# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Katherine Franz'
_publ_contact_author_email       KATHERINE.FRANZ@DUKE.EDU

_publ_section_title              
;
Toward the Development of Prochelators as Fluorescent
Probes of Copper-Mediated Oxidative Stress
;
loop_
_publ_author_name
'Katherine Franz'
'Marina G. Dickens'
'Lynne M. Hyman'
'Ken Shimizu'
'Clifton J. Stephenson'

#===END

data_monoc
_database_code_depnum_ccdc_archive 'CCDC 740843'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            CuFlamS
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C54 H34 Cl1.72 Cu2 N4 O10), '
_chemical_formula_sum            'C27 H17.5 Cl Cu N2 Na0.5 O5.5'
_chemical_formula_weight         565.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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 '
_symmetry_space_group_name_Hall  '-C 2yc'

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                   17.948(3)
_cell_length_b                   36.076(6)
_cell_length_c                   17.331(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.278(6)
_cell_angle_gamma                90.00
_cell_volume                     9691(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      23.86

_exptl_crystal_description       'faceted prism'
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4604
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_T_max  0.8318
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            34579
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         23.96
_reflns_number_total             6948
_reflns_number_gt                4691
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Apex II 2.0 Rev.2 (Bruker, 2005)'
_computing_cell_refinement       SAINT
_computing_data_reduction        'SAINT 7.12A (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'

_refine_special_details          
;
One batch of data was excluded in this solution to improve the resolution
of the disordered ions and solvent. This does not affect the final solution,
as the main residue has higher symmetry and needs less data to solve
satisfactorily.

No suitable hydrogen bonds were calculated.

The asymmetric unit consists of one [Cu2Cl(FlamS)2]Cl unit, where the
outer-sphere chloride appears at two positions at half occupancy,
both of which are disordered over two positions with refined populations
of 0.3/0.2 and 0.35/0.15. There is also a NaOH with the Na at half
occupancy and a disordered water molecule. The solvent and counterions
contain a significant amount of disorder, which leads to the higher R value.
It should be noted that the main residue contains only 1 % disorder,
which is due to the flexion of the xanthene ring.The significant disorder
in the water molecule prevented the proper affixing of hydrogen atoms,
leading to an incomplete connection. It also has an usual occupancy which
leads to non-integer values for atoms in the cell.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6948
_refine_ls_number_parameters     701
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.1942
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.004

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 0.05990(5) 0.06559(2) 0.84547(5) 0.0402(3) Uani 1 1 d . . .
Cu2 Cu 0.03666(6) 0.18511(3) 0.84738(5) 0.0504(3) Uani 1 1 d . . .
Cl1 Cl 0.09221(10) 0.12593(4) 0.93130(9) 0.0341(4) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.01473(9) 1.2500 0.0445(8) Uani 0.35 1 d P A 1
Cl2A Cl 0.0521(12) 0.0183(4) 1.3338(18) 0.097(7) Uani 0.15 1 d P B 2
Cl3 Cl 0.5000 0.23005(17) 1.2500 0.0607(19) Uani 0.20 1 d P C 1
Cl3A Cl 0.4678(4) 0.22975(14) 1.1561(4) 0.0412(12) Uani 0.30 1 d P D 2
N1 N 0.2073(3) 0.04563(14) 0.9936(3) 0.0346(12) Uani 1 1 d . . .
N1A N 0.0405(4) 0.20381(16) 1.0017(3) 0.0425(13) Uani 1 1 d . . .
N2 N 0.1820(3) 0.05501(13) 0.9078(3) 0.0307(11) Uani 1 1 d . . .
N2A N -0.0214(4) 0.19479(15) 0.9140(3) 0.0391(13) Uani 1 1 d . . .
O1A O -0.1143(3) 0.08277(16) 1.1521(4) 0.0655(15) Uani 1 1 d . . .
H1AA H -0.1571 0.0894 1.1562 0.098 Uiso 1 1 calc R . .
O1 O 0.4414(4) -0.08934(17) 1.0065(4) 0.0810(19) Uani 1 1 d . . .
H1A H 0.4943 -0.0855 1.0268 0.122 Uiso 1 1 calc R . .
O2 O 0.4731(3) 0.03135(15) 1.1133(4) 0.0666(16) Uani 1 1 d . . .
O2A O -0.1314(4) 0.20772(18) 1.0883(4) 0.085(2) Uani 1 1 d . . .
O3 O 0.5244(4) 0.15945(15) 1.1560(4) 0.0661(15) Uani 1 1 d . . .
H3A H 0.5731 0.1511 1.1691 0.099 Uiso 1 1 calc R . .
O3B O -0.1723(7) 0.3363(3) 1.0417(11) 0.206(7) Uani 1 1 d . . .
H3BA H -0.2131 0.3299 1.0494 0.309 Uiso 1 1 calc R . .
O4A O 0.1403(3) 0.20988(13) 0.9578(3) 0.0460(12) Uani 1 1 d . . .
O4 O 0.0664(3) 0.04159(11) 0.9553(3) 0.0355(10) Uani 1 1 d . . .
O5A O -0.0750(3) 0.18193(11) 0.7378(3) 0.0365(10) Uani 1 1 d . . .
O5 O 0.0612(3) 0.07177(11) 0.7348(2) 0.0324(9) Uani 1 1 d . . .
C1A C 0.0266(4) 0.1401(2) 1.1084(4) 0.0448(17) Uani 1 1 d . . .
H1AB H 0.0765 0.1374 1.1032 0.054 Uiso 1 1 calc R . .
C1 C 0.2830(5) -0.02704(19) 1.0066(5) 0.0479(17) Uani 1 1 d . . .
H1B H 0.2231 -0.0264 0.9868 0.058 Uiso 1 1 calc R . .
C2 C 0.3166(5) -0.0580(2) 0.9924(5) 0.057(2) Uani 1 1 d . . .
H2A H 0.2814 -0.0790 0.9644 0.068 Uiso 1 1 calc R . .
C2A C -0.0063(5) 0.1093(2) 1.1258(5) 0.0526(19) Uani 1 1 d . . .
H2AA H 0.0196 0.0858 1.1315 0.063 Uiso 1 1 calc R . .
C3A C -0.0792(5) 0.1130(2) 1.1351(5) 0.055(2) Uani 1 1 d . . .
C3 C 0.4045(6) -0.0583(2) 1.0200(5) 0.060(2) Uani 1 1 d . . .
C4A C -0.1183(5) 0.1450(3) 1.1218(5) 0.065(2) Uani 1 1 d . . .
H4AA H -0.1693 0.1469 1.1252 0.078 Uiso 1 1 calc R . .
C4 C 0.4553(5) -0.0294(2) 1.0602(5) 0.058(2) Uani 1 1 d . . .
H4A H 0.5149 -0.0302 1.0787 0.069 Uiso 1 1 calc R . .
C5 C 0.4190(4) 0.00218(19) 1.0746(4) 0.0461(17) Uani 1 1 d . . .
C5A C -0.0850(5) 0.1763(2) 1.1027(5) 0.057(2) Uani 1 1 d . . .
C6A C -0.0093(4) 0.17559(19) 1.0978(4) 0.0408(16) Uani 1 1 d . . .
C6 C 0.3327(4) 0.00389(17) 1.0489(4) 0.0357(14) Uani 1 1 d . . .
C7 C 0.2959(4) 0.03796(16) 1.0690(4) 0.0339(14) Uani 1 1 d . . .
C7A C 0.0291(4) 0.20863(18) 1.0812(4) 0.0390(15) Uani 1 1 d . . .
C8 C 0.3545(4) 0.07114(17) 1.0899(4) 0.0344(14) Uani 1 1 d . . .
C8A C -0.0270(5) 0.2428(2) 1.0675(4) 0.0459(17) Uani 1 1 d . . .
C9 C 0.3272(4) 0.10717(18) 1.0886(4) 0.0435(16) Uani 1 1 d . . .
H9A H 0.2686 0.1116 1.0712 0.052 Uiso 1 1 calc R . .
C9A C -0.0048(6) 0.2765(3) 1.0484(6) 0.076(3) Uani 1 1 d . . .
H9AA H 0.0442 0.2784 1.0413 0.091 Uiso 1 1 calc R . .
C10 C 0.3829(5) 0.13680(18) 1.1120(4) 0.0442(17) Uani 1 1 d . . .
H10A H 0.3629 0.1612 1.1118 0.053 Uiso 1 1 calc R . .
C10A C -0.0521(7) 0.3075(3) 1.0397(9) 0.100(4) Uani 1 1 d . . .
H10B H -0.0355 0.3307 1.0272 0.120 Uiso 1 1 calc R . .
C11 C 0.4683(5) 0.1309(2) 1.1359(5) 0.0480(17) Uani 1 1 d . . .
C11A C -0.1230(8) 0.3054(3) 1.0488(10) 0.111(4) Uani 1 1 d . . .
C12 C 0.4964(5) 0.0956(2) 1.1382(5) 0.058(2) Uani 1 1 d . . .
H12A H 0.5553 0.0912 1.1568 0.069 Uiso 1 1 calc R . .
C12A C -0.1483(6) 0.2729(3) 1.0656(6) 0.078(3) Uani 1 1 d . . .
H12B H -0.1984 0.2715 1.0710 0.093 Uiso 1 1 calc R . .
C13 C 0.4391(4) 0.06555(19) 1.1133(4) 0.0451(17) Uani 1 1 d . . .
C13A C -0.0989(6) 0.2405(2) 1.0753(5) 0.060(2) Uani 1 1 d . . .
C14 C 0.2732(4) 0.03067(17) 1.1417(4) 0.0374(15) Uani 1 1 d . . .
C14A C 0.1222(5) 0.21534(17) 1.1503(4) 0.0441(17) Uani 1 1 d . . .
C15A C 0.1574(5) 0.2191(2) 1.2423(4) 0.054(2) Uani 1 1 d . . .
H15A H 0.1224 0.2180 1.2690 0.065 Uiso 1 1 calc R . .
C15 C 0.3292(4) 0.02484(18) 1.2316(4) 0.0405(16) Uani 1 1 d . . .
H15B H 0.3899 0.0246 1.2559 0.049 Uiso 1 1 calc R . .
C16A C 0.2451(6) 0.2244(2) 1.2926(5) 0.062(2) Uani 1 1 d . . .
H16A H 0.2709 0.2267 1.3555 0.075 Uiso 1 1 calc R . .
C16 C 0.2929(5) 0.01933(19) 1.2853(4) 0.0459(17) Uani 1 1 d . . .
H16B H 0.3299 0.0154 1.3476 0.055 Uiso 1 1 calc R . .
C17A C 0.2983(5) 0.22664(19) 1.2547(5) 0.054(2) Uani 1 1 d . . .
H17A H 0.3586 0.2303 1.2921 0.065 Uiso 1 1 calc R . .
C17 C 0.2049(4) 0.01934(17) 1.2511(4) 0.0398(16) Uani 1 1 d . . .
H17B H 0.1829 0.0161 1.2903 0.048 Uiso 1 1 calc R . .
C18A C 0.2631(5) 0.22345(18) 1.1631(5) 0.0488(18) Uani 1 1 d . . .
H18A H 0.2976 0.2255 1.1360 0.059 Uiso 1 1 calc R . .
C18 C 0.1481(5) 0.02397(16) 1.1608(4) 0.0378(15) Uani 1 1 d . . .
H18B H 0.0874 0.0230 1.1364 0.045 Uiso 1 1 calc R . .
C19A C 0.1747(5) 0.21712(17) 1.1128(4) 0.0424(16) Uani 1 1 d . . .
C19 C 0.1843(4) 0.03020(16) 1.1074(4) 0.0319(14) Uani 1 1 d . . .
C20A C 0.1210(4) 0.21011(16) 1.0173(4) 0.0387(15) Uani 1 1 d . . .
C20 C 0.1441(4) 0.03927(16) 1.0127(4) 0.0333(14) Uani 1 1 d . . .
C21 C 0.2367(4) 0.06025(16) 0.8814(4) 0.0342(14) Uani 1 1 d . . .
H21A H 0.2964 0.0576 0.9239 0.041 Uiso 1 1 calc R . .
C21A C -0.1005(4) 0.19082(17) 0.8904(4) 0.0366(15) Uani 1 1 d . . .
H21B H -0.1167 0.1938 0.9345 0.044 Uiso 1 1 calc R . .
C22 C 0.2125(4) 0.07000(15) 0.7903(4) 0.0304(13) Uani 1 1 d . . .
C22A C -0.1667(4) 0.18202(16) 0.8010(4) 0.0360(15) Uani 1 1 d . . .
C23 C 0.1276(4) 0.07477(15) 0.7207(4) 0.0297(13) Uani 1 1 d . . .
C23A C -0.1531(4) 0.17857(15) 0.7276(4) 0.0329(14) Uani 1 1 d . . .
C24 C 0.1138(4) 0.08210(17) 0.6351(4) 0.0374(15) Uani 1 1 d . . .
H24A H 0.0565 0.0856 0.5870 0.045 Uiso 1 1 calc R . .
C24A C -0.2230(4) 0.17023(16) 0.6448(4) 0.0361(15) Uani 1 1 d . . .
H24B H -0.2140 0.1664 0.5959 0.043 Uiso 1 1 calc R . .
C25 C 0.1803(4) 0.08431(19) 0.6195(4) 0.0423(16) Uani 1 1 d . . .
H25A H 0.1682 0.0888 0.5602 0.051 Uiso 1 1 calc R . .
C25A C -0.3062(5) 0.16734(19) 0.6308(5) 0.0478(17) Uani 1 1 d . . .
H25B H -0.3538 0.1627 0.5728 0.057 Uiso 1 1 calc R . .
C26 C 0.2654(5) 0.0803(2) 0.6868(4) 0.0461(17) Uani 1 1 d . . .
H26A H 0.3116 0.0823 0.6751 0.055 Uiso 1 1 calc R . .
C26A C -0.3184(5) 0.1715(2) 0.7045(5) 0.0506(18) Uani 1 1 d . . .
H26B H -0.3748 0.1697 0.6962 0.061 Uiso 1 1 calc R . .
C27 C 0.2800(4) 0.07341(18) 0.7716(4) 0.0418(16) Uani 1 1 d . . .
H27A H 0.3378 0.0708 0.8192 0.050 Uiso 1 1 calc R . .
C27A C -0.2506(5) 0.1780(2) 0.7867(4) 0.0476(17) Uani 1 1 d . . .
H27B H -0.2597 0.1799 0.8360 0.057 Uiso 1 1 calc R . .
Na4 Na 0.2641(6) -0.1228(2) 0.7780(6) 0.096(2) Uani 0.50 1 d P . .
O4X O 0.3350(4) -0.13409(15) 0.8665(4) 0.0685(16) Uani 1 1 d . . .
H4X H 0.3235 -0.1277 0.9059 0.8(5) Uiso 1 1 calc R . .
O1X O 0.5000 0.1033(9) 0.7500 0.082(13) Uani 0.13 1 d P E 1
O2X O 0.461(2) 0.1148(7) 0.680(2) 0.083(8) Uani 0.25 1 d P F 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0288(5) 0.0635(6) 0.0266(4) 0.0060(3) 0.0128(3) 0.0109(4)
Cu2 0.0429(5) 0.0837(7) 0.0292(4) 0.0022(4) 0.0215(4) 0.0218(4)
Cl1 0.0370(9) 0.0317(8) 0.0324(8) 0.0003(6) 0.0166(7) 0.0002(6)
Cl2 0.049(2) 0.0309(18) 0.073(3) 0.000 0.045(2) 0.000
Cl2A 0.082(12) 0.040(7) 0.22(2) 0.049(10) 0.113(15) 0.030(7)
Cl3 0.036(3) 0.044(4) 0.103(6) 0.000 0.035(4) 0.000
Cl3A 0.044(3) 0.038(3) 0.057(4) 0.011(2) 0.037(3) 0.010(2)
N1 0.025(3) 0.045(3) 0.032(3) 0.003(2) 0.013(2) 0.004(2)
N1A 0.042(3) 0.058(3) 0.029(3) -0.015(2) 0.019(2) -0.003(3)
N2 0.032(3) 0.035(3) 0.021(2) 0.0014(19) 0.010(2) 0.002(2)
N2A 0.043(4) 0.050(3) 0.029(3) -0.002(2) 0.022(2) 0.004(3)
O1A 0.038(3) 0.086(4) 0.075(4) 0.010(3) 0.030(3) -0.006(3)
O1 0.068(4) 0.071(4) 0.099(4) -0.022(3) 0.038(3) 0.015(3)
O2 0.030(3) 0.066(3) 0.084(4) -0.033(3) 0.014(3) 0.002(2)
O2A 0.100(5) 0.088(4) 0.118(5) 0.061(4) 0.094(4) 0.059(4)
O3 0.058(3) 0.072(4) 0.092(4) -0.009(3) 0.055(3) -0.016(3)
O3B 0.120(8) 0.081(6) 0.44(2) 0.059(9) 0.158(11) 0.063(5)
O4A 0.045(3) 0.059(3) 0.047(3) -0.021(2) 0.033(2) -0.020(2)
O4 0.032(3) 0.040(2) 0.036(2) 0.0073(18) 0.018(2) 0.0001(19)
O5A 0.038(3) 0.049(3) 0.027(2) -0.0014(18) 0.0203(19) -0.013(2)
O5 0.029(2) 0.040(2) 0.026(2) -0.0029(16) 0.0127(18) -0.0057(18)
C1A 0.035(4) 0.058(4) 0.047(4) -0.019(3) 0.024(3) -0.003(3)
C1 0.042(4) 0.052(4) 0.059(4) 0.003(3) 0.032(4) 0.003(3)
C2 0.055(5) 0.047(4) 0.072(5) -0.004(4) 0.035(4) -0.006(4)
C2A 0.052(5) 0.051(4) 0.060(5) -0.020(3) 0.032(4) -0.014(4)
C3A 0.035(4) 0.079(6) 0.043(4) 0.009(4) 0.015(3) 0.007(4)
C3 0.062(5) 0.045(4) 0.068(5) -0.002(4) 0.029(4) 0.020(4)
C4A 0.045(4) 0.101(7) 0.068(5) 0.038(5) 0.044(4) 0.022(5)
C4 0.038(4) 0.067(5) 0.058(4) -0.016(4) 0.016(4) 0.009(4)
C5 0.037(4) 0.044(4) 0.048(4) -0.010(3) 0.014(3) 0.000(3)
C5A 0.063(5) 0.076(5) 0.046(4) 0.015(4) 0.038(4) 0.028(4)
C6A 0.036(4) 0.062(4) 0.025(3) -0.005(3) 0.016(3) 0.008(3)
C6 0.030(3) 0.041(4) 0.033(3) 0.006(3) 0.015(3) 0.007(3)
C7 0.028(3) 0.039(3) 0.028(3) 0.006(2) 0.009(3) 0.008(3)
C7A 0.044(4) 0.048(4) 0.031(3) -0.006(3) 0.023(3) 0.008(3)
C8 0.033(3) 0.040(4) 0.028(3) 0.006(2) 0.013(3) 0.006(3)
C8A 0.050(4) 0.049(4) 0.037(4) -0.005(3) 0.021(3) 0.011(3)
C9 0.037(4) 0.048(4) 0.049(4) 0.012(3) 0.024(3) 0.012(3)
C9A 0.046(5) 0.078(6) 0.092(7) 0.009(5) 0.027(5) 0.007(4)
C10 0.045(4) 0.037(4) 0.049(4) 0.016(3) 0.022(3) 0.006(3)
C10A 0.063(6) 0.060(6) 0.180(12) 0.022(6) 0.063(7) 0.023(5)
C11 0.047(4) 0.054(5) 0.054(4) 0.002(3) 0.033(4) -0.003(4)
C11A 0.086(8) 0.058(6) 0.181(12) 0.041(7) 0.061(8) 0.035(6)
C12 0.040(4) 0.070(5) 0.075(5) -0.016(4) 0.037(4) -0.007(4)
C12A 0.077(6) 0.089(7) 0.082(6) 0.029(5) 0.052(5) 0.042(5)
C13 0.033(4) 0.050(4) 0.043(4) -0.011(3) 0.012(3) 0.007(3)
C13A 0.069(5) 0.076(5) 0.048(4) 0.020(4) 0.040(4) 0.034(5)
C14 0.038(4) 0.040(3) 0.035(3) 0.005(3) 0.018(3) 0.014(3)
C14A 0.054(4) 0.036(3) 0.038(4) -0.005(3) 0.020(3) 0.014(3)
C15A 0.052(5) 0.067(5) 0.037(4) -0.012(3) 0.018(3) 0.018(4)
C15 0.036(4) 0.054(4) 0.030(3) 0.004(3) 0.016(3) 0.011(3)
C16A 0.065(6) 0.064(5) 0.047(4) -0.019(4) 0.021(4) 0.020(4)
C16 0.049(4) 0.053(4) 0.030(3) 0.009(3) 0.016(3) 0.017(3)
C17A 0.048(4) 0.053(4) 0.047(4) -0.022(3) 0.012(4) 0.005(3)
C17 0.052(4) 0.034(3) 0.043(4) 0.009(3) 0.031(3) 0.011(3)
C18A 0.043(4) 0.040(4) 0.059(5) -0.017(3) 0.023(4) 0.001(3)
C18 0.045(4) 0.035(3) 0.044(4) 0.011(3) 0.030(3) 0.009(3)
C19A 0.046(4) 0.035(3) 0.050(4) -0.011(3) 0.027(3) 0.001(3)
C19 0.032(3) 0.032(3) 0.034(3) 0.000(2) 0.018(3) 0.003(3)
C20A 0.048(4) 0.033(3) 0.039(4) -0.016(3) 0.025(3) -0.007(3)
C20 0.031(4) 0.032(3) 0.032(3) 0.006(2) 0.012(3) 0.007(3)
C21 0.022(3) 0.040(4) 0.035(3) -0.002(3) 0.011(3) 0.002(3)
C21A 0.042(4) 0.045(4) 0.033(3) 0.000(3) 0.027(3) 0.001(3)
C22 0.033(3) 0.030(3) 0.030(3) -0.006(2) 0.017(3) 0.000(2)
C22A 0.041(4) 0.034(3) 0.039(3) 0.003(3) 0.025(3) 0.010(3)
C23 0.033(3) 0.024(3) 0.036(3) -0.003(2) 0.020(3) -0.003(2)
C23A 0.038(4) 0.023(3) 0.038(3) 0.008(2) 0.019(3) 0.002(3)
C24 0.040(4) 0.041(3) 0.029(3) 0.003(3) 0.016(3) -0.005(3)
C24A 0.045(4) 0.033(3) 0.035(3) 0.000(3) 0.025(3) 0.002(3)
C25 0.043(4) 0.051(4) 0.037(4) -0.001(3) 0.024(3) 0.000(3)
C25A 0.044(4) 0.046(4) 0.053(4) 0.005(3) 0.024(3) 0.003(3)
C26 0.043(4) 0.063(4) 0.043(4) 0.005(3) 0.028(3) 0.004(3)
C26A 0.044(4) 0.063(5) 0.050(4) 0.004(3) 0.026(4) 0.010(3)
C27 0.031(4) 0.052(4) 0.040(4) 0.000(3) 0.016(3) 0.005(3)
C27A 0.046(4) 0.068(5) 0.036(4) 0.002(3) 0.026(3) 0.012(3)
Na4 0.083(5) 0.080(5) 0.116(6) 0.016(4) 0.043(5) 0.006(4)
O4X 0.071(4) 0.059(3) 0.075(4) -0.001(3) 0.037(3) -0.001(3)
O1X 0.05(2) 0.042(19) 0.08(2) 0.000 -0.021(18) 0.000
O2X 0.11(2) 0.060(14) 0.13(2) 0.004(15) 0.09(2) -0.001(15)

