O4 O 0.7403(3) 0.6325(3) 1.01015(10) 0.0156(6) Uani 1 1 d . . .
O5 O 1.0246(3) 1.0770(3) 1.08994(10) 0.0185(7) Uani 1 1 d . . .
O6 O 1.0726(3) 0.3898(3) 0.87614(10) 0.0192(7) Uani 1 1 d . . .
O7 O 0.9890(3) 0.5215(3) 0.92597(10) 0.0165(6) Uani 1 1 d . . .
O8 O 0.5037(3) 0.4838(3) 0.94953(9) 0.0140(6) Uani 1 1 d . . .
O9 O 0.3720(3) 0.4203(3) 0.88798(10) 0.0202(7) Uani 1 1 d . . .
O10 O 0.6819(3) 0.2315(3) 0.77498(10) 0.0176(7) Uani 1 1 d . . .
N1 N 1.5389(4) 1.1615(5) 1.23694(13) 0.0278(9) Uani 1 1 d . . .
N2 N 1.6290(4) 1.2432(4) 1.25532(13) 0.0277(10) Uani 1 1 d D . .
N3 N 1.6162(4) 1.3564(5) 1.23611(17) 0.0378(11) Uani 1 1 d . . .
N4 N 1.5150(4) 1.3504(4) 1.20398(17) 0.0356(11) Uani 1 1 d . . .
N5 N 1.7299(5) 1.2148(7) 1.29178(17) 0.0617(19) Uani 1 1 d D . .
N6 N 0.1894(3) 0.4049(4) 0.63365(12) 0.0187(8) Uani 1 1 d . . .
N7 N 0.0978(3) 0.3786(3) 0.59880(12) 0.0169(8) Uani 1 1 d D . .
N8 N 0.1040(3) 0.2610(4) 0.58368(12) 0.0174(8) Uani 1 1 d . . .
N9 N 0.2047(3) 0.2067(4) 0.60910(11) 0.0153(7) Uani 1 1 d . . .
N10 N 0.0100(5) 0.4724(5) 0.57728(17) 0.0403(12) Uani 1 1 d D . .
C1 C 1.1286(4) 0.8003(4) 1.02425(13) 0.0121(8) Uani 1 1 d . . .
C2 C 1.1366(4) 0.9114(4) 1.04974(14) 0.0141(8) Uani 1 1 d . . .
H2 H 1.2185 0.9489 1.0571 0.080 Uiso 1 1 calc . . .
C3 C 1.0226(4) 0.9664(4) 1.06423(14) 0.0133(8) Uani 1 1 d . . .
C4 C 0.8995(4) 0.9156(4) 1.05128(14) 0.0141(8) Uani 1 1 d . . .
H4 H 0.8227 0.9551 1.0596 0.080 Uiso 1 1 calc . . .
C5 C 0.8924(4) 0.8041(4) 1.02546(14) 0.0135(8) Uani 1 1 d . . .
C6 C 1.0058(4) 0.7432(4) 1.01238(13) 0.0121(8) Uani 1 1 d . . .
H6 H 1.0003 0.6672 0.9963 0.080 Uiso 1 1 calc . . .
C7 C 1.2559(4) 0.7428(4) 1.01054(13) 0.0118(8) Uani 1 1 d . . .
C8 C 0.7577(4) 0.7510(4) 1.01176(14) 0.0139(8) Uani 1 1 d . . .
C9 C 1.1396(4) 1.1080(4) 1.11745(14) 0.0164(9) Uani 1 1 d . . .
C10 C 1.2056(4) 1.0219(4) 1.14727(15) 0.0198(9) Uani 1 1 d . . .
H10 H 1.1770 0.9390 1.1480 0.080 Uiso 1 1 calc . . .
C11 C 1.3148(4) 1.0604(4) 1.17601(15) 0.0202(9) Uani 1 1 d . . .
H11 H 1.3603 1.0031 1.1958 0.080 Uiso 1 1 calc . . .
C12 C 1.3562(4) 1.1861(4) 1.17511(14) 0.0162(9) Uani 1 1 d . . .
C13 C 1.2887(4) 1.2696(4) 1.14526(16) 0.0217(10) Uani 1 1 d . . .
H13 H 1.3159 1.3530 1.1448 0.080 Uiso 1 1 calc . . .
C14 C 1.1803(4) 1.2312(5) 1.11571(16) 0.0210(10) Uani 1 1 d . . .
H14 H 1.1363 1.2878 1.0952 0.080 Uiso 1 1 calc . . .
C15 C 1.4693(4) 1.2310(5) 1.20570(15) 0.0196(9) Uani 1 1 d . . .
C16 C 0.8383(4) 0.4014(4) 0.87549(14) 0.0128(8) Uani 1 1 d . . .
C17 C 0.7299(4) 0.4352(4) 0.90029(13) 0.0130(8) Uani 1 1 d . . .
H17 H 0.7422 0.4801 0.9282 0.080 Uiso 1 1 calc . . .
C18 C 0.6030(4) 0.4009(4) 0.88271(13) 0.0115(8) Uani 1 1 d . . .
C19 C 0.5847(4) 0.3345(4) 0.84027(13) 0.0135(8) Uani 1 1 d . . .
H19 H 0.5000 0.3117 0.8285 0.080 Uiso 1 1 calc . . .
C20 C 0.6932(4) 0.3031(4) 0.81596(13) 0.0133(8) Uani 1 1 d . . .
C21 C 0.8207(4) 0.3351(4) 0.83341(13) 0.0139(8) Uani 1 1 d . . .
H21 H 0.8933 0.3125 0.8172 0.080 Uiso 1 1 calc . . .
C22 C 0.9753(4) 0.4396(4) 0.89362(14) 0.0131(8) Uani 1 1 d . . .
C23 C 0.4847(4) 0.4374(4) 0.90748(14) 0.0133(8) Uani 1 1 d . . .
C24 C 0.5731(4) 0.2498(4) 0.74302(13) 0.0143(9) Uani 1 1 d . . .
C25 C 0.5255(4) 0.3692(4) 0.73223(15) 0.0192(9) Uani 1 1 d . . .
H25 H 0.5634 0.4391 0.7475 0.080 Uiso 1 1 calc . . .
C26 C 0.4200(4) 0.3838(4) 0.69820(14) 0.0188(9) Uani 1 1 d . . .
H26 H 0.3868 0.4633 0.6908 0.080 Uiso 1 1 calc . . .
C27 C 0.3647(4) 0.2775(4) 0.67526(13) 0.0149(9) Uani 1 1 d . . .
C28 C 0.4132(4) 0.1583(4) 0.68670(14) 0.0194(9) Uani 1 1 d . . .
H28 H 0.3754 0.0880 0.6718 0.080 Uiso 1 1 calc . . .
C29 C 0.5191(4) 0.1446(4) 0.72065(15) 0.0194(9) Uani 1 1 d . . .
H29 H 0.5529 0.0653 0.7281 0.080 Uiso 1 1 calc . . .
C30 C 0.2540(4) 0.2953(4) 0.63932(14) 0.0154(9) Uani 1 1 d . . .
H5A H 1.790(6) 1.139(5) 1.286(3) 0.080 Uiso 1 1 d D . .
H5B H 1.692(7) 1.209(7) 1.3237(13) 0.080 Uiso 1 1 d D . .
H10A H -0.015(7) 0.535(6) 0.6022(19) 0.080 Uiso 1 1 d D . .
H10B H -0.069(5) 0.434(7) 0.558(2) 0.080 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
Cd1 O2 2.267(3) . ?
Cd1 O8 2.275(3) 1_655 ?
Cd1 O3 2.311(3) 1_655 ?
Cd1 O8 2.375(3) 3_767 ?
Cd1 O4 2.436(3) 1_655 ?
Cd1 N8 2.503(4) 2_656 ?
Cd1 O1 2.547(3) . ?
Cd1 C8 2.731(4) 1_655 ?
Cd1 C7 2.755(4) . ?
Cd2 O1 2.231(3) . ?
Cd2 O9 2.253(3) 1_655 ?
Cd2 O7 2.275(3) . ?
Cd2 O4 2.323(3) 3_767 ?
Cd2 O6 2.357(3) . ?
Cd2 N9 2.537(4) 2_656 ?
Cd2 C22 2.646(4) . ?
O1 C7 1.263(5) . ?
O2 C7 1.270(5) . ?
O3 C8 1.255(5) . ?