_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 O5 1.913(4) 2_556 ?
Cu1 N2 1.930(5) . ?
Cu1 O5 1.943(4) . ?
Cu1 O4 2.041(4) . ?
Cu1 Cl1 2.5331(17) . ?
Cu1 Cu1 2.8981(14) 2_556 ?
Cu2 O5A 1.921(4) 2_556 ?
Cu2 N2A 1.938(5) . ?
Cu2 O5A 1.949(4) . ?
Cu2 O4A 2.081(4) . ?
Cu2 Cl1 2.4911(17) . ?
Cu2 Cu2 2.9403(15) 2_556 ?
N1 C20 1.352(8) . ?
N1 N2 1.361(7) . ?
N1 C7 1.489(7) . ?
N1A C20A 1.349(9) . ?
N1A N2A 1.395(7) . ?
N1A C7A 1.502(8) . ?
N2 C21 1.291(8) . ?
N2A C21A 1.272(8) . ?
O1A C3A 1.363(10) . ?
O1A H1AA 0.8400 . ?
O1 C3 1.379(9) . ?
O1 H1A 0.8400 . ?
O2 C5 1.358(8) . ?
O2 C13 1.377(8) . ?
O2A C5A 1.353(9) . ?
O2A C13A 1.386(11) . ?
O3 C11 1.357(9) . ?
O3 H3A 0.8400 . ?
O3B C11A 1.390(13) . ?
O3B H3BA 0.8400 . ?
O4A C20A 1.242(8) . ?
O4 C20 1.242(7) . ?
O5A C23A 1.327(7) . ?
O5A Cu2 1.921(4) 2_556 ?
O5 C23 1.336(7) . ?
O5 Cu1 1.913(4) 2_556 ?
C1A C2A 1.361(10) . ?
C1A C6A 1.403(10) . ?
C1A H1AB 0.9500 . ?
C1 C2 1.348(10) . ?
C1 C6 1.385(10) . ?
C1 H1B 0.9500 . ?
C2 C3 1.399(11) . ?
C2 H2A 0.9500 . ?
C2A C3A 1.403(11) . ?
C2A H2AA 0.9500 . ?
C3A C4A 1.311(11) . ?
C3 C4 1.329(11) . ?
C4A C5A 1.392(12) . ?
C4A H4AA 0.9500 . ?
C4 C5 1.395(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.381(9) . ?
C5A C6A 1.403(10) . ?
C6A C7A 1.477(10) . ?
C6 C7 1.516(9) . ?
C7 C8 1.512(9) . ?
C7 C14 1.530(9) . ?
C7A C14A 1.505(10) . ?
C7A C8A 1.534(9) . ?
C8 C13 1.375(9) . ?
C8 C9 1.385(9) . ?
C8A C13A 1.366(11) . ?
C8A C9A 1.371(11) . ?
C9 C10 1.377(10) . ?
C9 H9A 0.9500 . ?
C9A C10A 1.365(13) . ?
C9A H9AA 0.9500 . ?
C10 C11 1.388(10) . ?
C10 H10A 0.9500 . ?
C10A C11A 1.361(15) . ?
C10A H10B 0.9500 . ?
C11 C12 1.364(10) . ?
C11A C12A 1.341(15) . ?
C12 C13 1.404(10) . ?
C12 H12A 0.9500 . ?
C12A C13A 1.424(11) . ?
C12A H12B 0.9500 . ?
C14 C15 1.380(8) . ?
C14 C19 1.395(9) . ?
C14A C19A 1.390(10) . ?
C14A C15A 1.394(9) . ?
C15A C16A 1.376(11) . ?
C15A H15A 0.9500 . ?
C15 C16 1.394(10) . ?
C15 H15B 0.9500 . ?
C16A C17A 1.408(12) . ?
C16A H16A 0.9500 . ?
C16 C17 1.379(10) . ?
C16 H16B 0.9500 . ?
C17A C18A 1.385(10) . ?
C17A H17A 0.9500 . ?
C17 C18 1.380(9) . ?
C17 H17B 0.9500 . ?
C18A C19A 1.391(10) . ?
C18A H18A 0.9500 . ?
C18 C19 1.391(9) . ?
C18 H18B 0.9500 . ?
C19A C20A 1.457(9) . ?
C19 C20 1.458(8) . ?
C21 C22 1.454(8) . ?
C21 H21A 0.9500 . ?
C21A C22A 1.435(9) . ?
C21A H21B 0.9500 . ?
C22 C23 1.397(8) . ?
C22 C27 1.409(9) . ?
C22A C27A 1.406(10) . ?
C22A C23A 1.416(9) . ?
C23 C24 1.400(8) . ?
C23A C24A 1.382(9) . ?
C24 C25 1.353(9) . ?
C24 H24A 0.9500 . ?
C24A C25A 1.391(10) . ?
C24A H24B 0.9500 . ?
C25 C26 1.385(10) . ?
C25 H25A 0.9500 . ?
C25A C26A 1.408(10) . ?
C25A H25B 0.9500 . ?
C26 C27 1.380(9) . ?
C26 H26A 0.9500 . ?
C26A C27A 1.348(10) . ?
C26A H26B 0.9500 . ?
C27 H27A 0.9500 . ?
C27A H27B 0.9500 . ?
Na4 O4X 1.473(10) . ?
O4X H4X 0.8400 . ?

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
O5 Cu1 N2 169.36(18) 2_556 . ?
O5 Cu1 O5 81.02(19) 2_556 . ?
N2 Cu1 O5 89.99(18) . . ?
O5 Cu1 O4 103.72(17) 2_556 . ?
N2 Cu1 O4 83.06(19) . . ?
O5 Cu1 O4 161.14(17) . . ?
O5 Cu1 Cl1 99.59(12) 2_556 . ?
N2 Cu1 Cl1 88.97(14) . . ?
O5 Cu1 Cl1 111.59(12) . . ?
O4 Cu1 Cl1 85.89(12) . . ?
O5 Cu1 Cu1 41.67(12) 2_556 2_556 ?
N2 Cu1 Cu1 128.19(14) . 2_556 ?
O5 Cu1 Cu1 40.90(12) . 2_556 ?
O4 Cu1 Cu1 136.54(12) . 2_556 ?
Cl1 Cu1 Cu1 119.27(4) . 2_556 ?
O5A Cu2 N2A 167.8(2) 2_556 . ?
O5A Cu2 O5A 80.7(2) 2_556 . ?
N2A Cu2 O5A 89.6(2) . . ?
O5A Cu2 O4A 103.44(18) 2_556 . ?
N2A Cu2 O4A 82.8(2) . . ?
O5A Cu2 O4A 157.6(2) . . ?
O5A Cu2 Cl1 101.80(13) 2_556 . ?
N2A Cu2 Cl1 89.07(16) . . ?
O5A Cu2 Cl1 115.51(13) . . ?
O4A Cu2 Cl1 85.53(14) . . ?
O5A Cu2 Cu2 40.91(13) 2_556 2_556 ?
N2A Cu2 Cu2 128.32(16) . 2_556 ?
O5A Cu2 Cu2 40.20(12) . 2_556 ?
O4A Cu2 Cu2 136.98(13) . 2_556 ?
Cl1 Cu2 Cu2 119.07(4) . 2_556 ?
Cu2 Cl1 Cu1 119.21(6) . . ?
C20 N1 N2 116.8(5) . . ?
C20 N1 C7 114.3(5) . . ?
N2 N1 C7 128.7(5) . . ?
C20A N1A N2A 116.3(5) . . ?
C20A N1A C7A 115.0(5) . . ?
N2A N1A C7A 128.6(5) . . ?
C21 N2 N1 122.0(5) . . ?
C21 N2 Cu1 128.7(4) . . ?
N1 N2 Cu1 108.7(4) . . ?
C21A N2A N1A 121.6(5) . . ?
C21A N2A Cu2 129.6(4) . . ?
N1A N2A Cu2 108.6(4) . . ?
C3A O1A H1AA 109.5 . . ?
C3 O1 H1A 109.5 . . ?
C5 O2 C13 119.2(5) . . ?
C5A O2A C13A 118.4(7) . . ?
C11 O3 H3A 109.5 . . ?
C11A O3B H3BA 109.5 . . ?
C20A O4A Cu2 105.9(4) . . ?
C20 O4 Cu1 106.8(4) . . ?
C23A O5A Cu2 131.8(4) . 2_556 ?
C23A O5A Cu2 129.3(4) . . ?
Cu2 O5A Cu2 98.9(2) 2_556 . ?
C23 O5 Cu1 131.9(3) . 2_556 ?
C23 O5 Cu1 130.2(3) . . ?
Cu1 O5 Cu1 97.43(19) 2_556 . ?
C2A C1A C6A 123.4(7) . . ?
C2A C1A H1AB 118.3 . . ?
C6A C1A H1AB 118.3 . . ?
C2 C1 C6 122.4(7) . . ?
C2 C1 H1B 118.8 . . ?
C6 C1 H1B 118.8 . . ?
C1 C2 C3 118.5(7) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C1A C2A C3A 118.9(7) . . ?
C1A C2A H2AA 120.6 . . ?
C3A C2A H2AA 120.6 . . ?
C4A C3A O1A 118.6(7) . . ?
C4A C3A C2A 120.6(8) . . ?
O1A C3A C2A 120.6(7) . . ?
C4 C3 O1 117.7(8) . . ?
C4 C3 C2 121.9(7) . . ?
O1 C3 C2 120.4(7) . . ?
C3A C4A C5A 120.1(8) . . ?
C3A C4A H4AA 119.9 . . ?
C5A C4A H4AA 119.9 . . ?
C3 C4 C5 118.5(7) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
O2 C5 C6 122.1(6) . . ?
O2 C5 C4 116.1(7) . . ?
C6 C5 C4 121.8(6) . . ?
O2A C5A C4A 115.2(7) . . ?
O2A C5A C6A 121.9(7) . . ?
C4A C5A C6A 122.9(7) . . ?
C5A C6A C1A 113.8(7) . . ?
C5A C6A C7A 124.0(6) . . ?
C1A C6A C7A 122.2(6) . . ?
C5 C6 C1 116.9(6) . . ?
C5 C6 C7 120.6(6) . . ?
C1 C6 C7 122.4(6) . . ?
N1 C7 C8 111.7(5) . . ?
N1 C7 C6 110.2(5) . . ?
C8 C7 C6 111.5(5) . . ?
N1 C7 C14 98.3(5) . . ?
C8 C7 C14 112.3(5) . . ?
C6 C7 C14 112.2(5) . . ?
C6A C7A N1A 112.2(5) . . ?
C6A C7A C14A 114.5(5) . . ?
N1A C7A C14A 98.0(5) . . ?
C6A C7A C8A 110.2(6) . . ?
N1A C7A C8A 109.5(5) . . ?
C14A C7A C8A 111.9(5) . . ?
C13 C8 C9 118.1(6) . . ?
C13 C8 C7 119.1(5) . . ?
C9 C8 C7 122.8(6) . . ?
C13A C8A C9A 118.8(7) . . ?
C13A C8A C7A 121.0(7) . . ?
C9A C8A C7A 120.2(7) . . ?
C10 C9 C8 121.7(7) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C10A C9A C8A 120.9(10) . . ?
C10A C9A H9AA 119.6 . . ?
C8A C9A H9AA 119.6 . . ?
C9 C10 C11 119.8(6) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C11A C10A C9A 120.3(10) . . ?
C11A C10A H10B 119.8 . . ?
C9A C10A H10B 119.8 . . ?
O3 C11 C12 119.1(7) . . ?
O3 C11 C10 121.6(7) . . ?
C12 C11 C10 119.3(7) . . ?
C12A C11A C10A 121.0(9) . . ?
C12A C11A O3B 116.7(12) . . ?
C10A C11A O3B 122.3(11) . . ?
C11 C12 C13 120.6(7) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C11A C12A C13A 118.9(10) . . ?
C11A C12A H12B 120.6 . . ?
C13A C12A H12B 120.6 . . ?
O2 C13 C8 123.7(6) . . ?
O2 C13 C12 115.8(6) . . ?
C8 C13 C12 120.5(6) . . ?
C8A C13A O2A 124.3(7) . . ?
C8A C13A C12A 120.1(8) . . ?
O2A C13A C12A 115.5(8) . . ?
C15 C14 C19 120.3(6) . . ?
C15 C14 C7 127.7(6) . . ?
C19 C14 C7 112.0(5) . . ?
C19A C14A C15A 120.4(7) . . ?
C19A C14A C7A 112.3(6) . . ?
C15A C14A C7A 127.3(7) . . ?
C16A C15A C14A 116.9(8) . . ?
C16A C15A H15A 121.6 . . ?
C14A C15A H15A 121.6 . . ?
C14 C15 C16 117.1(6) . . ?
C14 C15 H15B 121.4 . . ?
C16 C15 H15B 121.4 . . ?
C15A C16A C17A 122.8(7) . . ?
C15A C16A H16A 118.6 . . ?
C17A C16A H16A 118.6 . . ?
C17 C16 C15 122.2(6) . . ?
C17 C16 H16B 118.9 . . ?
C15 C16 H16B 118.9 . . ?
C18A C17A C16A 120.3(7) . . ?
C18A C17A H17A 119.8 . . ?
C16A C17A H17A 119.8 . . ?
C16 C17 C18 121.2(6) . . ?
C16 C17 H17B 119.4 . . ?
C18 C17 H17B 119.4 . . ?
C17A C18A C19A 116.6(8) . . ?
C17A C18A H18A 121.7 . . ?
C19A C18A H18A 121.7 . . ?
C17 C18 C19 116.7(6) . . ?
C17 C18 H18B 121.7 . . ?
C19 C18 H18B 121.7 . . ?
C14A C19A C18A 122.9(6) . . ?
C14A C19A C20A 107.8(6) . . ?
C18A C19A C20A 129.2(7) . . ?
C18 C19 C14 122.4(6) . . ?
C18 C19 C20 130.8(6) . . ?
C14 C19 C20 106.7(5) . . ?
O4A C20A N1A 123.4(6) . . ?
O4A C20A C19A 130.0(6) . . ?
N1A C20A C19A 106.6(5) . . ?
O4 C20 N1 122.3(5) . . ?
O4 C20 C19 129.4(6) . . ?
N1 C20 C19 108.3(5) . . ?
N2 C21 C22 123.8(5) . . ?
N2 C21 H21A 118.1 . . ?
C22 C21 H21A 118.1 . . ?
N2A C21A C22A 123.6(6) . . ?
N2A C21A H21B 118.2 . . ?
C22A C21A H21B 118.2 . . ?
C23 C22 C27 118.7(5) . . ?
C23 C22 C21 124.5(6) . . ?
C27 C22 C21 116.7(5) . . ?
C27A C22A C23A 119.2(6) . . ?
C27A C22A C21A 116.3(5) . . ?
C23A C22A C21A 124.5(6) . . ?
O5 C23 C22 121.1(5) . . ?
O5 C23 C24 120.7(5) . . ?
C22 C23 C24 118.1(6) . . ?
O5A C23A C24A 120.2(5) . . ?
O5A C23A C22A 121.4(5) . . ?
C24A C23A C22A 118.3(6) . . ?
C25 C24 C23 121.3(6) . . ?
C25 C24 H24A 119.3 . . ?
C23 C24 H24A 119.3 . . ?
C23A C24A C25A 122.0(6) . . ?
C23A C24A H24B 119.0 . . ?
C25A C24A H24B 119.0 . . ?
C24 C25 C26 122.4(6) . . ?
C24 C25 H25A 118.8 . . ?
C26 C25 H25A 118.8 . . ?
C24A C25A C26A 118.5(7) . . ?
C24A C25A H25B 120.7 . . ?
C26A C25A H25B 120.7 . . ?
C27 C26 C25 116.9(7) . . ?
C27 C26 H26A 121.6 . . ?
C25 C26 H26A 121.6 . . ?
C27A C26A C25A 120.5(7) . . ?
C27A C26A H26B 119.7 . . ?
C25A C26A H26B 119.7 . . ?
C26 C27 C22 122.5(6) . . ?
C26 C27 H27A 118.7 . . ?
C22 C27 H27A 118.7 . . ?
C26A C27A C22A 121.3(6) . . ?
C26A C27A H27B 119.4 . . ?
C22A C27A H27B 119.4 . . ?
Na4 O4X H4X 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5A Cu2 Cl1 Cu1 -51.00(15) 2_556 . . . ?
N2A Cu2 Cl1 Cu1 123.35(17) . . . . ?
O5A Cu2 Cl1 Cu1 34.22(16) . . . . ?
O4A Cu2 Cl1 Cu1 -153.82(14) . . . . ?
Cu2 Cu2 Cl1 Cu1 -11.11(10) 2_556 . . . ?
O5 Cu1 Cl1 Cu2 -47.71(14) 2_556 . . . ?
N2 Cu1 Cl1 Cu2 125.93(16) . . . . ?
O5 Cu1 Cl1 Cu2 36.35(15) . . . . ?
O4 Cu1 Cl1 Cu2 -150.95(14) . . . . ?
Cu1 Cu1 Cl1 Cu2 -8.40(10) 2_556 . . . ?
C20 N1 N2 C21 -177.2(5) . . . . ?
C7 N1 N2 C21 -3.3(9) . . . . ?
C20 N1 N2 Cu1 11.2(6) . . . . ?
C7 N1 N2 Cu1 -174.9(5) . . . . ?
O5 Cu1 N2 C21 46.1(13) 2_556 . . . ?
O5 Cu1 N2 C21 13.9(5) . . . . ?
O4 Cu1 N2 C21 176.4(5) . . . . ?
Cl1 Cu1 N2 C21 -97.6(5) . . . . ?
Cu1 Cu1 N2 C21 29.8(6) 2_556 . . . ?
O5 Cu1 N2 N1 -143.0(9) 2_556 . . . ?
O5 Cu1 N2 N1 -175.2(4) . . . . ?
O4 Cu1 N2 N1 -12.8(3) . . . . ?
Cl1 Cu1 N2 N1 73.2(3) . . . . ?
Cu1 Cu1 N2 N1 -159.4(3) 2_556 . . . ?
C20A N1A N2A C21A -175.1(6) . . . . ?
C7A N1A N2A C21A 2.9(10) . . . . ?
C20A N1A N2A Cu2 10.9(6) . . . . ?
C7A N1A N2A Cu2 -171.2(5) . . . . ?
O5A Cu2 N2A C21A 51.4(13) 2_556 . . . ?
O5A Cu2 N2A C21A 14.0(6) . . . . ?
O4A Cu2 N2A C21A 172.8(6) . . . . ?
Cl1 Cu2 N2A C21A -101.6(6) . . . . ?
Cu2 Cu2 N2A C21A 25.8(7) 2_556 . . . ?
O5A Cu2 N2A N1A -135.2(9) 2_556 . . . ?
O5A Cu2 N2A N1A -172.6(4) . . . . ?
O4A Cu2 N2A N1A -13.8(4) . . . . ?
Cl1 Cu2 N2A N1A 71.9(4) . . . . ?
Cu2 Cu2 N2A N1A -160.8(3) 2_556 . . . ?
O5A Cu2 O4A C20A -175.3(4) 2_556 . . . ?
N2A Cu2 O4A C20A 15.4(4) . . . . ?
O5A Cu2 O4A C20A 86.4(6) . . . . ?