O3 Cd1 2.311(3) 1_455 ?
O4 C8 1.274(5) . ?
O4 Cd2 2.323(3) 3_767 ?
O4 Cd1 2.436(3) 1_455 ?
O5 C3 1.386(5) . ?
O5 C9 1.396(5) . ?
O6 C22 1.254(5) . ?
O7 C22 1.270(5) . ?
O8 C23 1.299(5) . ?
O8 Cd1 2.275(3) 1_455 ?
O8 Cd1 2.375(3) 3_767 ?
O9 C23 1.246(5) . ?
O9 Cd2 2.253(3) 1_455 ?
O10 C24 1.392(5) . ?
O10 C20 1.393(5) . ?
N1 C15 1.321(6) . ?
N1 N2 1.339(6) . ?
N2 N3 1.327(6) . ?
N2 N5 1.436(4) . ?
N3 N4 1.326(6) . ?
N4 C15 1.355(7) . ?
N5 H5A 1.03(2) . ?
N5 H5B 1.02(2) . ?
N6 N7 1.339(5) . ?
N6 C30 1.341(6) . ?
N7 N8 1.328(5) . ?
N7 N10 1.443(4) . ?
N8 N9 1.338(5) . ?
N8 Cd1 2.503(4) 2_646 ?
N9 C30 1.349(6) . ?
N9 Cd2 2.537(4) 2_646 ?
N10 H10A 1.02(2) . ?
N10 H10B 1.02(2) . ?
C1 C2 1.388(6) . ?
C1 C6 1.403(6) . ?
C1 C7 1.505(5) . ?
C2 C3 1.385(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(6) . ?
C4 C5 1.396(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(6) . ?
C5 C8 1.502(6) . ?
C6 H6 0.9300 . ?
C8 Cd1 2.731(4) 1_455 ?
C9 C14 1.377(7) . ?
C9 C10 1.389(6) . ?
C10 C11 1.389(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.403(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.378(6) . ?
C12 C15 1.468(6) . ?
C13 C14 1.396(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C21 1.393(6) . ?
C16 C17 1.396(6) . ?
C16 C22 1.502(5) . ?
C17 C18 1.393(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.402(5) . ?
C18 C23 1.487(5) . ?
C19 C20 1.383(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.392(5) . ?
C21 H21 0.9300 . ?
C24 C29 1.382(6) . ?
C24 C25 1.386(6) . ?
C25 C26 1.399(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.403(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.390(6) . ?
C27 C30 1.475(6) . ?
C28 C29 1.399(6) . ?
C28 H28 0.9300 . ?
C29 H29 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 O8 139.72(10) . 1_655 ?
O2 Cd1 O3 86.69(11) . 1_655 ?
O8 Cd1 O3 132.63(10) 1_655 1_655 ?
O2 Cd1 O8 93.87(10) . 3_767 ?
O8 Cd1 O8 77.35(10) 1_655 3_767 ?
O3 Cd1 O8 116.31(10) 1_655 3_767 ?
O2 Cd1 O4 129.88(10) . 1_655 ?
O8 Cd1 O4 87.50(10) 1_655 1_655 ?
O3 Cd1 O4 55.02(11) 1_655 1_655 ?
O8 Cd1 O4 79.07(10) 3_767 1_655 ?
O2 Cd1 N8 80.73(11) . 2_656 ?
O8 Cd1 N8 86.02(11) 1_655 2_656 ?
O3 Cd1 N8 95.80(12) 1_655 2_656 ?
O8 Cd1 N8 147.19(11) 3_767 2_656 ?
O4 Cd1 N8 128.73(11) 1_655 2_656 ?
O2 Cd1 O1 54.31(10) . . ?
O8 Cd1 O1 85.42(10) 1_655 . ?
O3 Cd1 O1 139.54(10) 1_655 . ?
O8 Cd1 O1 80.45(10) 3_767 . ?
O4 Cd1 O1 159.34(10) 1_655 . ?
N8 Cd1 O1 70.09(11) 2_656 . ?
O2 Cd1 C8 108.62(12) . 1_655 ?
O8 Cd1 C8 111.50(11) 1_655 1_655 ?
O3 Cd1 C8 27.22(12) 1_655 1_655 ?
O8 Cd1 C8 98.01(11) 3_767 1_655 ?
O4 Cd1 C8 27.81(12) 1_655 1_655 ?
N8 Cd1 C8 114.45(12) 2_656 1_655 ?
O1 Cd1 C8 162.39(11) . 1_655 ?
O2 Cd1 C7 27.13(11) . . ?
O8 Cd1 C7 112.61(12) 1_655 . ?
O3 Cd1 C7 113.12(12) 1_655 . ?
O8 Cd1 C7 87.39(11) 3_767 . ?
O4 Cd1 C7 152.78(10) 1_655 . ?
N8 Cd1 C7 73.07(12) 2_656 . ?
O1 Cd1 C7 27.19(11) . . ?
C8 Cd1 C7 135.68(12) 1_655 . ?
O1 Cd2 O9 123.63(10) . 1_655 ?
O1 Cd2 O7 96.94(10) . . ?
O9 Cd2 O7 139.25(10) 1_655 . ?
O1 Cd2 O4 78.93(10) . 3_767 ?
O9 Cd2 O4 90.41(11) 1_655 3_767 ?
O7 Cd2 O4 102.15(11) . 3_767 ?
O1 Cd2 O6 153.72(10) . . ?
O9 Cd2 O6 82.64(10) 1_655 . ?
O7 Cd2 O6 56.95(10) . . ?
O4 Cd2 O6 102.21(11) 3_767 . ?
O1 Cd2 N9 75.86(11) . 2_656 ?
O9 Cd2 N9 81.99(12) 1_655 2_656 ?
O7 Cd2 N9 106.93(11) . 2_656 ?
O4 Cd2 N9 143.33(10) 3_767 2_656 ?
O6 Cd2 N9 112.18(11) . 2_656 ?
O1 Cd2 C22 125.52(12) . . ?
O9 Cd2 C22 110.83(12) 1_655 . ?
O7 Cd2 C22 28.66(12) . . ?
O4 Cd2 C22 103.49(11) 3_767 . ?
O6 Cd2 C22 28.29(11) . . ?
N9 Cd2 C22 112.78(12) 2_656 . ?
C7 O1 Cd2 156.4(3) . . ?
C7 O1 Cd1 85.6(2) . . ?
Cd2 O1 Cd1 102.54(10) . . ?
C7 O2 Cd1 98.4(2) . . ?
C8 O3 Cd1 95.4(3) . 1_455 ?
C8 O4 Cd2 126.3(3) . 3_767 ?
C8 O4 Cd1 89.1(2) . 1_455 ?
Cd2 O4 Cd1 114.75(12) 3_767 1_455 ?
C3 O5 C9 118.5(3) . . ?
C22 O6 Cd2 88.7(2) . . ?
C22 O7 Cd2 92.1(2) . . ?
C23 O8 Cd1 142.2(3) . 1_455 ?
C23 O8 Cd1 113.8(3) . 3_767 ?
Cd1 O8 Cd1 102.65(10) 1_455 3_767 ?
C23 O9 Cd2 111.9(3) . 1_455 ?
C24 O10 C20 119.0(3) . . ?
C15 N1 N2 102.4(4) . . ?
N3 N2 N1 112.7(4) . . ?
N3 N2 N5 122.2(5) . . ?
N1 N2 N5 125.1(5) . . ?
N4 N3 N2 106.8(4) . . ?
N3 N4 C15 105.6(4) . . ?
N2 N5 H5A 116(4) . . ?
N2 N5 H5B 111(4) . . ?
H5A N5 H5B 111(6) . . ?
N7 N6 C30 102.3(3) . . ?
N8 N7 N6 113.0(3) . . ?
N8 N7 N10 123.8(4) . . ?
N6 N7 N10 122.9(4) . . ?
N7 N8 N9 106.5(3) . . ?
N7 N8 Cd1 128.0(3) . 2_646 ?
N9 N8 Cd1 123.8(3) . 2_646 ?
N8 N9 C30 106.0(4) . . ?
N8 N9 Cd2 112.9(2) . 2_646 ?
C30 N9 Cd2 137.4(3) . 2_646 ?
N7 N10 H10A 109(4) . . ?
N7 N10 H10B 112(5) . . ?
H10A N10 H10B 114(6) . . ?
C2 C1 C6 120.8(4) . . ?