Cl1 Cu2 O4A C20A -74.2(4) . . . . ?
Cu2 Cu2 O4A C20A 156.7(3) 2_556 . . . ?
O5 Cu1 O4 C20 -175.3(4) 2_556 . . . ?
N2 Cu1 O4 C20 13.0(4) . . . . ?
O5 Cu1 O4 C20 82.1(6) . . . . ?
Cl1 Cu1 O4 C20 -76.4(4) . . . . ?
Cu1 Cu1 O4 C20 154.0(3) 2_556 . . . ?
O5A Cu2 O5A C23A 173.1(4) 2_556 . . . ?
N2A Cu2 O5A C23A -14.4(5) . . . . ?
O4A Cu2 O5A C23A -84.2(6) . . . . ?
Cl1 Cu2 O5A C23A 74.3(5) . . . . ?
Cu2 Cu2 O5A C23A 180(100) 2_556 . . . ?
O5A Cu2 O5A Cu2 -6.9(3) 2_556 . . 2_556 ?
N2A Cu2 O5A Cu2 165.6(2) . . . 2_556 ?
O4A Cu2 O5A Cu2 95.8(5) . . . 2_556 ?
Cl1 Cu2 O5A Cu2 -105.63(15) . . . 2_556 ?
O5 Cu1 O5 C23 173.7(4) 2_556 . . . ?
N2 Cu1 O5 C23 -12.0(5) . . . . ?
O4 Cu1 O5 C23 -80.0(7) . . . . ?
Cl1 Cu1 O5 C23 76.9(4) . . . . ?
Cu1 Cu1 O5 C23 -172.8(5) 2_556 . . . ?
O5 Cu1 O5 Cu1 -13.4(2) 2_556 . . 2_556 ?
N2 Cu1 O5 Cu1 160.86(19) . . . 2_556 ?
O4 Cu1 O5 Cu1 92.8(5) . . . 2_556 ?
Cl1 Cu1 O5 Cu1 -110.26(13) . . . 2_556 ?
C6 C1 C2 C3 -1.4(12) . . . . ?
C6A C1A C2A C3A -1.0(10) . . . . ?
C1A C2A C3A C4A 4.3(11) . . . . ?
C1A C2A C3A O1A 179.7(6) . . . . ?
C1 C2 C3 C4 0.7(13) . . . . ?
C1 C2 C3 O1 -179.7(7) . . . . ?
O1A C3A C4A C5A -178.8(7) . . . . ?
C2A C3A C4A C5A -3.3(12) . . . . ?
O1 C3 C4 C5 -179.8(7) . . . . ?
C2 C3 C4 C5 -0.3(13) . . . . ?
C13 O2 C5 C6 -11.4(11) . . . . ?
C13 O2 C5 C4 167.0(7) . . . . ?
C3 C4 C5 O2 -178.0(8) . . . . ?
C3 C4 C5 C6 0.5(12) . . . . ?
C13A O2A C5A C4A 175.4(7) . . . . ?
C13A O2A C5A C6A -5.0(11) . . . . ?
C3A C4A C5A O2A 178.7(7) . . . . ?
C3A C4A C5A C6A -0.9(12) . . . . ?
O2A C5A C6A C1A -175.7(7) . . . . ?
C4A C5A C6A C1A 3.8(10) . . . . ?
O2A C5A C6A C7A 3.0(11) . . . . ?
C4A C5A C6A C7A -177.5(7) . . . . ?
C2A C1A C6A C5A -2.8(9) . . . . ?
C2A C1A C6A C7A 178.5(6) . . . . ?
O2 C5 C6 C1 177.3(7) . . . . ?
C4 C5 C6 C1 -1.1(10) . . . . ?
O2 C5 C6 C7 -4.3(10) . . . . ?
C4 C5 C6 C7 177.4(6) . . . . ?
C2 C1 C6 C5 1.5(10) . . . . ?
C2 C1 C6 C7 -176.9(6) . . . . ?
C20 N1 C7 C8 -125.4(6) . . . . ?
N2 N1 C7 C8 60.5(8) . . . . ?
C20 N1 C7 C6 110.0(6) . . . . ?
N2 N1 C7 C6 -64.0(7) . . . . ?
C20 N1 C7 C14 -7.4(6) . . . . ?
N2 N1 C7 C14 178.6(5) . . . . ?
C5 C6 C7 N1 142.9(6) . . . . ?
C1 C6 C7 N1 -38.8(8) . . . . ?
C5 C6 C7 C8 18.2(8) . . . . ?
C1 C6 C7 C8 -163.4(6) . . . . ?
C5 C6 C7 C14 -108.7(7) . . . . ?
C1 C6 C7 C14 69.6(7) . . . . ?
C5A C6A C7A N1A -124.0(7) . . . . ?
C1A C6A C7A N1A 54.6(8) . . . . ?
C5A C6A C7A C14A 125.5(7) . . . . ?
C1A C6A C7A C14A -55.9(8) . . . . ?
C5A C6A C7A C8A -1.7(8) . . . . ?
C1A C6A C7A C8A 176.9(5) . . . . ?
C20A N1A C7A C6A -126.2(6) . . . . ?
N2A N1A C7A C6A 55.8(8) . . . . ?
C20A N1A C7A C14A -5.5(7) . . . . ?
N2A N1A C7A C14A 176.5(6) . . . . ?
C20A N1A C7A C8A 111.1(6) . . . . ?
N2A N1A C7A C8A -66.9(8) . . . . ?
N1 C7 C8 C13 -141.9(6) . . . . ?
C6 C7 C8 C13 -18.1(7) . . . . ?
C14 C7 C8 C13 108.8(6) . . . . ?
N1 C7 C8 C9 39.6(8) . . . . ?
C6 C7 C8 C9 163.4(5) . . . . ?
C14 C7 C8 C9 -69.7(7) . . . . ?
C6A C7A C8A C13A 2.9(8) . . . . ?
N1A C7A C8A C13A 126.8(7) . . . . ?
C14A C7A C8A C13A -125.7(7) . . . . ?
C6A C7A C8A C9A -178.1(7) . . . . ?
N1A C7A C8A C9A -54.2(8) . . . . ?
C14A C7A C8A C9A 53.3(9) . . . . ?
C13 C8 C9 C10 -1.5(9) . . . . ?
C7 C8 C9 C10 177.0(6) . . . . ?
C13A C8A C9A C10A 1.7(14) . . . . ?
C7A C8A C9A C10A -177.3(9) . . . . ?
C8 C9 C10 C11 1.3(10) . . . . ?
C8A C9A C10A C11A -0.7(18) . . . . ?
C9 C10 C11 O3 177.4(6) . . . . ?
C9 C10 C11 C12 -1.8(10) . . . . ?
C9A C10A C11A C12A -1(2) . . . . ?
C9A C10A C11A O3B 179.1(14) . . . . ?
O3 C11 C12 C13 -176.7(7) . . . . ?
C10 C11 C12 C13 2.6(11) . . . . ?
C10A C11A C12A C13A 1.0(19) . . . . ?
O3B C11A C12A C13A -178.8(12) . . . . ?
C5 O2 C13 C8 11.4(11) . . . . ?
C5 O2 C13 C12 -167.8(7) . . . . ?
C9 C8 C13 O2 -177.0(6) . . . . ?
C7 C8 C13 O2 4.4(10) . . . . ?
C9 C8 C13 C12 2.2(10) . . . . ?
C7 C8 C13 C12 -176.3(6) . . . . ?
C11 C12 C13 O2 176.5(7) . . . . ?
C11 C12 C13 C8 -2.8(11) . . . . ?
C9A C8A C13A O2A 175.4(7) . . . . ?
C7A C8A C13A O2A -5.6(11) . . . . ?
C9A C8A C13A C12A -1.4(12) . . . . ?
C7A C8A C13A C12A 177.6(7) . . . . ?
C5A O2A C13A C8A 6.5(11) . . . . ?
C5A O2A C13A C12A -176.5(7) . . . . ?
C11A C12A C13A C8A 0.0(14) . . . . ?
C11A C12A C13A O2A -177.0(10) . . . . ?
N1 C7 C14 C15 -174.0(6) . . . . ?
C8 C7 C14 C15 -56.4(8) . . . . ?
C6 C7 C14 C15 70.2(8) . . . . ?
N1 C7 C14 C19 6.2(6) . . . . ?
C8 C7 C14 C19 123.8(6) . . . . ?
C6 C7 C14 C19 -109.6(6) . . . . ?
C6A C7A C14A C19A 123.5(6) . . . . ?
N1A C7A C14A C19A 4.6(7) . . . . ?
C8A C7A C14A C19A -110.2(6) . . . . ?
C6A C7A C14A C15A -55.5(9) . . . . ?
N1A C7A C14A C15A -174.4(7) . . . . ?
C8A C7A C14A C15A 70.8(9) . . . . ?
C19A C14A C15A C16A -0.1(10) . . . . ?
C7A C14A C15A C16A 178.8(6) . . . . ?
C19 C14 C15 C16 -1.2(9) . . . . ?
C7 C14 C15 C16 179.0(6) . . . . ?
C14A C15A C16A C17A 0.8(11) . . . . ?
C14 C15 C16 C17 0.5(10) . . . . ?
C15A C16A C17A C18A 0.1(11) . . . . ?
C15 C16 C17 C18 1.6(10) . . . . ?
C16A C17A C18A C19A -1.6(10) . . . . ?
C16 C17 C18 C19 -2.7(9) . . . . ?
C15A C14A C19A C18A -1.6(10) . . . . ?
C7A C14A C19A C18A 179.4(6) . . . . ?
C15A C14A C19A C20A 176.6(6) . . . . ?
C7A C14A C19A C20A -2.4(7) . . . . ?
C17A C18A C19A C14A 2.4(10) . . . . ?
C17A C18A C19A C20A -175.4(6) . . . . ?
C17 C18 C19 C14 2.0(9) . . . . ?
C17 C18 C19 C20 -174.0(6) . . . . ?
C15 C14 C19 C18 0.0(9) . . . . ?
C7 C14 C19 C18 179.8(5) . . . . ?
C15 C14 C19 C20 176.8(6) . . . . ?
C7 C14 C19 C20 -3.4(7) . . . . ?
Cu2 O4A C20A N1A -14.5(7) . . . . ?
Cu2 O4A C20A C19A 166.4(6) . . . . ?
N2A N1A C20A O4A 3.4(9) . . . . ?
C7A N1A C20A O4A -174.8(6) . . . . ?
N2A N1A C20A C19A -177.3(5) . . . . ?
C7A N1A C20A C19A 4.5(7) . . . . ?
C14A C19A C20A O4A 178.1(6) . . . . ?
C18A C19A C20A O4A -3.9(12) . . . . ?
C14A C19A C20A N1A -1.2(7) . . . . ?
C18A C19A C20A N1A 176.9(6) . . . . ?
Cu1 O4 C20 N1 -11.0(7) . . . . ?
Cu1 O4 C20 C19 168.5(5) . . . . ?
N2 N1 C20 O4 0.4(8) . . . . ?
C7 N1 C20 O4 -174.4(5) . . . . ?
N2 N1 C20 C19 -179.2(5) . . . . ?
C7 N1 C20 C19 6.0(7) . . . . ?
C18 C19 C20 O4 -4.6(11) . . . . ?
C14 C19 C20 O4 179.0(6) . . . . ?
C18 C19 C20 N1 175.0(6) . . . . ?
C14 C19 C20 N1 -1.5(7) . . . . ?
N1 N2 C21 C22 179.5(5) . . . . ?
Cu1 N2 C21 C22 -10.8(8) . . . . ?
N1A N2A C21A C22A 179.2(6) . . . . ?
Cu2 N2A C21A C22A -8.1(9) . . . . ?
N2 C21 C22 C23 -0.1(9) . . . . ?
N2 C21 C22 C27 -177.7(6) . . . . ?
N2A C21A C22A C27A 178.9(6) . . . . ?
N2A C21A C22A C23A -3.4(10) . . . . ?
Cu1 O5 C23 C22 -164.0(4) 2_556 . . . ?
Cu1 O5 C23 C22 6.4(7) . . . . ?
Cu1 O5 C23 C24 14.8(8) 2_556 . . . ?
Cu1 O5 C23 C24 -174.8(4) . . . . ?
C27 C22 C23 O5 179.9(5) . . . . ?
C21 C22 C23 O5 2.3(8) . . . . ?
C27 C22 C23 C24 1.1(8) . . . . ?
C21 C22 C23 C24 -176.5(5) . . . . ?
Cu2 O5A C23A C24A 11.4(8) 2_556 . . . ?
Cu2 O5A C23A C24A -168.6(4) . . . . ?
Cu2 O5A C23A C22A -170.9(4) 2_556 . . . ?
Cu2 O5A C23A C22A 9.1(8) . . . . ?
C27A C22A C23A O5A -179.6(5) . . . . ?
C21A C22A C23A O5A 2.8(9) . . . . ?
C27A C22A C23A C24A -1.9(8) . . . . ?
C21A C22A C23A C24A -179.5(6) . . . . ?
O5 C23 C24 C25 -178.4(6) . . . . ?
C22 C23 C24 C25 0.4(9) . . . . ?
O5A C23A C24A C25A -178.4(5) . . . . ?
C22A C23A C24A C25A 3.8(9) . . . . ?
C23 C24 C25 C26 -1.4(10) . . . . ?
C23A C24A C25A C26A -2.8(10) . . . . ?
C24 C25 C26 C27 0.8(10) . . . . ?
C24A C25A C26A C27A -0.2(10) . . . . ?
C25 C26 C27 C22 0.8(10) . . . . ?
C23 C22 C27 C26 -1.7(9) . . . . ?
C21 C22 C27 C26 176.0(6) . . . . ?
C25A C26A C27A C22A 2.1(11) . . . . ?
C23A C22A C27A C26A -1.1(10) . . . . ?
C21A C22A C27A C26A 176.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        23.96
_diffrn_measured_fraction_theta_full 0.917
_refine_diff_density_max         0.927
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.102


#===END

data_s1
_database_code_depnum_ccdc_archive 'CCDC 740844'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            FlamB
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H29 B N2 O6, C H4 O, H2 O'
_chemical_formula_sum            'C34 H35 B N2 O8'
_chemical_formula_weight         610.45

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'
B B 0.0013 0.0007 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6200(3)
_cell_length_b                   12.0315(4)
_cell_length_c                   14.4614(5)
_cell_angle_alpha                100.699(2)
_cell_angle_beta                 107.549(2)
_cell_angle_gamma                99.854(2)
_cell_volume                     1521.39(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3984
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      21.44

_exptl_crystal_description       prism
_exptl_crystal_colour            bronze
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9704
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            23306
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         24.85
_reflns_number_total             5114
_reflns_number_gt                3547
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Apex II 2.0 Rev.2 (Bruker, 2005)'
_computing_cell_refinement       SAINT
_computing_data_reduction        'SAINT 7.12A (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'

_refine_special_details          
;

No suitable H bond was determined for O1-H1a. The water molecule was not moved
into the cell as it is not the main residue.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5114
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1878
_refine_ls_wR_factor_gt          0.1703
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_restrained_S_all      1.330
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
B1 B 0.7123(4) 0.6744(3) 0.2282(3) 0.0482(8) Uani 1 1 d . . .
N1 N 0.2258(2) 0.79310(19) 0.05426(15) 0.0391(5) Uani 1 1 d . . .
N2 N 0.3218(2) 0.74022(18) 0.01879(16) 0.0405(5) Uani 1 1 d . . .
O1 O 0.2453(3) 0.5285(2) 0.40163(17) 0.0720(7) Uani 1 1 d . . .
H1A H 0.2987 0.5629 0.4593 0.108 Uiso 1 1 calc R . .
O1W O 0.8298(3) 1.3617(3) 0.2415(2) 0.0741(8) Uani 1 1 d . . .
H1G H 0.804(6) 1.442(6) 0.259(4) 0.15(2) Uiso 1 1 d . . .
H1F H 0.853(5) 1.351(4) 0.198(3) 0.086(17) Uiso 1 1 d . . .
O2 O 0.4129(3) 0.90636(18) 0.37134(14) 0.0599(6) Uani 1 1 d . . .
O2W O 0.8232(3) 0.7002(3) 0.6984(2) 0.0977(9) Uani 1 1 d . . .
H2W H 0.8874 0.7234 0.7545 0.146 Uiso 1 1 calc R . .
O3 O 0.7612(3) 1.2221(2) 0.35899(18) 0.0839(8) Uani 1 1 d . . .
H3B H 0.7779 1.2621 0.3216 0.126 Uiso 1 1 calc R . .
O4 O 0.0471(2) 0.75014(18) -0.10365(14) 0.0544(5) Uani 1 1 d . . .
O5 O 0.7720(3) 0.5962(2) 0.27631(15) 0.0690(7) Uani 1 1 d . . .
O6 O 0.7049(3) 0.7687(2) 0.29182(15) 0.0724(7) Uani 1 1 d . . .
C1 C 0.2482(3) 0.7597(2) 0.22185(19) 0.0399(6) Uani 1 1 d . . .
C1W C 0.6945(5) 0.7386(4) 0.6996(3) 0.0920(12) Uani 1 1 d . . .
H1W1 H 0.6679 0.7216 0.7553 0.138 Uiso 1 1 calc R . .
H1W2 H 0.6132 0.6994 0.6383 0.138 Uiso 1 1 calc R . .
H1W3 H 0.7140 0.8212 0.7062 0.138 Uiso 1 1 calc R . .
C2 C 0.1669(3) 0.6450(2) 0.1823(2) 0.0477(7) Uani 1 1 d . . .
H2A H 0.1127 0.6202 0.1140 0.057 Uiso 1 1 calc R . .
C3 C 0.1626(3) 0.5662(3) 0.2395(2) 0.0517(7) Uani 1 1 d . . .
H3A H 0.1075 0.4895 0.2104 0.062 Uiso 1 1 calc R . .
C4 C 0.2424(4) 0.6034(3) 0.3422(2) 0.0529(8) Uani 1 1 d . . .
C5 C 0.3222(4) 0.7174(3) 0.3842(2) 0.0551(8) Uani 1 1 d . . .
H5A H 0.3730 0.7430 0.4530 0.066 Uiso 1 1 calc R . .
C6 C 0.3270(3) 0.7944(2) 0.3241(2) 0.0462(7) Uani 1 1 d . . .
C7 C 0.4606(3) 0.9714(2) 0.3117(2) 0.0457(7) Uani 1 1 d . . .
C8 C 0.5843(4) 1.0637(3) 0.3606(2) 0.0567(8) Uani 1 1 d . . .
H8A H 0.6309 1.0790 0.4296 0.068 Uiso 1 1 calc R . .
C9 C 0.6392(3) 1.1334(3) 0.3074(2) 0.0556(8) Uani 1 1 d . . .
C10 C 0.5685(3) 1.1081(3) 0.2041(2) 0.0533(8) Uani 1 1 d . . .
H10A H 0.6046 1.1534 0.1669 0.064 Uiso 1 1 calc R . .
C11 C 0.4450(3) 1.0157(3) 0.1572(2) 0.0467(7) Uani 1 1 d . . .
H11A H 0.3988 0.9996 0.0881 0.056 Uiso 1 1 calc R . .
C12 C 0.3872(3) 0.9460(2) 0.20934(19) 0.0409(6) Uani 1 1 d . . .
C13 C 0.2467(3) 0.8479(2) 0.16026(19) 0.0396(6) Uani 1 1 d . . .
C14 C 0.1044(3) 0.8910(2) 0.1448(2) 0.0418(6) Uani 1 1 d . . .
C15 C 0.0586(3) 0.9519(3) 0.2168(2) 0.0517(7) Uani 1 1 d . . .
H15A H 0.1195 0.9754 0.2839 0.062 Uiso 1 1 calc R . .
C16 C -0.0811(4) 0.9767(3) 0.1854(3) 0.0604(8) Uani 1 1 d . . .
H16A H -0.1142 1.0179 0.2321 0.072 Uiso 1 1 calc R . .
C17 C -0.1713(4) 0.9413(3) 0.0862(3) 0.0581(8) Uani 1 1 d . . .
H17A H -0.2655 0.9575 0.0674 0.070 Uiso 1 1 calc R . .
C18 C -0.1256(3) 0.8827(3) 0.0144(2) 0.0504(7) Uani 1 1 d . . .
H18A H -0.1862 0.8605 -0.0528 0.060 Uiso 1 1 calc R . .
C19 C 0.0145(3) 0.8576(2) 0.0455(2) 0.0423(6) Uani 1 1 d . . .
C20 C 0.0907(3) 0.7945(2) -0.0128(2) 0.0402(6) Uani 1 1 d . . .
C21 C 0.4422(3) 0.7302(2) 0.0815(2) 0.0407(6) Uani 1 1 d . . .
H21A H 0.4627 0.7567 0.1500 0.049 Uiso 1 1 calc R . .
C22 C 0.5483(3) 0.6765(2) 0.04480(19) 0.0400(6) Uani 1 1 d . . .
C23 C 0.6702(3) 0.6517(2) 0.1132(2) 0.0436(7) Uani 1 1 d . . .
C24 C 0.7677(3) 0.6007(3) 0.0739(2) 0.0545(8) Uani 1 1 d . . .
H26A H 0.8491 0.5830 0.1174 0.065 Uiso 1 1 calc R . .
C25 C 0.7473(4) 0.5763(3) -0.0258(2) 0.0590(8) Uani 1 1 d . . .
H25A H 0.8159 0.5447 -0.0492 0.071 Uiso 1 1 calc R . .
C26 C 0.6258(4) 0.5983(3) -0.0914(2) 0.0579(8) Uani 1 1 d . . .
H24A H 0.6101 0.5795 -0.1597 0.069 Uiso 1 1 calc R . .
C27 C 0.5268(3) 0.6481(3) -0.0567(2) 0.0487(7) Uani 1 1 d . . .
H23A H 0.4444 0.6629 -0.1019 0.058 Uiso 1 1 calc R . .
C28 C 0.7845(4) 0.6354(3) 0.3816(2) 0.0684(9) Uani 1 1 d . . .
C29 C 0.8009(4) 0.7677(3) 0.3933(2) 0.0716(10) Uani 1 1 d . . .
C30 C 0.9186(4) 0.6032(4) 0.4473(3) 0.0799(11) Uani 1 1 d . . .
H30A H 0.8990 0.5200 0.4364 0.120 Uiso 1 1 calc R . .
H30B H 0.9363 0.6383 0.5164 0.120 Uiso 1 1 calc R . .
H30C H 1.0056 0.6308 0.4309 0.120 Uiso 1 1 calc R . .
C31 C 0.6373(4) 0.5755(4) 0.3913(3) 0.0846(12) Uani 1 1 d . . .
H31A H 0.6317 0.4937 0.3838 0.127 Uiso 1 1 calc R . .
H31B H 0.5537 0.5861 0.3402 0.127 Uiso 1 1 calc R . .
H31C H 0.6343 0.6092 0.4561 0.127 Uiso 1 1 calc R . .
C32 C 0.7441(5) 0.8279(4) 0.4701(3) 0.0825(11) Uani 1 1 d . . .
H32A H 0.6433 0.7867 0.4585 0.124 Uiso 1 1 calc R . .
H32B H 0.7452 0.9064 0.4649 0.124 Uiso 1 1 calc R . .
H32C H 0.8076 0.8291 0.5359 0.124 Uiso 1 1 calc R . .
C33 C 0.9649(4) 0.8297(4) 0.4108(3) 0.0911(13) Uani 1 1 d . . .
H33A H 0.9730 0.9116 0.4173 0.137 Uiso 1 1 calc R . .
H33B H 0.9927 0.7978 0.3549 0.137 Uiso 1 1 calc R . .
H33C H 1.0307 0.8180 0.4710 0.137 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.0407(17) 0.059(2) 0.0492(19) 0.0204(17) 0.0134(15) 0.0195(15)
N1 0.0389(12) 0.0422(13) 0.0370(12) 0.0115(10) 0.0103(10) 0.0149(10)
N2 0.0420(12) 0.0408(13) 0.0407(12) 0.0136(10) 0.0136(10) 0.0126(10)
O1 0.1032(18) 0.0676(15) 0.0597(14) 0.0374(12) 0.0325(13) 0.0266(13)
O1W 0.0891(19) 0.0686(18) 0.0673(18) 0.0167(14) 0.0337(15) 0.0142(14)
O2 0.0889(15) 0.0507(13) 0.0371(11) 0.0120(9) 0.0214(10) 0.0084(11)
O2W 0.099(2) 0.082(2) 0.0850(19) 0.0146(16) -0.0085(16) 0.0334(17)
O3 0.0837(17) 0.0663(16) 0.0652(15) 0.0135(12) -0.0047(13) -0.0174(13)
O4 0.0524(12) 0.0632(13) 0.0407(12) 0.0091(10) 0.0050(9) 0.0206(10)
O5 0.0882(16) 0.0780(16) 0.0502(13) 0.0252(11) 0.0186(11) 0.0442(13)
O6 0.0985(18) 0.0793(17) 0.0456(12) 0.0200(12) 0.0165(12) 0.0481(14)
C1 0.0423(14) 0.0439(16) 0.0389(15) 0.0160(12) 0.0154(12) 0.0161(12)
C1W 0.103(3) 0.084(3) 0.093(3) 0.031(2) 0.033(2) 0.024(3)
C2 0.0460(16) 0.0485(17) 0.0496(17) 0.0186(14) 0.0137(13) 0.0122(13)
C3 0.0526(17) 0.0462(17) 0.0590(19) 0.0186(14) 0.0200(15) 0.0119(14)
C4 0.0675(19) 0.0543(19) 0.0538(19) 0.0287(15) 0.0310(16) 0.0235(16)
C5 0.075(2) 0.059(2) 0.0406(16) 0.0190(15) 0.0253(15) 0.0235(17)
C6 0.0553(17) 0.0430(16) 0.0429(16) 0.0112(13) 0.0181(13) 0.0160(13)
C7 0.0572(17) 0.0389(15) 0.0397(15) 0.0113(12) 0.0131(13) 0.0131(13)
C8 0.069(2) 0.0471(18) 0.0390(16) 0.0063(14) 0.0019(15) 0.0119(16)
C9 0.0564(18) 0.0459(17) 0.0526(18) 0.0073(15) 0.0074(15) 0.0079(15)
C10 0.0565(18) 0.0489(18) 0.0529(18) 0.0189(14) 0.0155(15) 0.0081(15)
C11 0.0455(15) 0.0531(18) 0.0389(15) 0.0169(13) 0.0079(12) 0.0120(14)
C12 0.0436(15) 0.0386(15) 0.0407(15) 0.0126(12) 0.0108(12) 0.0142(12)
C13 0.0428(15) 0.0418(15) 0.0369(14) 0.0118(12) 0.0136(11) 0.0154(12)
C14 0.0436(15) 0.0381(15) 0.0485(16) 0.0183(13) 0.0160(13) 0.0139(12)
C15 0.0548(17) 0.0561(19) 0.0503(17) 0.0168(14) 0.0205(14) 0.0211(15)
C16 0.066(2) 0.066(2) 0.069(2) 0.0257(17) 0.0346(18) 0.0346(17)
C17 0.0488(17) 0.065(2) 0.077(2) 0.0358(18) 0.0251(16) 0.0280(15)
C18 0.0455(16) 0.0520(18) 0.0563(18) 0.0236(15) 0.0130(14) 0.0158(14)
C19 0.0410(15) 0.0384(15) 0.0495(17) 0.0193(13) 0.0128(13) 0.0112(12)
C20 0.0409(14) 0.0366(15) 0.0409(16) 0.0147(12) 0.0084(12) 0.0093(12)
C21 0.0431(15) 0.0420(15) 0.0393(15) 0.0145(12) 0.0134(12) 0.0131(12)
C22 0.0393(14) 0.0382(15) 0.0432(15) 0.0137(12) 0.0142(12) 0.0081(11)
C23 0.0415(15) 0.0454(16) 0.0483(16) 0.0185(13) 0.0167(13) 0.0123(12)
C24 0.0460(16) 0.062(2) 0.064(2) 0.0247(16) 0.0206(15) 0.0231(14)