C2 C1 C7 117.7(4) . . ?
C6 C1 C7 121.5(4) . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 O5 116.8(4) . . ?
C2 C3 O5 122.5(4) . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 121.7(4) . . ?
C6 C5 C8 120.4(4) . . ?
C4 C5 C8 117.9(4) . . ?
C5 C6 C1 117.9(4) . . ?
C5 C6 H6 121.0 . . ?
C1 C6 H6 121.0 . . ?
O1 C7 O2 121.7(4) . . ?
O1 C7 C1 120.7(4) . . ?
O2 C7 C1 117.6(4) . . ?
O1 C7 Cd1 67.2(2) . . ?
O2 C7 Cd1 54.5(2) . . ?
C1 C7 Cd1 172.1(3) . . ?
O3 C8 O4 120.5(4) . . ?
O3 C8 C5 119.3(4) . . ?
O4 C8 C5 120.2(4) . . ?
O3 C8 Cd1 57.4(2) . 1_455 ?
O4 C8 Cd1 63.1(2) . 1_455 ?
C5 C8 Cd1 176.1(3) . 1_455 ?
C14 C9 C10 121.3(4) . . ?
C14 C9 O5 116.4(4) . . ?
C10 C9 O5 122.2(4) . . ?
C9 C10 C11 119.6(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 119.8(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 C15 119.1(4) . . ?
C11 C12 C15 121.4(4) . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C13 118.8(4) . . ?
C9 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N1 C15 N4 112.5(4) . . ?
N1 C15 C12 124.9(5) . . ?
N4 C15 C12 122.5(4) . . ?
C21 C16 C17 120.8(4) . . ?
C21 C16 C22 119.4(4) . . ?
C17 C16 C22 119.8(4) . . ?
C18 C17 C16 119.3(4) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 C23 121.0(4) . . ?
C19 C18 C23 118.8(3) . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.8(4) . . ?
C19 C20 O10 122.3(3) . . ?
C21 C20 O10 116.8(3) . . ?
C20 C21 C16 119.3(4) . . ?
C20 C21 H21 120.4 . . ?
C16 C21 H21 120.4 . . ?
O6 C22 O7 122.2(4) . . ?
O6 C22 C16 118.8(4) . . ?
O7 C22 C16 119.0(4) . . ?
O6 C22 Cd2 63.0(2) . . ?
O7 C22 Cd2 59.2(2) . . ?
C16 C22 Cd2 177.9(3) . . ?
O9 C23 O8 122.5(4) . . ?
O9 C23 C18 119.6(4) . . ?
O8 C23 C18 117.9(3) . . ?
C29 C24 C25 121.4(4) . . ?
C29 C24 O10 117.2(4) . . ?
C25 C24 O10 121.3(4) . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C26 C27 119.5(4) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 120.3(4) . . ?
C28 C27 C30 121.2(4) . . ?
C26 C27 C30 118.5(4) . . ?
C27 C28 C29 119.9(4) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C24 C29 C28 119.5(4) . . ?
C24 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
N6 C30 N9 112.2(4) . . ?
N6 C30 C27 122.3(4) . . ?
N9 C30 C27 125.5(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5B O6 1.02(2) 2.25(4) 3.184(6) 152(6) 4_676
N10 H10B O3 1.02(2) 2.24(4) 3.177(6) 153(6) 2_546

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.137
_database_code_depnum_ccdc_archive 'CCDC 972184'

data_c2c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C45 H23.5 Mn3 N15 O18.25'
_chemical_formula_sum            'C45 H23.50 Mn3 N15 O18.25'
_chemical_formula_weight         1231.11

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   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                   19.408(4)
_cell_length_b                   38.069(8)
_cell_length_c                   14.436(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.32(3)
_cell_angle_gamma                90.00
_cell_volume                     10287(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11191
_cell_measurement_theta_min      9.30
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4956
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            47116
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         9.30
_diffrn_reflns_theta_max         27.47
_reflns_number_total             11191
_reflns_number_gt                6874
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0884P)²+26.1377P] 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         11191
_refine_ls_number_parameters     711
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.1917
_refine_ls_wR_factor_gt          0.1651
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.026
_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 0.2500 0.7500 0.5000 0.0273(2) Uani 1 2 d S . .
Mn2 Mn 0.19975(3) 0.674014(15) 0.35522(4) 0.02600(17) Uani 1 1 d . . .
Mn3 Mn 0.2500 0.7500 0.0000 0.0267(2) Uani 1 2 d S . .
Mn4 Mn 0.29288(3) 0.673630(15) 0.14333(4) 0.02494(16) Uani 1 1 d . . .
O1 O 0.28215(13) 0.71555(8) 0.3884(2) 0.0373(7) Uani 1 1 d . . .
O2 O 0.32124(13) 0.67672(8) 0.3027(2) 0.0345(6) Uani 1 1 d . . .
O3 O 0.59586(14) 0.67954(9) 0.3546(2) 0.0435(8) Uani 1 1 d . . .
O4 O 0.64913(14) 0.72850(10) 0.4125(2) 0.0496(8) Uani 1 1 d . . .
O5 O 0.44309(17) 0.81686(9) 0.3599(4) 0.0722(13) Uani 1 1 d . . .
O6 O 0.21669(13) 0.71863(8) 0.1170(2) 0.0375(7) Uani 1 1 d . . .
O7 O 0.17019(14) 0.68156(8) 0.1992(2) 0.0361(6) Uani 1 1 d . . .
O8 O -0.10006(15) 0.69431(11) 0.1351(2) 0.0504(9) Uani 1 1 d . . .
O9 O -0.14644(14) 0.74723(11) 0.0930(2) 0.0557(10) Uani 1 1 d . . .
O10 O 0.0553(2) 0.82441(11) 0.0690(3) 0.0713(11) Uani 1 1 d . . .
O11 O 0.25846(17) 0.65688(8) -0.0011(2) 0.0428(7) Uani 1 1 d . . .
O12 O 0.23264(17) 0.70586(8) -0.0890(2) 0.0410(7) Uani 1 1 d . . .
O13 O 0.23539(17) 0.70296(8) -0.4265(2) 0.0423(7) Uani 1 1 d . . .
O14 O 0.22761(19) 0.65191(9) -0.5047(2) 0.0497(8) Uani 1 1 d . . .
O15 O 0.25597(18) 0.56126(9) -0.2399(3) 0.0547(9) Uani 1 1 d . . .
O16 O 0.2028(3) 0.61914(10) 0.3164(3) 0.0679(11) Uani 1 1 d . . .
O17 O 0.28371(19) 0.61797(9) 0.1715(2) 0.0511(8) Uani 1 1 d . . .
O1W O 0.1847(12) 0.9172(6) 0.5650(17) 0.097(6) Uani 0.25 1 d PU . .
O2W O 0.1042(6) 0.9119(3) 0.7020(8) 0.097(3) Uani 0.50 1 d PU . .
O3W O 0.0000 0.8703(2) 0.7500 0.095(2) Uani 1 2 d S . .
C15 C 0.6330(2) 0.92915(10) 0.4720(3) 0.0594(14) Uani 1 1 d G . .
N1 N 0.6181(2) 0.96188(9) 0.4429(3) 0.0835(17) Uani 1 1 d G . .
N2 N 0.6753(2) 0.98130(9) 0.4798(3) 0.0719(14) Uani 1 1 d G . .
N3 N 0.7255(2) 0.96057(9) 0.5318(3) 0.0739(14) Uani 1 1 d G . .
N4 N 0.69934(19) 0.92835(10) 0.5270(3) 0.0677(13) Uani 1 1 d G . .
N5 N 0.6805(6) 1.0182(2) 0.4709(7) 0.138(3) Uani 1 1 d . . .
C30 C 0.0931(3) 0.94626(18) 0.2905(6) 0.102(3) Uani 1 1 d GU . .
N6 N 0.0826(3) 0.97799(18) 0.2561(6) 0.154(4) Uani 1 1 d G . .
N7 N 0.0950(4) 0.99977(18) 0.3281(6) 0.161(3) Uani 1 1 d GU . .
N8 N 0.1132(4) 0.98149(19) 0.4070(6) 0.161(3) Uani 1 1 d GU . .
N9 N 0.1120(4) 0.94841(19) 0.3838(6) 0.143(4) Uani 1 1 d G . .
N10 N 0.0924(7) 1.0348(3) 0.3554(9) 0.258(8) Uani 1 1 d GU . .