C25 0.061(2) 0.062(2) 0.067(2) 0.0164(17) 0.0357(17) 0.0225(16)
C26 0.067(2) 0.060(2) 0.0494(18) 0.0107(15) 0.0276(16) 0.0116(16)
C27 0.0485(16) 0.0554(18) 0.0414(16) 0.0138(13) 0.0131(13) 0.0130(14)
C28 0.074(2) 0.083(3) 0.0512(19) 0.0250(18) 0.0168(17) 0.0278(19)
C29 0.085(2) 0.081(3) 0.051(2) 0.0218(18) 0.0168(17) 0.031(2)
C30 0.081(3) 0.096(3) 0.066(2) 0.038(2) 0.0122(19) 0.037(2)
C31 0.075(2) 0.097(3) 0.081(3) 0.041(2) 0.026(2) 0.001(2)
C32 0.105(3) 0.094(3) 0.060(2) 0.022(2) 0.031(2) 0.045(2)
C33 0.081(3) 0.099(3) 0.078(3) 0.027(2) 0.020(2) -0.009(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 O6 1.348(4) . ?
B1 O5 1.373(4) . ?
B1 C23 1.547(4) . ?
N1 C20 1.372(3) . ?
N1 N2 1.373(3) . ?
N1 C13 1.490(3) . ?
N2 C21 1.278(3) . ?
O1 C4 1.354(3) . ?
O1 H1A 0.8200 . ?
O1W H1G 1.04(7) . ?
O1W H1F 0.72(4) . ?
O2 C6 1.379(3) . ?
O2 C7 1.390(3) . ?
O2W C1W 1.398(5) . ?
O2W H2W 0.8200 . ?
O3 C9 1.349(4) . ?
O3 H3B 0.8200 . ?
O4 C20 1.232(3) . ?
O5 C28 1.470(4) . ?
O6 C29 1.483(4) . ?
C1 C2 1.382(4) . ?
C1 C6 1.387(4) . ?
C1 C13 1.506(4) . ?
C1W H1W1 0.9600 . ?
C1W H1W2 0.9600 . ?
C1W H1W3 0.9600 . ?
C2 C3 1.372(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.393(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.374(4) . ?
C5 C6 1.387(4) . ?
C5 H5A 0.9300 . ?
C7 C8 1.377(4) . ?
C7 C12 1.382(4) . ?
C8 C9 1.381(4) . ?
C8 H8A 0.9300 . ?
C9 C10 1.392(4) . ?
C10 C11 1.374(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.382(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.513(4) . ?
C13 C14 1.515(4) . ?
C14 C19 1.374(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.385(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.373(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.371(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.391(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.466(4) . ?
C21 C22 1.472(4) . ?
C21 H21A 0.9300 . ?
C22 C27 1.386(4) . ?
C22 C23 1.404(4) . ?
C23 C24 1.403(4) . ?
C24 C25 1.363(4) . ?
C24 H26A 0.9300 . ?
C25 C26 1.366(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.375(4) . ?
C26 H24A 0.9300 . ?
C27 H23A 0.9300 . ?
C28 C30 1.512(5) . ?
C28 C31 1.534(5) . ?
C28 C29 1.545(5) . ?
C29 C32 1.503(5) . ?
C29 C33 1.547(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 B1 O5 113.0(3) . . ?
O6 B1 C23 127.2(3) . . ?
O5 B1 C23 119.7(3) . . ?
C20 N1 N2 118.6(2) . . ?
C20 N1 C13 113.5(2) . . ?
N2 N1 C13 127.8(2) . . ?
C21 N2 N1 118.9(2) . . ?
C4 O1 H1A 109.5 . . ?
H1G O1W H1F 115(5) . . ?
C6 O2 C7 116.8(2) . . ?
C1W O2W H2W 109.5 . . ?
C9 O3 H3B 109.5 . . ?
B1 O5 C28 106.5(3) . . ?
B1 O6 C29 106.2(3) . . ?
C2 C1 C6 117.2(2) . . ?
C2 C1 C13 123.0(2) . . ?
C6 C1 C13 119.7(2) . . ?
O2W C1W H1W1 109.5 . . ?
O2W C1W H1W2 109.5 . . ?
H1W1 C1W H1W2 109.5 . . ?
O2W C1W H1W3 109.5 . . ?
H1W1 C1W H1W3 109.5 . . ?
H1W2 C1W H1W3 109.5 . . ?
C3 C2 C1 122.9(3) . . ?
C3 C2 H2A 118.6 . . ?
C1 C2 H2A 118.6 . . ?
C2 C3 C4 118.7(3) . . ?
C2 C3 H3A 120.6 . . ?
C4 C3 H3A 120.6 . . ?
O1 C4 C5 118.9(3) . . ?
O1 C4 C3 121.2(3) . . ?
C5 C4 C3 119.9(3) . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
O2 C6 C5 116.7(2) . . ?
O2 C6 C1 122.1(2) . . ?
C5 C6 C1 121.2(3) . . ?
C8 C7 C12 121.8(3) . . ?
C8 C7 O2 116.2(2) . . ?
C12 C7 O2 122.0(2) . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8A 119.9 . . ?
C9 C8 H8A 119.9 . . ?
O3 C9 C8 117.7(3) . . ?
O3 C9 C10 123.4(3) . . ?
C8 C9 C10 118.9(3) . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 122.2(3) . . ?
C10 C11 H11A 118.9 . . ?
C12 C11 H11A 118.9 . . ?
C11 C12 C7 117.2(3) . . ?
C11 C12 C13 123.2(2) . . ?
C7 C12 C13 119.6(2) . . ?
N1 C13 C1 111.9(2) . . ?
N1 C13 C12 112.3(2) . . ?
C1 C13 C12 110.0(2) . . ?
N1 C13 C14 99.9(2) . . ?
C1 C13 C14 110.0(2) . . ?
C12 C13 C14 112.4(2) . . ?
C19 C14 C15 120.9(3) . . ?
C19 C14 C13 111.1(2) . . ?
C15 C14 C13 128.0(3) . . ?
C14 C15 C16 117.8(3) . . ?
C14 C15 H15A 121.1 . . ?
C16 C15 H15A 121.1 . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 H17A 119.3 . . ?
C16 C17 H17A 119.3 . . ?
C17 C18 C19 117.7(3) . . ?
C17 C18 H18A 121.1 . . ?
C19 C18 H18A 121.1 . . ?
C14 C19 C18 121.1(3) . . ?
C14 C19 C20 108.9(2) . . ?
C18 C19 C20 130.0(3) . . ?
O4 C20 N1 124.7(2) . . ?
O4 C20 C19 128.9(2) . . ?
N1 C20 C19 106.5(2) . . ?
N2 C21 C22 119.7(2) . . ?
N2 C21 H21A 120.2 . . ?
C22 C21 H21A 120.2 . . ?
C27 C22 C23 120.0(2) . . ?
C27 C22 C21 120.4(2) . . ?
C23 C22 C21 119.5(2) . . ?
C24 C23 C22 117.0(3) . . ?
C24 C23 B1 115.0(2) . . ?
C22 C23 B1 128.0(2) . . ?
C25 C24 C23 122.3(3) . . ?
C25 C24 H26A 118.8 . . ?
C23 C24 H26A 118.8 . . ?
C24 C25 C26 119.7(3) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
C25 C26 C27 120.2(3) . . ?
C25 C26 H24A 119.9 . . ?
C27 C26 H24A 119.9 . . ?
C26 C27 C22 120.7(3) . . ?
C26 C27 H23A 119.7 . . ?
C22 C27 H23A 119.7 . . ?
O5 C28 C30 109.0(3) . . ?
O5 C28 C31 107.3(3) . . ?
C30 C28 C31 111.8(3) . . ?
O5 C28 C29 101.1(3) . . ?
C30 C28 C29 114.7(3) . . ?
C31 C28 C29 112.2(3) . . ?
O6 C29 C32 109.3(3) . . ?
O6 C29 C28 100.8(3) . . ?
C32 C29 C28 115.7(3) . . ?
O6 C29 C33 108.7(3) . . ?
C32 C29 C33 111.2(3) . . ?
C28 C29 C33 110.5(3) . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C33 H33A 109.5 . . ?
C29 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C29 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N1 N2 C21 -174.4(2) . . . . ?
C13 N1 N2 C21 3.2(4) . . . . ?
O6 B1 O5 C28 9.1(4) . . . . ?
C23 B1 O5 C28 -174.2(3) . . . . ?
O5 B1 O6 C29 14.4(4) . . . . ?
C23 B1 O6 C29 -162.0(3) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
C13 C1 C2 C3 -176.7(2) . . . . ?
C1 C2 C3 C4 0.7(4) . . . . ?
C2 C3 C4 O1 -178.2(3) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
O1 C4 C5 C6 176.9(3) . . . . ?
C3 C4 C5 C6 -2.0(5) . . . . ?
C7 O2 C6 C5 158.7(3) . . . . ?
C7 O2 C6 C1 -21.7(4) . . . . ?
C4 C5 C6 O2 -178.2(3) . . . . ?
C4 C5 C6 C1 2.2(4) . . . . ?
C2 C1 C6 O2 179.4(3) . . . . ?
C13 C1 C6 O2 -4.2(4) . . . . ?
C2 C1 C6 C5 -0.9(4) . . . . ?
C13 C1 C6 C5 175.4(2) . . . . ?
C6 O2 C7 C8 -158.3(3) . . . . ?
C6 O2 C7 C12 22.5(4) . . . . ?
C12 C7 C8 C9 -0.5(5) . . . . ?
O2 C7 C8 C9 -179.7(3) . . . . ?
C7 C8 C9 O3 -179.6(3) . . . . ?
C7 C8 C9 C10 -0.6(5) . . . . ?
O3 C9 C10 C11 179.7(3) . . . . ?
C8 C9 C10 C11 0.8(5) . . . . ?
C9 C10 C11 C12 0.1(5) . . . . ?
C10 C11 C12 C7 -1.2(4) . . . . ?
C10 C11 C12 C13 176.7(3) . . . . ?
C8 C7 C12 C11 1.4(4) . . . . ?
O2 C7 C12 C11 -179.5(2) . . . . ?
C8 C7 C12 C13 -176.5(3) . . . . ?
O2 C7 C12 C13 2.6(4) . . . . ?
C20 N1 C13 C1 112.4(2) . . . . ?
N2 N1 C13 C1 -65.3(3) . . . . ?
C20 N1 C13 C12 -123.4(2) . . . . ?
N2 N1 C13 C12 58.9(3) . . . . ?
C20 N1 C13 C14 -4.0(3) . . . . ?
N2 N1 C13 C14 178.3(2) . . . . ?
C2 C1 C13 N1 -31.6(3) . . . . ?
C6 C1 C13 N1 152.3(2) . . . . ?
C2 C1 C13 C12 -157.1(3) . . . . ?
C6 C1 C13 C12 26.8(3) . . . . ?
C2 C1 C13 C14 78.5(3) . . . . ?
C6 C1 C13 C14 -97.6(3) . . . . ?
C11 C12 C13 N1 31.0(3) . . . . ?
C7 C12 C13 N1 -151.2(2) . . . . ?
C11 C12 C13 C1 156.2(2) . . . . ?
C7 C12 C13 C1 -26.0(3) . . . . ?
C11 C12 C13 C14 -80.7(3) . . . . ?
C7 C12 C13 C14 97.1(3) . . . . ?
N1 C13 C14 C19 3.6(3) . . . . ?
C1 C13 C14 C19 -114.1(2) . . . . ?
C12 C13 C14 C19 122.8(2) . . . . ?
N1 C13 C14 C15 -179.1(3) . . . . ?
C1 C13 C14 C15 63.1(4) . . . . ?
C12 C13 C14 C15 -59.9(4) . . . . ?
C19 C14 C15 C16 0.7(4) . . . . ?
C13 C14 C15 C16 -176.4(3) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C15 C16 C17 C18 -1.5(5) . . . . ?
C16 C17 C18 C19 1.5(4) . . . . ?
C15 C14 C19 C18 -0.6(4) . . . . ?
C13 C14 C19 C18 176.9(2) . . . . ?
C15 C14 C19 C20 -179.6(2) . . . . ?
C13 C14 C19 C20 -2.2(3) . . . . ?
C17 C18 C19 C14 -0.4(4) . . . . ?
C17 C18 C19 C20 178.4(3) . . . . ?
N2 N1 C20 O4 0.9(4) . . . . ?
C13 N1 C20 O4 -177.1(2) . . . . ?
N2 N1 C20 C19 -179.1(2) . . . . ?
C13 N1 C20 C19 3.0(3) . . . . ?
C14 C19 C20 O4 179.6(3) . . . . ?
C18 C19 C20 O4 0.7(5) . . . . ?
C14 C19 C20 N1 -0.5(3) . . . . ?
C18 C19 C20 N1 -179.4(3) . . . . ?
N1 N2 C21 C22 -178.4(2) . . . . ?
N2 C21 C22 C27 6.9(4) . . . . ?
N2 C21 C22 C23 -171.7(2) . . . . ?
C27 C22 C23 C24 1.5(4) . . . . ?
C21 C22 C23 C24 -179.9(2) . . . . ?
C27 C22 C23 B1 -179.0(3) . . . . ?
C21 C22 C23 B1 -0.3(4) . . . . ?
O6 B1 C23 C24 139.6(3) . . . . ?
O5 B1 C23 C24 -36.6(4) . . . . ?
O6 B1 C23 C22 -40.0(5) . . . . ?
O5 B1 C23 C22 143.9(3) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
B1 C23 C24 C25 -179.3(3) . . . . ?
C23 C24 C25 C26 -2.0(5) . . . . ?
C24 C25 C26 C27 1.9(5) . . . . ?
C25 C26 C27 C22 -0.1(5) . . . . ?
C23 C22 C27 C26 -1.6(4) . . . . ?
C21 C22 C27 C26 179.7(3) . . . . ?
B1 O5 C28 C30 -148.3(3) . . . . ?
B1 O5 C28 C31 90.5(3) . . . . ?
B1 O5 C28 C29 -27.2(3) . . . . ?
B1 O6 C29 C32 -152.4(3) . . . . ?
B1 O6 C29 C28 -30.1(3) . . . . ?
B1 O6 C29 C33 86.1(4) . . . . ?
O5 C28 C29 O6 34.0(3) . . . . ?
C30 C28 C29 O6 151.1(3) . . . . ?
C31 C28 C29 O6 -80.0(3) . . . . ?
O5 C28 C29 C32 151.8(3) . . . . ?
C30 C28 C29 C32 -91.2(4) . . . . ?
C31 C28 C29 C32 37.8(4) . . . . ?
O5 C28 C29 C33 -80.8(3) . . . . ?
C30 C28 C29 C33 36.3(4) . . . . ?
C31 C28 C29 C33 165.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        24.85
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.047