C45 C 0.0649(3) 0.44862(15) -0.3368(5) 0.091(2) Uani 1 1 d G . .
N11 N 0.0020(3) 0.44802(16) -0.3931(5) 0.126(3) Uani 1 1 d G . .
N12 N -0.0213(3) 0.41659(16) -0.3962(4) 0.146(4) Uani 1 1 d G . .
N13 N 0.0272(4) 0.39775(15) -0.3417(5) 0.186(7) Uani 1 1 d G . .
N14 N 0.0805(4) 0.41755(14) -0.3050(5) 0.120(3) Uani 1 1 d G . .
N15 N -0.0749(5) 0.3952(3) -0.4428(8) 0.189(5) Uani 1 1 d GU . .
C1 C 0.4554(2) 0.78125(12) 0.3691(4) 0.0426(11) Uani 1 1 d . . .
C2 C 0.39430(19) 0.76161(11) 0.3652(3) 0.0341(9) Uani 1 1 d . . .
H2 H 0.3516 0.7728 0.3650 0.080 Uiso 1 1 calc . . .
C3 C 0.39746(17) 0.72533(11) 0.3617(3) 0.0288(8) Uani 1 1 d . . .
C4 C 0.46130(17) 0.70816(11) 0.3641(3) 0.0302(8) Uani 1 1 d . . .
H4 H 0.4628 0.6838 0.3592 0.080 Uiso 1 1 calc . . .
C5 C 0.52294(18) 0.72833(12) 0.3741(3) 0.0317(9) Uani 1 1 d . . .
C6 C 0.52011(19) 0.76481(12) 0.3744(3) 0.0386(10) Uani 1 1 d . . .
H6 H 0.5610 0.7780 0.3780 0.080 Uiso 1 1 calc . . .
C7 C 0.33031(17) 0.70472(11) 0.3503(3) 0.0261(8) Uani 1 1 d . . .
C8 C 0.59352(18) 0.71112(13) 0.3816(3) 0.0340(9) Uani 1 1 d . . .
C9 C 0.4930(2) 0.84249(13) 0.3930(5) 0.0573(14) Uani 1 1 d . . .
C10 C 0.4766(4) 0.87449(19) 0.3470(7) 0.098(3) Uani 1 1 d U . .
H10 H 0.4349 0.8769 0.2978 0.080 Uiso 1 1 calc . . .
C11 C 0.5221(4) 0.90291(18) 0.3741(6) 0.091(2) Uani 1 1 d U . .
H11 H 0.5099 0.9244 0.3437 0.080 Uiso 1 1 calc . . .
C12 C 0.5848(3) 0.89985(15) 0.4449(4) 0.0601(14) Uani 1 1 d . . .
C13 C 0.6001(3) 0.86848(14) 0.4888(4) 0.0529(12) Uani 1 1 d . . .
H13 H 0.6416 0.8661 0.5383 0.080 Uiso 1 1 calc . . .
C14 C 0.5557(3) 0.83977(14) 0.4621(4) 0.0583(13) Uani 1 1 d . . .
H14 H 0.5690 0.8182 0.4919 0.080 Uiso 1 1 calc . . .
C16 C 0.0504(2) 0.79053(13) 0.1048(4) 0.0466(11) Uani 1 1 d . . .
C17 C 0.1103(2) 0.76941(12) 0.1246(3) 0.0381(10) Uani 1 1 d . . .
H17 H 0.1546 0.7789 0.1253 0.080 Uiso 1 1 calc . . .
C18 C 0.10430(18) 0.73376(12) 0.1435(3) 0.0315(9) Uani 1 1 d . . .
C19 C 0.03842(18) 0.71975(12) 0.1447(3) 0.0338(9) Uani 1 1 d . . .
H19 H 0.0346 0.6961 0.1589 0.080 Uiso 1 1 calc . . .
C20 C -0.02183(19) 0.74118(13) 0.1248(3) 0.0372(10) Uani 1 1 d . . .
C21 C -0.0156(2) 0.77687(14) 0.1054(3) 0.0439(11) Uani 1 1 d . . .
H21 H -0.0556 0.7914 0.0931 0.080 Uiso 1 1 calc . . .
C22 C 0.16725(18) 0.70982(11) 0.1548(3) 0.0293(8) Uani 1 1 d . . .
C23 C -0.0951(2) 0.72679(15) 0.1172(3) 0.0410(11) Uani 1 1 d . . .
C24 C 0.0641(3) 0.85314(17) 0.1272(5) 0.0638(15) Uani 1 1 d . . .
C25 C 0.0576(4) 0.88557(19) 0.0812(6) 0.085(2) Uani 1 1 d . . .
H25 H 0.0475 0.8867 0.0146 0.080 Uiso 1 1 calc . . .
C26 C 0.0661(4) 0.9153(2) 0.1335(9) 0.103(3) Uani 1 1 d . . .
H26 H 0.0602 0.9370 0.1026 0.080 Uiso 1 1 calc . . .
C27 C 0.0841(3) 0.9139(2) 0.2356(7) 0.080(2) Uani 1 1 d . . .
C28 C 0.0908(3) 0.8817(2) 0.2785(6) 0.082(2) Uani 1 1 d . . .
H28 H 0.1016 0.8803 0.3451 0.080 Uiso 1 1 calc . . .
C29 C 0.0818(3) 0.85077(16) 0.2246(6) 0.0670(16) Uani 1 1 d . . .
H29 H 0.0878 0.8290 0.2548 0.080 Uiso 1 1 calc . . .
C31 C 0.2417(2) 0.59753(12) -0.2488(3) 0.0431(10) Uani 1 1 d . . .
C32 C 0.2430(2) 0.61617(12) -0.1655(3) 0.0393(10) Uani 1 1 d . . .
H32 H 0.2468 0.6044 -0.1080 0.080 Uiso 1 1 calc . . .
C33 C 0.2387(2) 0.65233(11) -0.1689(3) 0.0336(9) Uani 1 1 d . . .
C34 C 0.2336(2) 0.66970(11) -0.2554(3) 0.0338(9) Uani 1 1 d . . .
H34 H 0.2307 0.6941 -0.2577 0.080 Uiso 1 1 calc . . .
C35 C 0.2329(2) 0.65089(12) -0.3388(3) 0.0359(9) Uani 1 1 d . . .
C36 C 0.2358(2) 0.61428(12) -0.3353(3) 0.0412(10) Uani 1 1 d . . .
H36 H 0.2337 0.6013 -0.3906 0.080 Uiso 1 1 calc . . .
C37 C 0.2433(2) 0.67320(11) -0.0789(3) 0.0325(9) Uani 1 1 d . . .
C38 C 0.2320(2) 0.67017(12) -0.4300(3) 0.0362(9) Uani 1 1 d . . .
C39 C 0.2057(3) 0.53631(15) -0.2637(4) 0.0564(13) Uani 1 1 d . . .
C40 C 0.1354(4) 0.54205(17) -0.3053(6) 0.0785(19) Uani 1 1 d . . .
H40 H 0.1186 0.5649 -0.3181 0.080 Uiso 1 1 calc . . .
C41 C 0.0880(4) 0.5138(2) -0.3292(6) 0.089(2) Uani 1 1 d . . .
H41 H 0.0396 0.5181 -0.3558 0.080 Uiso 1 1 calc . . .
C42 C 0.1122(4) 0.47987(17) -0.3138(5) 0.0712(17) Uani 1 1 d . . .
C43 C 0.1827(4) 0.47446(16) -0.2711(5) 0.0743(17) Uani 1 1 d . . .
H43 H 0.1993 0.4516 -0.2575 0.080 Uiso 1 1 calc . . .
C44 C 0.2302(4) 0.50212(15) -0.2474(5) 0.0666(16) Uani 1 1 d . . .
H44 H 0.2785 0.4978 -0.2205 0.080 Uiso 1 1 calc . . .


_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 O9 2.104(3) 8_566 ?
Mn1 O9 2.104(3) 2 ?
Mn1 O13 2.138(3) 7_565 ?
Mn1 O13 2.138(3) 1_556 ?
Mn1 O1 2.289(3) 7_566 ?
Mn1 O1 2.289(3) . ?
Mn2 O8 2.122(3) 2 ?
Mn2 O14 2.124(3) 1_556 ?
Mn2 O16 2.168(4) . ?
Mn2 O7 2.192(3) . ?