# Attachment 'Flam_crystals.cif'

data_sp97m
_database_code_depnum_ccdc_archive 'CCDC 740845'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            FlamS
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H18 N2 O5, 2(C2 D3 N)'
_chemical_formula_sum            'C31 H18 D6 N4 O5'
_chemical_formula_weight         538.58

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   14.8323(6)
_cell_length_b                   9.7901(4)
_cell_length_c                   18.5178(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.2450(10)
_cell_angle_gamma                90.00
_cell_volume                     2654.04(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6388
_cell_measurement_theta_min      2.360
_cell_measurement_theta_max      28.125

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43720
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5427
_reflns_number_gt                4481
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.9004P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5427
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1131
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.49746(9) 0.50042(14) 0.30757(8) 0.0200(3) Uani 1 1 d . . .
C2 C 0.55273(9) 0.58081(14) 0.36922(8) 0.0203(3) Uani 1 1 d . . .
C3 C 0.57738(10) 0.54421(16) 0.44186(8) 0.0246(3) Uani 1 1 d . . .
H3 H 0.5578 0.4601 0.4598 0.029 Uiso 1 1 calc R . .
C4 C 0.63164(11) 0.63444(17) 0.48769(9) 0.0295(4) Uani 1 1 d . . .
H4 H 0.6487 0.6121 0.5379 0.035 Uiso 1 1 calc R . .
C5 C 0.66157(11) 0.75724(17) 0.46151(9) 0.0311(4) Uani 1 1 d . . .
H5 H 0.6984 0.8173 0.4941 0.037 Uiso 1 1 calc R . .
C6 C 0.63821(10) 0.79245(16) 0.38859(9) 0.0271(3) Uani 1 1 d . . .
H6 H 0.6589 0.8754 0.3702 0.032 Uiso 1 1 calc R . .
C7 C 0.58336(9) 0.70200(14) 0.34317(8) 0.0215(3) Uani 1 1 d . . .
C8 C 0.55267(9) 0.71053(14) 0.26347(8) 0.0203(3) Uani 1 1 d . . .
C9 C 0.39966(9) 0.47222(14) 0.31730(8) 0.0207(3) Uani 1 1 d . . .
C10 C 0.34482(10) 0.57423(15) 0.34005(8) 0.0252(3) Uani 1 1 d . . .
H10 H 0.3710 0.6611 0.3531 0.030 Uiso 1 1 calc R . .
C11 C 0.25363(10) 0.55329(16) 0.34430(9) 0.0274(3) Uani 1 1 d . . .
H11 H 0.2177 0.6246 0.3598 0.033 Uiso 1 1 calc R . .
C12 C 0.21536(10) 0.42561(16) 0.32542(9) 0.0278(3) Uani 1 1 d . . .
C13 C 0.26820(10) 0.32160(16) 0.30397(9) 0.0277(3) Uani 1 1 d . . .
H13 H 0.2423 0.2342 0.2920 0.033 Uiso 1 1 calc R . .
C14 C 0.35942(10) 0.34585(15) 0.30000(8) 0.0232(3) Uani 1 1 d . . .
C15 C 0.49836(9) 0.24758(15) 0.27828(8) 0.0219(3) Uani 1 1 d . . .
C16 C 0.54137(10) 0.12771(15) 0.26290(8) 0.0233(3) Uani 1 1 d . . .
H16 H 0.5077 0.0451 0.2544 0.028 Uiso 1 1 calc R . .
C17 C 0.63383(9) 0.13010(14) 0.26005(8) 0.0205(3) Uani 1 1 d . . .
C18 C 0.68308(10) 0.25147(15) 0.27296(8) 0.0239(3) Uani 1 1 d . . .
H18 H 0.7467 0.2534 0.2709 0.029 Uiso 1 1 calc R . .
C19 C 0.63849(9) 0.36855(15) 0.28872(8) 0.0224(3) Uani 1 1 d . . .
H19 H 0.6723 0.4510 0.2975 0.027 Uiso 1 1 calc R . .
C20 C 0.54518(9) 0.36959(14) 0.29210(8) 0.0198(3) Uani 1 1 d . . .
C21 C 0.45880(10) 0.62474(15) 0.12034(8) 0.0243(3) Uani 1 1 d . . .
H21 H 0.4934 0.7068 0.1236 0.029 Uiso 1 1 calc R . .
C22 C 0.41189(10) 0.57841(16) 0.04967(8) 0.0268(3) Uani 1 1 d . . .
C23 C 0.35602(11) 0.46179(17) 0.04075(9) 0.0322(4) Uani 1 1 d . . .
C24 C 0.31513(12) 0.4227(2) -0.02932(10) 0.0412(4) Uani 1 1 d . . .
H24 H 0.2762 0.3451 -0.0356 0.049 Uiso 1 1 calc R . .
C25 C 0.33102(12) 0.4964(2) -0.08958(10) 0.0407(5) Uani 1 1 d . . .
H25 H 0.3039 0.4677 -0.1372 0.049 Uiso 1 1 calc R . .
C26 C 0.38578(12) 0.6111(2) -0.08158(9) 0.0393(4) Uani 1 1 d . . .
H26 H 0.3961 0.6617 -0.1233 0.047 Uiso 1 1 calc R . .
C27 C 0.42543(11) 0.65147(18) -0.01236(9) 0.0328(4) Uani 1 1 d . . .
H27 H 0.4628 0.7308 -0.0068 0.039 Uiso 1 1 calc R . .
N1 N 0.49911(8) 0.59855(12) 0.24538(6) 0.0204(3) Uani 1 1 d . . .
N2 N 0.45387(8) 0.55551(12) 0.17852(7) 0.0222(3) Uani 1 1 d . . .
O1 O 0.57216(7) 0.79802(10) 0.22044(6) 0.0246(2) Uani 1 1 d . . .
O2 O 0.40567(7) 0.23554(11) 0.27832(7) 0.0308(3) Uani 1 1 d . . .
O3 O 0.12572(8) 0.39610(13) 0.32568(8) 0.0406(3) Uani 1 1 d . . .
H3A H 0.1026(16) 0.453(2) 0.3510(13) 0.058(7) Uiso 1 1 d . . .
O4 O 0.68023(7) 0.01678(11) 0.24444(6) 0.0253(2) Uani 1 1 d . . .
H4A H 0.6414(13) -0.056(2) 0.2388(10) 0.042(5) Uiso 1 1 d . . .
O5 O 0.33996(9) 0.38498(13) 0.09841(8) 0.0454(3) Uani 1 1 d . . .
H5A H 0.3743(17) 0.422(3) 0.1395(14) 0.069(7) Uiso 1 1 d . . .
N3 N 0.57629(16) 0.1774(2) 0.49256(15) 0.0808(7) Uani 1 1 d . . .
C28 C 0.59053(16) 0.1083(2) 0.54227(15) 0.0594(6) Uani 1 1 d . . .
C29 C 0.6081(2) 0.0203(3) 0.60573(14) 0.0723(7) Uani 1 1 d . . .
D29A D 0.5877 0.0656 0.6475 0.108 Uiso 1 1 calc R . .
D29B D 0.6738 0.0017 0.6174 0.108 Uiso 1 1 calc R . .
D29C D 0.5749 -0.0658 0.5954 0.108 Uiso 1 1 calc R . .
N4A N -0.00123(17) 0.4756(2) 0.59285(13) 0.0418(7) Uiso 0.661(3) 1 d P A 1
C30A C 0.06998(18) 0.4898(3) 0.57968(15) 0.0361(7) Uiso 0.661(3) 1 d P A 1
C31A C 0.15926(18) 0.5159(3) 0.56502(15) 0.0715(7) Uiso 0.661(3) 1 d P A 1
D31A D 0.1788 0.6071 0.5830 0.107 Uiso 0.661(3) 1 calc PR A 1
D31B D 0.1593 0.5115 0.5121 0.107 Uiso 0.661(3) 1 calc PR A 1
D31C D 0.2015 0.4473 0.5897 0.107 Uiso 0.661(3) 1 calc PR A 1
N4B N 0.0768(4) 0.5423(5) 0.4377(3) 0.0518(15) Uiso 0.339(3) 1 d P A 2
C30B C 0.1126(4) 0.5412(6) 0.4966(3) 0.0450(15) Uiso 0.339(3) 1 d P A 2
C31B C 0.15926(18) 0.5159(3) 0.56502(15) 0.0715(7) Uiso 0.339(3) 1 d P A 2
D31D D 0.1181 0.5269 0.6011 0.107 Uiso 0.339(3) 1 calc PR A 2
D31E D 0.2102 0.5804 0.5759 0.107 Uiso 0.339(3) 1 calc PR A 2
D31F D 0.1830 0.4224 0.5672 0.107 Uiso 0.339(3) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0209(7) 0.0183(7) 0.0207(7) 0.0009(5) 0.0028(6) -0.0015(5)
C2 0.0168(7) 0.0196(7) 0.0250(7) -0.0031(6) 0.0047(6) 0.0009(5)
C3 0.0244(7) 0.0255(8) 0.0246(8) 0.0019(6) 0.0066(6) -0.0007(6)
C4 0.0289(8) 0.0384(9) 0.0208(8) -0.0009(7) 0.0028(6) -0.0004(7)
C5 0.0307(8) 0.0330(9) 0.0284(9) -0.0073(7) 0.0008(7) -0.0071(7)
C6 0.0272(8) 0.0234(8) 0.0301(8) -0.0019(6) 0.0033(6) -0.0053(6)
C7 0.0197(7) 0.0205(7) 0.0245(8) -0.0013(6) 0.0043(6) 0.0005(5)
C8 0.0169(6) 0.0173(7) 0.0266(8) -0.0014(6) 0.0035(6) 0.0006(5)
C9 0.0197(7) 0.0218(7) 0.0202(7) 0.0028(6) 0.0020(5) -0.0005(5)
C10 0.0260(7) 0.0190(7) 0.0301(8) 0.0010(6) 0.0036(6) -0.0001(6)
C11 0.0246(7) 0.0246(8) 0.0334(9) 0.0013(6) 0.0060(6) 0.0060(6)
C12 0.0180(7) 0.0311(8) 0.0337(9) 0.0024(7) 0.0027(6) 0.0007(6)
C13 0.0217(7) 0.0241(8) 0.0369(9) -0.0040(7) 0.0030(6) -0.0038(6)
C14 0.0214(7) 0.0214(7) 0.0266(8) -0.0019(6) 0.0030(6) 0.0016(6)
C15 0.0176(7) 0.0230(7) 0.0253(8) -0.0012(6) 0.0037(6) -0.0017(5)
C16 0.0231(7) 0.0191(7) 0.0279(8) -0.0028(6) 0.0042(6) -0.0042(6)
C17 0.0218(7) 0.0196(7) 0.0201(7) 0.0007(5) 0.0035(5) 0.0020(5)
C18 0.0187(7) 0.0245(8) 0.0287(8) 0.0008(6) 0.0044(6) -0.0021(6)
C19 0.0210(7) 0.0195(7) 0.0266(8) -0.0002(6) 0.0035(6) -0.0038(6)
C20 0.0214(7) 0.0191(7) 0.0188(7) 0.0006(5) 0.0026(5) -0.0013(5)
C21 0.0227(7) 0.0220(7) 0.0277(8) -0.0009(6) 0.0028(6) 0.0007(6)
C22 0.0240(7) 0.0285(8) 0.0267(8) -0.0035(6) 0.0009(6) 0.0062(6)
C23 0.0297(8) 0.0327(9) 0.0322(9) -0.0028(7) -0.0013(7) 0.0034(7)
C24 0.0337(9) 0.0412(10) 0.0442(11) -0.0137(8) -0.0080(8) 0.0026(8)
C25 0.0367(9) 0.0535(12) 0.0280(9) -0.0125(8) -0.0071(7) 0.0173(8)
C26 0.0402(10) 0.0502(11) 0.0260(9) 0.0000(8) 0.0006(7) 0.0168(8)
C27 0.0335(9) 0.0352(9) 0.0286(9) -0.0003(7) 0.0018(7) 0.0072(7)
N1 0.0210(6) 0.0189(6) 0.0207(6) -0.0006(5) 0.0014(5) -0.0024(5)
N2 0.0210(6) 0.0223(6) 0.0222(6) -0.0025(5) 0.0003(5) 0.0003(5)
O1 0.0260(5) 0.0197(5) 0.0275(6) 0.0028(4) 0.0028(4) -0.0046(4)
O2 0.0180(5) 0.0235(6) 0.0519(7) -0.0119(5) 0.0085(5) -0.0037(4)
O3 0.0196(6) 0.0361(7) 0.0676(9) -0.0073(6) 0.0119(6) -0.0004(5)
O4 0.0220(5) 0.0192(5) 0.0353(6) -0.0025(4) 0.0060(4) 0.0004(4)
O5 0.0514(8) 0.0403(7) 0.0404(8) -0.0006(6) -0.0049(6) -0.0201(6)
N3 0.0882(16) 0.0595(14) 0.0986(18) 0.0154(13) 0.0271(14) 0.0034(12)
C28 0.0602(14) 0.0436(13) 0.0790(17) -0.0057(12) 0.0255(12) -0.0015(10)
C29 0.0884(19) 0.0601(16) 0.0722(17) 0.0021(13) 0.0246(15) 0.0005(13)

_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 N1 1.5029(18) . ?
C1 C20 1.5129(19) . ?
C1 C2 1.5146(19) . ?
C1 C9 1.5155(19) . ?
C2 C3 1.383(2) . ?
C2 C7 1.385(2) . ?
C3 C4 1.389(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.475(2) . ?
C8 O1 1.2353(17) . ?
C8 N1 1.3637(18) . ?
C9 C14 1.389(2) . ?
C9 C10 1.395(2) . ?
C10 C11 1.383(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(2) . ?
C11 H11 0.9500 . ?
C12 O3 1.3614(18) . ?
C12 C13 1.382(2) . ?
C13 C14 1.387(2) . ?
C13 H13 0.9500 . ?
C14 O2 1.3735(17) . ?
C15 O2 1.3800(17) . ?
C15 C20 1.3847(19) . ?
C15 C16 1.387(2) . ?
C16 C17 1.381(2) . ?
C16 H16 0.9500 . ?
C17 O4 1.3609(17) . ?
C17 C18 1.395(2) . ?
C18 C19 1.378(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3955(19) . ?
C19 H19 0.9500 . ?
C21 N2 1.2847(19) . ?
C21 C22 1.453(2) . ?
C21 H21 0.9500 . ?
C22 C27 1.395(2) . ?
C22 C23 1.405(2) . ?
C23 O5 1.358(2) . ?
C23 C24 1.395(2) . ?
C24 C25 1.380(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.379(2) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
N1 N2 1.3762(16) . ?
O3 H3A 0.84(2) . ?
O4 H4A 0.91(2) . ?
O5 H5A 0.92(3) . ?
N3 C28 1.134(3) . ?
C28 C29 1.447(4) . ?
C29 D29A 0.9800 . ?
C29 D29B 0.9800 . ?
C29 D29C 0.9800 . ?
N4A C30A 1.130(3) . ?
C30A C31A 1.417(4) . ?
C31A D31A 0.9800 . ?
C31A D31B 0.9800 . ?
C31A D31C 0.9800 . ?
N4B C30B 1.134(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C20 109.29(11) . . ?
N1 C1 C2 99.90(11) . . ?
C20 C1 C2 111.69(11) . . ?
N1 C1 C9 109.95(11) . . ?
C20 C1 C9 110.74(11) . . ?
C2 C1 C9 114.68(12) . . ?
C3 C2 C7 120.70(13) . . ?
C3 C2 C1 128.67(13) . . ?
C7 C2 C1 110.53(12) . . ?
C2 C3 C4 117.78(14) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C3 C4 C5 121.42(15) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 120.69(14) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 117.54(14) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
C2 C7 C6 121.85(14) . . ?
C2 C7 C8 109.35(12) . . ?
C6 C7 C8 128.72(14) . . ?
O1 C8 N1 125.90(13) . . ?
O1 C8 C7 128.17(13) . . ?
N1 C8 C7 105.91(12) . . ?
C14 C9 C10 117.23(13) . . ?
C14 C9 C1 121.27(13) . . ?
C10 C9 C1 121.41(13) . . ?
C11 C10 C9 122.29(14) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C12 118.77(14) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
O3 C12 C13 116.37(14) . . ?
O3 C12 C11 123.22(14) . . ?
C13 C12 C11 120.40(13) . . ?
C12 C13 C14 119.49(14) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
O2 C14 C13 114.71(13) . . ?
O2 C14 C9 123.48(13) . . ?
C13 C14 C9 121.80(13) . . ?
O2 C15 C20 122.94(13) . . ?
O2 C15 C16 114.77(12) . . ?
C20 C15 C16 122.30(13) . . ?
C17 C16 C15 119.07(13) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
O4 C17 C16 122.24(13) . . ?
O4 C17 C18 117.51(12) . . ?
C16 C17 C18 120.25(13) . . ?
C19 C18 C17 119.27(13) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 121.93(13) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 H19 119.0 . . ?
C15 C20 C19 117.19(13) . . ?
C15 C20 C1 121.96(12) . . ?
C19 C20 C1 120.82(12) . . ?
N2 C21 C22 120.48(14) . . ?
N2 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C27 C22 C23 118.70(15) . . ?
C27 C22 C21 118.05(15) . . ?
C23 C22 C21 123.22(15) . . ?
O5 C23 C24 118.33(16) . . ?
O5 C23 C22 122.17(15) . . ?
C24 C23 C22 119.50(16) . . ?
C25 C24 C23 120.26(17) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 120.82(16) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 119.24(17) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C22 121.47(17) . . ?
C26 C27 H27 119.3 . . ?
C22 C27 H27 119.3 . . ?
C8 N1 N2 130.37(12) . . ?
C8 N1 C1 113.97(11) . . ?
N2 N1 C1 115.35(11) . . ?
C21 N2 N1 120.51(12) . . ?
C14 O2 C15 118.51(11) . . ?
C12 O3 H3A 110.5(16) . . ?
C17 O4 H4A 109.2(12) . . ?
C23 O5 H5A 106.7(15) . . ?
N3 C28 C29 179.6(3) . . ?
C28 C29 D29A 109.5 . . ?
C28 C29 D29B 109.5 . . ?
D29A C29 D29B 109.5 . . ?
C28 C29 D29C 109.5 . . ?
D29A C29 D29C 109.5 . . ?
D29B C29 D29C 109.5 . . ?
N4A C30A C31A 176.5(3) . . ?
C30A C31A D31A 109.5 . . ?
C30A C31A D31B 109.5 . . ?
D31A C31A D31B 109.5 . . ?
C30A C31A D31C 109.5 . . ?
D31A C31A D31C 109.5 . . ?
D31B C31A D31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -178.90(14) . . . . ?
C20 C1 C2 C3 -63.41(18) . . . . ?
C9 C1 C2 C3 63.62(19) . . . . ?
N1 C1 C2 C7 -2.47(14) . . . . ?
C20 C1 C2 C7 113.02(13) . . . . ?
C9 C1 C2 C7 -119.95(13) . . . . ?
C7 C2 C3 C4 1.6(2) . . . . ?
C1 C2 C3 C4 177.69(14) . . . . ?
C2 C3 C4 C5 -0.9(2) . . . . ?
C3 C4 C5 C6 -0.3(2) . . . . ?
C4 C5 C6 C7 0.7(2) . . . . ?
C3 C2 C7 C6 -1.2(2) . . . . ?
C1 C2 C7 C6 -177.95(13) . . . . ?
C3 C2 C7 C8 175.88(13) . . . . ?
C1 C2 C7 C8 -0.88(15) . . . . ?
C5 C6 C7 C2 0.0(2) . . . . ?
C5 C6 C7 C8 -176.45(14) . . . . ?
C2 C7 C8 O1 -174.16(14) . . . . ?
C6 C7 C8 O1 2.6(2) . . . . ?
C2 C7 C8 N1 4.25(15) . . . . ?
C6 C7 C8 N1 -178.93(14) . . . . ?
N1 C1 C9 C14 110.02(15) . . . . ?
C20 C1 C9 C14 -10.87(19) . . . . ?
C2 C1 C9 C14 -138.38(14) . . . . ?
N1 C1 C9 C10 -66.34(17) . . . . ?
C20 C1 C9 C10 172.77(13) . . . . ?
C2 C1 C9 C10 45.26(18) . . . . ?
C14 C9 C10 C11 -1.2(2) . . . . ?
C1 C9 C10 C11 175.35(14) . . . . ?
C9 C10 C11 C12 0.2(2) . . . . ?
C10 C11 C12 O3 -177.97(15) . . . . ?
C10 C11 C12 C13 1.0(2) . . . . ?
O3 C12 C13 C14 177.81(14) . . . . ?
C11 C12 C13 C14 -1.2(2) . . . . ?
C12 C13 C14 O2 179.83(14) . . . . ?
C12 C13 C14 C9 0.2(2) . . . . ?
C10 C9 C14 O2 -178.64(13) . . . . ?
C1 C9 C14 O2 4.9(2) . . . . ?
C10 C9 C14 C13 0.9(2) . . . . ?
C1 C9 C14 C13 -175.58(14) . . . . ?
O2 C15 C16 C17 178.63(13) . . . . ?
C20 C15 C16 C17 -1.1(2) . . . . ?
C15 C16 C17 O4 -179.22(13) . . . . ?
C15 C16 C17 C18 0.4(2) . . . . ?
O4 C17 C18 C19 179.79(13) . . . . ?
C16 C17 C18 C19 0.2(2) . . . . ?
C17 C18 C19 C20 -0.1(2) . . . . ?
O2 C15 C20 C19 -178.54(13) . . . . ?
C16 C15 C20 C19 1.1(2) . . . . ?
O2 C15 C20 C1 -0.7(2) . . . . ?
C16 C15 C20 C1 178.94(14) . . . . ?
C18 C19 C20 C15 -0.5(2) . . . . ?
C18 C19 C20 C1 -178.39(13) . . . . ?
N1 C1 C20 C15 -112.34(15) . . . . ?
C2 C1 C20 C15 138.07(14) . . . . ?
C9 C1 C20 C15 8.94(19) . . . . ?
N1 C1 C20 C19 65.40(16) . . . . ?
C2 C1 C20 C19 -44.19(18) . . . . ?
C9 C1 C20 C19 -173.32(13) . . . . ?
N2 C21 C22 C27 -174.99(14) . . . . ?
N2 C21 C22 C23 3.1(2) . . . . ?
C27 C22 C23 O5 179.65(15) . . . . ?
C21 C22 C23 O5 1.6(2) . . . . ?
C27 C22 C23 C24 -0.5(2) . . . . ?
C21 C22 C23 C24 -178.55(15) . . . . ?
O5 C23 C24 C25 -178.75(16) . . . . ?
C22 C23 C24 C25 1.4(3) . . . . ?
C23 C24 C25 C26 -1.4(3) . . . . ?
C24 C25 C26 C27 0.5(3) . . . . ?
C25 C26 C27 C22 0.4(2) . . . . ?
C23 C22 C27 C26 -0.4(2) . . . . ?
C21 C22 C27 C26 177.74(14) . . . . ?
O1 C8 N1 N2 -0.8(2) . . . . ?
C7 C8 N1 N2 -179.29(13) . . . . ?
O1 C8 N1 C1 172.31(13) . . . . ?
C7 C8 N1 C1 -6.16(15) . . . . ?
C20 C1 N1 C8 -111.86(13) . . . . ?
C2 C1 N1 C8 5.44(14) . . . . ?
C9 C1 N1 C8 126.39(12) . . . . ?
C20 C1 N1 N2 62.36(14) . . . . ?
C2 C1 N1 N2 179.66(11) . . . . ?
C9 C1 N1 N2 -59.39(15) . . . . ?
C22 C21 N2 N1 179.29(12) . . . . ?
C8 N1 N2 C21 0.2(2) . . . . ?
C1 N1 N2 C21 -172.83(12) . . . . ?
C13 C14 O2 C15 -175.12(13) . . . . ?
C9 C14 O2 C15 4.5(2) . . . . ?
C20 C15 O2 C14 -6.6(2) . . . . ?
C16 C15 O2 C14 173.73(13) . . . . ?

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
O5 H5A N2 0.92(3) 1.83(3) 2.6529(17) 148(2) .
O3 H3A N4B 0.84(2) 1.92(2) 2.714(6) 158(2) .
O3 H3A N4A 0.84(2) 2.08(2) 2.856(3) 154(2) 3_566
O4 H4A O1 0.91(2) 1.76(2) 2.6692(14) 174.1(18) 1_545

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.043