Mn2 O1 2.210(3) . ?
Mn3 O12 2.088(3) 7_565 ?
Mn3 O12 2.088(3) . ?
Mn3 O4 2.189(3) 2_655 ?
Mn3 O4 2.189(3) 8_465 ?
Mn3 O6 2.296(3) 7_565 ?
Mn3 O6 2.296(3) . ?
Mn4 O11 2.113(3) . ?
Mn4 O3 2.163(3) 2_655 ?
Mn4 O17 2.174(3) . ?
Mn4 O2 2.223(3) . ?
Mn4 O6 2.229(3) . ?
O1 C7 1.272(4) . ?
O2 C7 1.255(5) . ?
O3 C8 1.268(6) . ?
O3 Mn4 2.163(3) 2_655 ?
O4 C8 1.244(5) . ?
O4 Mn3 2.189(3) 2_655 ?
O5 C9 1.370(6) . ?
O5 C1 1.377(6) . ?
O6 C22 1.268(5) . ?
O7 C22 1.246(5) . ?
O8 C23 1.272(6) . ?
O8 Mn2 2.122(3) 2 ?
O9 C23 1.239(6) . ?
O9 Mn1 2.104(3) 2 ?
O10 C24 1.361(8) . ?
O10 C16 1.402(6) . ?
O11 C37 1.249(5) . ?
O12 C37 1.262(5) . ?
O13 C38 1.250(5) . ?
O13 Mn1 2.138(3) 1_554 ?
O14 C38 1.266(5) . ?
O14 Mn2 2.124(3) 1_554 ?
O15 C39 1.339(6) . ?
O15 C31 1.408(6) . ?
C15 N4 1.322(3) . ?
C15 N1 1.322(3) . ?
C15 C12 1.443(7) . ?
N1 N2 1.322(3) . ?
N2 N3 1.322(3) . ?
N2 N5 1.416(8) . ?
N3 N4 1.322(3) . ?
C30 N6 1.302(6) . ?
C30 N9 1.302(6) . ?
C30 C27 1.449(11) . ?
N6 N7 1.302(6) . ?
N7 N8 1.302(6) . ?
N7 N10 1.395(6) . ?
N8 N9 1.302(6) . ?
C45 N14 1.276(4) . ?
C45 N11 1.276(4) . ?
C45 C42 1.485(8) . ?
N11 N12 1.276(4) . ?
N12 N13 1.276(4) . ?
N12 N15 1.351(5) . ?
N13 N14 1.276(4) . ?
C1 C6 1.388(6) . ?
C1 C2 1.390(6) . ?
C2 C3 1.384(6) . ?
C3 C4 1.393(5) . ?
C3 C7 1.493(5) . ?
C4 C5 1.397(5) . ?
C5 C6 1.390(6) . ?
C5 C8 1.496(5) . ?
C9 C14 1.358(7) . ?
C9 C10 1.384(9) . ?
C10 C11 1.386(10) . ?
C11 C12 1.371(8) . ?
C12 C13 1.347(8) . ?
C13 C14 1.382(7) . ?
C16 C17 1.381(6) . ?
C16 C21 1.384(7) . ?
C17 C18 1.395(6) . ?
C18 C19 1.390(5) . ?
C18 C22 1.498(5) . ?
C19 C20 1.392(6) . ?
C20 C21 1.399(7) . ?
C20 C23 1.501(6) . ?
C24 C29 1.360(9) . ?
C24 C25 1.392(10) . ?
C25 C26 1.347(13) . ?
C26 C27 1.423(14) . ?
C27 C28 1.365(11) . ?
C28 C29 1.397(10) . ?
C31 C36 1.379(7) . ?
C31 C32 1.391(7) . ?
C32 C33 1.379(6) . ?
C33 C34 1.393(6) . ?
C33 C37 1.506(6) . ?
C34 C35 1.397(6) . ?
C35 C36 1.395(6) . ?
C35 C38 1.504(6) . ?
C39 C40 1.356(9) . ?
C39 C44 1.384(8) . ?
C40 C41 1.397(10) . ?
C41 C42 1.372(10) . ?
C42 C43 1.360(10) . ?
C43 C44 1.382(9) . ?

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 Mn1 O9 180.0(2) 8_566 2 ?
O9 Mn1 O13 92.59(13) 8_566 7_565 ?
O9 Mn1 O13 87.41(13) 2 7_565 ?
O9 Mn1 O13 87.41(13) 8_566 1_556 ?
O9 Mn1 O13 92.59(13) 2 1_556 ?
O13 Mn1 O13 180.000(1) 7_565 1_556 ?
O9 Mn1 O1 85.08(12) 8_566 7_566 ?
O9 Mn1 O1 94.92(12) 2 7_566 ?
O13 Mn1 O1 88.06(11) 7_565 7_566 ?
O13 Mn1 O1 91.94(11) 1_556 7_566 ?
O9 Mn1 O1 94.92(12) 8_566 . ?
O9 Mn1 O1 85.08(12) 2 . ?
O13 Mn1 O1 91.94(11) 7_565 . ?
O13 Mn1 O1 88.06(11) 1_556 . ?
O1 Mn1 O1 180.00(13) 7_566 . ?
O8 Mn2 O14 95.09(14) 2 1_556 ?
O8 Mn2 O16 117.11(17) 2 . ?
O14 Mn2 O16 81.19(14) 1_556 . ?
O8 Mn2 O7 91.40(12) 2 . ?
O14 Mn2 O7 164.17(13) 1_556 . ?
O16 Mn2 O7 83.00(14) . . ?
O8 Mn2 O1 110.22(13) 2 . ?
O14 Mn2 O1 95.15(13) 1_556 . ?
O16 Mn2 O1 132.68(15) . . ?
O7 Mn2 O1 96.12(11) . . ?
O12 Mn3 O12 180.00(10) 7_565 . ?
O12 Mn3 O4 88.38(12) 7_565 2_655 ?
O12 Mn3 O4 91.62(12) . 2_655 ?
O12 Mn3 O4 91.62(12) 7_565 8_465 ?
O12 Mn3 O4 88.38(12) . 8_465 ?
O4 Mn3 O4 180.00(18) 2_655 8_465 ?
O12 Mn3 O6 90.16(11) 7_565 7_565 ?
O12 Mn3 O6 89.84(11) . 7_565 ?
O4 Mn3 O6 103.65(12) 2_655 7_565 ?
O4 Mn3 O6 76.35(11) 8_465 7_565 ?
O12 Mn3 O6 89.84(11) 7_565 . ?
O12 Mn3 O6 90.16(11) . . ?
O4 Mn3 O6 76.35(11) 2_655 . ?
O4 Mn3 O6 103.65(11) 8_465 . ?
O6 Mn3 O6 180.0 7_565 . ?
O11 Mn4 O3 95.68(13) . 2_655 ?
O11 Mn4 O17 82.54(12) . . ?
O3 Mn4 O17 103.27(14) 2_655 . ?
O11 Mn4 O2 164.72(12) . . ?
O3 Mn4 O2 90.41(11) 2_655 . ?
O17 Mn4 O2 82.43(12) . . ?
O11 Mn4 O6 92.36(12) . . ?
O3 Mn4 O6 122.49(12) 2_655 . ?
O17 Mn4 O6 134.24(12) . . ?
O2 Mn4 O6 96.17(11) . . ?
C7 O1 Mn2 104.3(2) . . ?
C7 O1 Mn1 149.1(2) . . ?
Mn2 O1 Mn1 104.25(11) . . ?
C7 O2 Mn4 124.9(3) . . ?
C8 O3 Mn4 102.2(2) . 2_655 ?
C8 O4 Mn3 164.8(3) . 2_655 ?
C9 O5 C1 125.4(3) . . ?
C22 O6 Mn4 105.5(3) . . ?
C22 O6 Mn3 147.8(2) . . ?
Mn4 O6 Mn3 102.83(10) . . ?
C22 O7 Mn2 127.3(3) . . ?
C23 O8 Mn2 119.1(3) . 2 ?
C23 O9 Mn1 140.6(3) . 2 ?
C24 O10 C16 121.4(5) . . ?
C37 O11 Mn4 132.5(3) . . ?
C37 O12 Mn3 136.7(3) . . ?
C38 O13 Mn1 145.9(3) . 1_554 ?
C38 O14 Mn2 122.4(3) . 1_554 ?
C39 O15 C31 124.1(4) . . ?
N4 C15 N1 108.0 . . ?
N4 C15 C12 127.2(3) . . ?
N1 C15 C12 124.8(3) . . ?
C15 N1 N2 108.0 . . ?
N1 N2 N3 108.0 . . ?
N1 N2 N5 126.1(5) . . ?
N3 N2 N5 125.7(5) . . ?
N4 N3 N2 108.0 . . ?
N3 N4 C15 108.0 . . ?
N6 C30 N9 108.0 . . ?
N6 C30 C27 126.6(7) . . ?
N9 C30 C27 125.4(7) . . ?
C30 N6 N7 108.0 . . ?
N8 N7 N6 108.0 . . ?
N8 N7 N10 106.6 . . ?
N6 N7 N10 145.2 . . ?
N7 N8 N9 108.0 . . ?
C30 N9 N8 108.0 . . ?
N14 C45 N11 108.0 . . ?
N14 C45 C42 126.1(5) . . ?
N11 C45 C42 125.9(5) . . ?
N12 N11 C45 108.0 . . ?
N11 N12 N13 108.0 . . ?
N11 N12 N15 143.2 . . ?
N13 N12 N15 108.3 . . ?
N12 N13 N14 108.0 . . ?
C45 N14 N13 108.0 . . ?
O5 C1 C6 125.5(4) . . ?
O5 C1 C2 113.7(4) . . ?
C6 C1 C2 120.6(4) . . ?
C3 C2 C1 119.5(4) . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 C7 118.8(3) . . ?
C4 C3 C7 120.1(4) . . ?
C3 C4 C5 118.5(4) . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 C8 118.3(3) . . ?
C4 C5 C8 120.6(4) . . ?
C1 C6 C5 119.1(4) . . ?
O2 C7 O1 119.9(3) . . ?
O2 C7 C3 119.9(3) . . ?
O1 C7 C3 120.2(3) . . ?
O4 C8 O3 121.1(4) . . ?
O4 C8 C5 118.9(4) . . ?
O3 C8 C5 119.9(3) . . ?
C14 C9 O5 128.0(5) . . ?
C14 C9 C10 117.9(5) . . ?
O5 C9 C10 114.1(5) . . ?
C9 C10 C11 120.2(5) . . ?
C12 C11 C10 121.1(6) . . ?
C13 C12 C11 117.9(5) . . ?
C13 C12 C15 120.7(5) . . ?
C11 C12 C15 121.4(5) . . ?
C12 C13 C14 121.7(5) . . ?
C9 C14 C13 121.1(5) . . ?
C17 C16 C21 120.7(4) . . ?
C17 C16 O10 118.4(4) . . ?
C21 C16 O10 120.1(4) . . ?
C16 C17 C18 119.8(4) . . ?
C19 C18 C17 120.0(4) . . ?
C19 C18 C22 119.5(4) . . ?
C17 C18 C22 120.3(3) . . ?
C18 C19 C20 119.9(4) . . ?
C19 C20 C21 119.9(4) . . ?
C19 C20 C23 121.9(4) . . ?
C21 C20 C23 118.1(4) . . ?
C16 C21 C20 119.7(4) . . ?
O7 C22 O6 120.8(3) . . ?
O7 C22 C18 120.5(3) . . ?
O6 C22 C18 118.7(4) . . ?
O9 C23 O8 124.7(4) . . ?
O9 C23 C20 117.8(5) . . ?
O8 C23 C20 117.5(4) . . ?
C29 C24 O10 122.7(6) . . ?
C29 C24 C25 121.2(7) . . ?
O10 C24 C25 116.0(7) . . ?
C26 C25 C24 119.7(8) . . ?
C25 C26 C27 120.7(7) . . ?
C28 C27 C26 118.1(7) . . ?
C28 C27 C30 122.2(9) . . ?
C26 C27 C30 119.7(8) . . ?
C27 C28 C29 121.5(8) . . ?
C24 C29 C28 118.8(7) . . ?
C36 C31 C32 121.7(4) . . ?
C36 C31 O15 120.3(4) . . ?
C32 C31 O15 117.6(4) . . ?
C33 C32 C31 119.4(4) . . ?
C32 C33 C34 119.7(4) . . ?
C32 C33 C37 120.4(4) . . ?
C34 C33 C37 119.8(4) . . ?
C33 C34 C35 120.7(4) . . ?
C36 C35 C34 119.3(4) . . ?
C36 C35 C38 120.7(4) . . ?
C34 C35 C38 120.0(4) . . ?
C31 C36 C35 119.2(4) . . ?
O11 C37 O12 125.9(4) . . ?
O11 C37 C33 117.4(4) . . ?
O12 C37 C33 116.7(4) . . ?
O13 C38 O14 125.0(4) . . ?
O13 C38 C35 117.6(4) . . ?
O14 C38 C35 117.4(4) . . ?
O15 C39 C40 125.4(5) . . ?
O15 C39 C44 115.4(5) . . ?
C40 C39 C44 119.1(5) . . ?
C39 C40 C41 120.3(6) . . ?
C42 C41 C40 120.7(6) . . ?
C43 C42 C41 118.4(6) . . ?
C43 C42 C45 117.9(6) . . ?
C41 C42 C45 123.6(6) . . ?
C42 C43 C44 121.5(6) . . ?
C43 C44 C39 119.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.078
_database_code_depnum_ccdc_archive 'CCDC 972185'

data_sad

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C30 H19 Cu3 N10 O12'
_chemical_formula_sum            'C30 H19 Cu3 N10 O12'
_chemical_formula_weight         902.17

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                   9.976(2)
_cell_length_b                   9.999(2)
_cell_length_c                   17.099(3)
_cell_angle_alpha                85.38(3)
_cell_angle_beta                 75.37(3)
_cell_angle_gamma                84.31(3)
_cell_volume                     1639.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7333
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16088
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7333
_reflns_number_gt                5602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0582P)²+2.5019P] 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         7333
_refine_ls_number_parameters     526
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.63887(4) 0.74442(5) 0.51639(3) 0.02622(13) Uani 1 1 d . . .
Cu2 Cu 0.49127(4) 0.56883(4) 0.40568(2) 0.02322(12) Uani 1 1 d . . .
Cu3 Cu 0.34716(4) 0.40522(5) 0.29391(3) 0.02842(13) Uani 1 1 d . . .
O1 O 0.3481(3) 0.6734(3) 0.48404(17) 0.0351(7) Uani 1 1 d . . .
O2 O 0.4456(2) 0.8111(3) 0.54712(16) 0.0317(6) Uani 1 1 d . . .
O3 O -0.2902(3) 0.8460(3) 0.59430(18) 0.0386(7) Uani 1 1 d . . .
O4 O -0.1534(3) 0.7423(3) 0.49400(17) 0.0368(7) Uani 1 1 d . . .
O5 O 0.0281(3) 1.1168(3) 0.68978(18) 0.0392(7) Uani 1 1 d . . .
O6 O 0.2801(2) 0.3288(3) 0.20601(16) 0.0338(6) Uani 1 1 d . . .
O7 O 0.1393(3) 0.4167(3) 0.31077(16) 0.0329(6) Uani 1 1 d . . .
O8 O -0.3625(3) 0.4558(3) 0.33561(16) 0.0340(6) Uani 1 1 d . . .
O9 O -0.4573(2) 0.3585(3) 0.25053(16) 0.0317(6) Uani 1 1 d . . .
O10 O -0.0201(3) 0.2187(3) 0.03015(16) 0.0385(7) Uani 1 1 d . . .
O11 O 0.6347(3) 0.6675(3) 0.42049(17) 0.0386(7) Uani 1 1 d . . .
O12 O 0.3512(2) 0.4517(3) 0.40031(14) 0.0250(5) Uani 1 1 d . . .
N1 N 0.3688(4) 1.1481(5) 0.9636(2) 0.0516(10) Uani 1 1 d D . .
N2 N 0.4172(5) 1.2303(6) 1.0079(3) 0.0635(13) Uani 1 1 d D . .
N3 N 0.3876(6) 1.3590(6) 0.9908(3) 0.0754(15) Uani 1 1 d D . .
N4 N 0.3154(5) 1.3630(5) 0.9341(3) 0.0592(12) Uani 1 1 d . . .
N5 N 0.4947(7) 1.1850(7) 1.0667(4) 0.104(2) Uani 1 1 d DU . .
N6 N -0.3751(4) 0.1268(3) -0.2212(2) 0.0339(7) Uani 1 1 d . . .
N7 N -0.4356(4) 0.1695(4) -0.2804(2) 0.0394(8) Uani 1 1 d D . .
N8 N -0.4345(4) 0.3018(4) -0.2950(2) 0.0411(9) Uani 1 1 d . . .
N9 N -0.3728(3) 0.3484(3) -0.24359(19) 0.0315(7) Uani 1 1 d . . .
N10 N -0.4885(6) 0.0823(5) -0.3262(3) 0.0692(14) Uani 1 1 d D . .
C1 C 0.2031(3) 0.8398(4) 0.5613(2) 0.0225(7) Uani 1 1 d . . .
C2 C 0.1876(3) 0.9459(4) 0.6117(2) 0.0261(8) Uani 1 1 d . . .
H2 H 0.2649 0.9766 0.6234 0.080 Uiso 1 1 calc . . .
C3 C 0.0560(4) 1.0051(4) 0.6440(2) 0.0286(8) Uani 1 1 d . . .
C4 C -0.0608(4) 0.9599(4) 0.6270(2) 0.0298(8) Uani 1 1 d . . .
H4 H -0.1490 0.9985 0.6506 0.080 Uiso 1 1 calc . . .
C5 C -0.0447(3) 0.8576(4) 0.5750(2) 0.0257(7) Uani 1 1 d . . .
C6 C 0.0874(4) 0.7966(4) 0.5415(2) 0.0253(7) Uani 1 1 d . . .
H6 H 0.0982 0.7280 0.5062 0.080 Uiso 1 1 calc . . .
C7 C 0.3440(4) 0.7687(4) 0.5281(2) 0.0248(7) Uani 1 1 d . . .
C8 C -0.1685(4) 0.8130(4) 0.5535(2) 0.0277(8) Uani 1 1 d . . .
C9 C 0.1042(4) 1.1374(4) 0.7445(2) 0.0280(8) Uani 1 1 d . . .
C10 C 0.1661(5) 1.0352(4) 0.7856(3) 0.0373(9) Uani 1 1 d . . .
H10 H 0.1637 0.9459 0.7749 0.080 Uiso 1 1 calc . . .
C11 C 0.2320(5) 1.0668(4) 0.8431(3) 0.0397(10) Uani 1 1 d . . .
H11 H 0.2732 0.9980 0.8713 0.080 Uiso 1 1 calc . . .
C12 C 0.2376(4) 1.1999(4) 0.8592(2) 0.0333(9) Uani 1 1 d . . .
C13 C 0.1736(5) 1.3005(4) 0.8174(3) 0.0401(10) Uani 1 1 d . . .
H13 H 0.1753 1.3900 0.8280 0.080 Uiso 1 1 calc . . .
C14 C 0.1071(4) 1.2697(4) 0.7600(2) 0.0352(9) Uani 1 1 d . . .
H14 H 0.0647 1.3380 0.7321 0.080 Uiso 1 1 calc . . .
C15 C 0.3081(5) 1.2368(5) 0.9190(3) 0.0414(10) Uani 1 1 d . . .
C16 C 0.0351(3) 0.3367(4) 0.2127(2) 0.0221(7) Uani 1 1 d . . .
C17 C -0.0985(3) 0.3669(4) 0.2582(2) 0.0210(7) Uani 1 1 d . . .
H17 H -0.1134 0.3978 0.3098 0.080 Uiso 1 1 calc . . .
C18 C -0.2117(3) 0.3508(3) 0.2259(2) 0.0197(6) Uani 1 1 d . . .
C19 C -0.1900(3) 0.3048(4) 0.1484(2) 0.0229(7) Uani 1 1 d . . .
H19 H -0.2648 0.2948 0.1267 0.080 Uiso 1 1 calc . . .
C20 C -0.0548(4) 0.2742(4) 0.1043(2) 0.0256(7) Uani 1 1 d . . .
C21 C 0.0583(3) 0.2893(4) 0.1358(2) 0.0255(7) Uani 1 1 d . . .
H21 H 0.1484 0.2680 0.1057 0.080 Uiso 1 1 calc . . .
C22 C 0.1570(3) 0.3610(4) 0.2446(2) 0.0249(7) Uani 1 1 d . . .
C23 C -0.3560(3) 0.3910(4) 0.2749(2) 0.0233(7) Uani 1 1 d . . .
C24 C -0.1115(4) 0.2304(4) -0.0206(2) 0.0283(8) Uani 1 1 d . . .
C25 C -0.1721(5) 0.3513(4) -0.0429(2) 0.0372(9) Uani 1 1 d . . .
H25 H -0.1618 0.4295 -0.0197 0.080 Uiso 1 1 calc . . .
C26 C -0.2499(4) 0.3564(4) -0.1010(2) 0.0360(9) Uani 1 1 d . . .
H26 H -0.2934 0.4376 -0.1158 0.080 Uiso 1 1 calc . . .
C27 C -0.2615(4) 0.2393(4) -0.1363(2) 0.0278(8) Uani 1 1 d . . .
C28 C -0.2023(4) 0.1174(4) -0.1109(3) 0.0350(9) Uani 1 1 d . . .
H28 H -0.2133 0.0383 -0.1329 0.080 Uiso 1 1 calc . . .
C29 C -0.1267(4) 0.1131(4) -0.0528(2) 0.0332(9) Uani 1 1 d . . .
H29 H -0.0867 0.0315 -0.0358 0.080 Uiso 1 1 calc . . .
C30 C -0.3372(4) 0.2400(4) -0.2005(2) 0.0283(8) Uani 1 1 d . . .
O1W O 0.9117(14) 0.5182(15) 0.4336(10) 0.116(5) Uani 0.40 1 d P . .
O1W' O 1.053(4) 0.531(5) 0.453(3) 0.10(2) Uani 0.10 1 d P . .
H10B H -0.564(5) 0.130(6) -0.352(3) 0.080 Uiso 1 1 d D . .
H10A H -0.426(5) 0.050(6) -0.379(2) 0.080 Uiso 1 1 d D . .
H5A H 0.455(5) 1.100(4) 1.097(2) 0.080 Uiso 1 1 d D . .
H5B H 0.508(5) 1.220(3) 1.1205(19) 0.080 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 O11 1.878(3) . ?
Cu1 O2 1.931(2) . ?
Cu1 O4 2.008(3) 1_655 ?
Cu1 O3 2.035(3) 1_655 ?
Cu1 O12 2.338(3) 2_666 ?
Cu1 C8 2.348(3) 1_655 ?
Cu2 O11 1.894(3) . ?
Cu2 O12 1.934(2) . ?
Cu2 O8 1.962(3) 1_655 ?
Cu2 O1 1.973(3) . ?
Cu2 N8 2.361(4) 2_565 ?
Cu3 O12 1.925(2) . ?
Cu3 O9 1.929(2) 1_655 ?
Cu3 O7 2.013(2) . ?
Cu3 O6 2.021(3) . ?
Cu3 C22 2.353(3) . ?
O1 C7 1.252(4) . ?
O2 C7 1.261(4) . ?
O3 C8 1.265(4) . ?
O3 Cu1 2.035(3) 1_455 ?
O4 C8 1.255(4) . ?
O4 Cu1 2.008(3) 1_455 ?
O5 C3 1.380(4) . ?
O5 C9 1.384(5) . ?
O6 C22 1.263(4) . ?
O7 C22 1.265(4) . ?
O8 C23 1.252(4) . ?
O8 Cu2 1.962(3) 1_455 ?
O9 C23 1.265(4) . ?
O9 Cu3 1.929(2) 1_455 ?
O10 C20 1.374(4) . ?
O10 C24 1.401(4) . ?
O12 Cu1 2.338(3) 2_666 ?
N1 C15 1.324(6) . ?
N1 N2 1.359(6) . ?
N2 N3 1.318(7) . ?
N2 N5 1.436(4) . ?
N3 N4 1.343(6) . ?
N4 C15 1.321(6) . ?
N5 H5A 1.022(19) . ?
N5 H5B 1.055(18) . ?
N6 N7 1.326(5) . ?
N6 C30 1.330(5) . ?
N7 N8 1.327(5) . ?
N7 N10 1.435(4) . ?
N8 N9 1.329(5) . ?
N8 Cu2 2.361(4) 2_565 ?
N9 C30 1.331(5) . ?
N10 H10B 1.03(2) . ?
N10 H10A 1.02(2) . ?
C1 C2 1.392(5) . ?
C1 C6 1.398(5) . ?
C1 C7 1.506(5) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(5) . ?
C4 C5 1.381(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(5) . ?
C5 C8 1.491(5) . ?
C6 H6 0.9300 . ?
C8 Cu1 2.348(3) 1_455 ?
C9 C14 1.374(5) . ?
C9 C10 1.378(6) . ?
C10 C11 1.383(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.385(6) . ?
C12 C15 1.466(6) . ?
C13 C14 1.385(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C17 1.381(5) . ?
C16 C21 1.391(5) . ?
C16 C22 1.501(4) . ?
C17 C18 1.404(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.396(5) . ?
C18 C23 1.505(5) . ?
C19 C20 1.387(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.392(5) . ?
C21 H21 0.9300 . ?
C24 C25 1.368(6) . ?
C24 C29 1.372(5) . ?
C25 C26 1.402(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.388(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(5) . ?
C27 C30 1.479(5) . ?
C28 C29 1.387(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
O1W O1W' 1.54(4) . ?
O1W' O1W' 1.79(12) 2_766 ?

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
O11 Cu1 O2 97.59(12) . . ?
O11 Cu1 O4 96.51(11) . 1_655 ?
O2 Cu1 O4 159.39(12) . 1_655 ?
O11 Cu1 O3 159.36(12) . 1_655 ?
O2 Cu1 O3 98.39(11) . 1_655 ?
O4 Cu1 O3 64.85(11) 1_655 1_655 ?
O11 Cu1 O12 99.37(12) . 2_666 ?
O2 Cu1 O12 103.52(11) . 2_666 ?
O4 Cu1 O12 88.89(11) 1_655 2_666 ?
O3 Cu1 O12 89.49(11) 1_655 2_666 ?
O11 Cu1 C8 128.24(13) . 1_655 ?
O2 Cu1 C8 129.91(12) . 1_655 ?
O4 Cu1 C8 32.29(12) 1_655 1_655 ?
O3 Cu1 C8 32.56(12) 1_655 1_655 ?
O12 Cu1 C8 89.30(12) 2_666 1_655 ?
O11 Cu2 O12 172.87(12) . . ?
O11 Cu2 O8 87.01(12) . 1_655 ?
O12 Cu2 O8 91.61(11) . 1_655 ?
O11 Cu2 O1 92.21(11) . . ?
O12 Cu2 O1 88.58(11) . . ?
O8 Cu2 O1 175.13(12) 1_655 . ?
O11 Cu2 N8 99.39(14) . 2_565 ?
O12 Cu2 N8 87.67(12) . 2_565 ?
O8 Cu2 N8 93.09(13) 1_655 2_565 ?
O1 Cu2 N8 91.78(13) . 2_565 ?
O12 Cu3 O9 99.41(11) . 1_655 ?
O12 Cu3 O7 97.77(11) . . ?
O9 Cu3 O7 161.51(11) 1_655 . ?
O12 Cu3 O6 159.42(11) . . ?
O9 Cu3 O6 96.81(10) 1_655 . ?
O7 Cu3 O6 64.96(10) . . ?
O12 Cu3 C22 129.50(11) . . ?
O9 Cu3 C22 129.20(11) 1_655 . ?
O7 Cu3 C22 32.52(11) . . ?
O6 Cu3 C22 32.44(11) . . ?
C7 O1 Cu2 137.0(2) . . ?
C7 O2 Cu1 128.1(2) . . ?
C8 O3 Cu1 87.4(2) . 1_455 ?
C8 O4 Cu1 88.9(2) . 1_455 ?
C3 O5 C9 122.0(3) . . ?
C22 O6 Cu3 88.4(2) . . ?
C22 O7 Cu3 88.7(2) . . ?
C23 O8 Cu2 134.6(2) . 1_455 ?
C23 O9 Cu3 128.2(2) . 1_455 ?
C20 O10 C24 121.9(3) . . ?
Cu1 O11 Cu2 125.94(15) . . ?
Cu3 O12 Cu2 116.41(13) . . ?
Cu3 O12 Cu1 109.56(11) . 2_666 ?
Cu2 O12 Cu1 111.59(11) . 2_666 ?
C15 N1 N2 101.3(4) . . ?
N3 N2 N1 112.9(4) . . ?
N3 N2 N5 122.3(5) . . ?
N1 N2 N5 124.8(5) . . ?
N2 N3 N4 105.7(4) . . ?
C15 N4 N3 106.5(5) . . ?
N2 N5 H5A 108.6(16) . . ?
N2 N5 H5B 136.4(19) . . ?
H5A N5 H5B 91.1(17) . . ?
N7 N6 C30 102.7(3) . . ?
N6 N7 N8 111.7(3) . . ?
N6 N7 N10 124.1(4) . . ?
N8 N7 N10 124.1(4) . . ?
N7 N8 N9 107.6(3) . . ?
N7 N8 Cu2 127.5(3) . 2_565 ?
N9 N8 Cu2 124.0(3) . 2_565 ?
N8 N9 C30 105.0(3) . . ?
N7 N10 H10B 113(4) . . ?
N7 N10 H10A 119(4) . . ?
H10B N10 H10A 95(5) . . ?
C2 C1 C6 120.3(3) . . ?
C2 C1 C7 120.8(3) . . ?
C6 C1 C7 118.9(3) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
O5 C3 C2 124.7(3) . . ?
O5 C3 C4 114.2(3) . . ?
C2 C3 C4 120.9(3) . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 C8 119.9(3) . . ?
C6 C5 C8 119.7(3) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
O1 C7 O2 126.6(3) . . ?
O1 C7 C1 116.5(3) . . ?
O2 C7 C1 116.9(3) . . ?
O4 C8 O3 118.8(3) . . ?
O4 C8 C5 120.3(3) . . ?
O3 C8 C5 120.9(3) . . ?
O4 C8 Cu1 58.77(18) . 1_455 ?
O3 C8 Cu1 59.99(18) . 1_455 ?
C5 C8 Cu1 178.6(3) . 1_455 ?
C14 C9 C10 120.9(4) . . ?
C14 C9 O5 115.0(3) . . ?
C10 C9 O5 124.0(3) . . ?
C9 C10 C11 119.3(4) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.4(4) . . ?
C13 C12 C15 119.3(4) . . ?
C11 C12 C15 122.3(4) . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C9 C14 C13 119.5(4) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
N4 C15 N1 113.5(4) . . ?
N4 C15 C12 122.7(4) . . ?
N1 C15 C12 123.8(4) . . ?
C17 C16 C21 120.6(3) . . ?
C17 C16 C22 120.0(3) . . ?
C21 C16 C22 119.3(3) . . ?
C16 C17 C18 119.6(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 C23 120.9(3) . . ?
C17 C18 C23 118.6(3) . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
O10 C20 C19 124.3(3) . . ?
O10 C20 C21 114.3(3) . . ?
C19 C20 C21 121.3(3) . . ?
C16 C21 C20 119.3(3) . . ?
C16 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
O6 C22 O7 117.9(3) . . ?
O6 C22 C16 121.3(3) . . ?
O7 C22 C16 120.7(3) . . ?
O6 C22 Cu3 59.14(17) . . ?
O7 C22 Cu3 58.77(17) . . ?
C16 C22 Cu3 178.5(3) . . ?
O8 C23 O9 126.7(3) . . ?
O8 C23 C18 115.6(3) . . ?
O9 C23 C18 117.7(3) . . ?
C25 C24 C29 121.6(3) . . ?
C25 C24 O10 122.9(4) . . ?
C29 C24 O10 115.3(3) . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C27 C26 C25 119.5(4) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 119.8(3) . . ?
C28 C27 C30 118.5(3) . . ?
C26 C27 C30 121.7(4) . . ?
C29 C28 C27 120.2(4) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C24 C29 C28 119.4(4) . . ?
C24 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
N6 C30 N9 113.1(3) . . ?
N6 C30 C27 121.3(3) . . ?
N9 C30 C27 125.6(4) . . ?
O1W O1W' O1W' 76(2) . 2_766 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10B O11 1.03(2) 2.39(4) 3.287(6) 145(5) 2_565
N10 H10A O3 1.02(2) 2.34(5) 3.095(6) 130(5) 1_544
N5 H5B O6 1.055(18) 2.56(5) 3.113(8) 112(3) 1_566

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 972186'
