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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_jak041

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H48 Cu2 N12 O24'
_chemical_formula_weight         1640.34

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'
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                   8.7906(18)
_cell_length_b                   9.799(2)
_cell_length_c                   20.206(4)
_cell_angle_alpha                101.78(3)
_cell_angle_beta                 95.46(3)
_cell_angle_gamma                99.72(3)
_cell_volume                     1664.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    5608
_cell_measurement_theta_min      1.7317
_cell_measurement_theta_max      32.0330

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             838
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7875
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      108(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 Saturn 724'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26049
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5862
_reflns_number_gt                5389
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. Disordered NO2 and Py groups.
 Carbon atoms on lower occupancy py disorder isotropic all other non-H atoms 
 ANIS all H calc and ride.
;

_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)+(0.0395P)²+1.7839P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5862
_refine_ls_number_parameters     568
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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 0.31732(4) -0.08630(3) 0.558699(15) 0.01761(11) Uani 1 1 d . . .
N1 N 1.3374(5) 0.7085(4) 1.0195(2) 0.0356(10) Uani 0.65 1 d P A 1
O1 O 1.4701(4) 0.7428(4) 1.00796(19) 0.0526(10) Uani 0.65 1 d P A 1
O2 O 1.2948(4) 0.7426(3) 1.07511(15) 0.0349(8) Uani 0.65 1 d P A 1
O10 O 1.1945(8) 0.7931(6) 1.0920(3) 0.0318(14) Uani 0.35 1 d P B 2
N20 N 1.0921(9) 0.8300(7) 1.0586(4) 0.0317(17) Uani 0.35 1 d P B 2
O11 O 1.0618(8) 0.9499(7) 1.0753(4) 0.0481(18) Uani 0.35 1 d P B 2
N2 N 0.7600(3) 0.3512(2) 0.79299(11) 0.0213(5) Uani 1 1 d . A .
N3 N 0.4619(3) 0.0584(2) 0.63422(11) 0.0207(5) Uani 1 1 d . . .
O3 O 0.5589(2) 0.4498(2) 0.82928(11) 0.0354(5) Uani 1 1 d . . .
O4 O 0.9615(2) 0.2565(2) 0.75664(10) 0.0339(5) Uani 1 1 d . A .
C1 C 0.6966(3) 0.4486(3) 0.83685(14) 0.0252(6) Uani 1 1 d . . .
C2 C 0.8061(3) 0.5481(3) 0.89264(13) 0.0245(6) Uani 1 1 d . A .
C3 C 0.7500(4) 0.6484(3) 0.93569(15) 0.0323(7) Uani 1 1 d . . .
H3 H 0.6433 0.6548 0.9285 0.039 Uiso 1 1 calc R . .
C4 C 0.8495(4) 0.7417(3) 0.99024(16) 0.0350(7) Uani 1 1 d . B .
H4 H 0.8099 0.8115 1.0200 0.042 Uiso 1 1 calc R . .
C5 C 1.0018(4) 0.7337(3) 1.00117(14) 0.0282(7) Uani 1 1 d . . .
H5 H 1.0669 0.7973 1.0390 0.034 Uiso 0.35 1 calc PR B 1
C6 C 1.0661(3) 0.6336(3) 0.95784(14) 0.0263(6) Uani 1 1 d . A .
C7 C 1.2240(3) 0.6201(3) 0.96241(14) 0.0291(7) Uani 1 1 d . . .
H7 H 1.2950 0.6798 0.9995 0.035 Uiso 0.65 1 calc PR A 2
C8 C 1.2787(4) 0.5261(3) 0.91648(15) 0.0336(7) Uani 1 1 d . A .
H8 H 1.3863 0.5220 0.9212 0.040 Uiso 1 1 calc R . .
C9 C 1.1764(3) 0.4346(3) 0.86191(15) 0.0307(7) Uani 1 1 d . . .
H9 H 1.2145 0.3687 0.8294 0.037 Uiso 1 1 calc R A .
C10 C 1.0223(3) 0.4406(3) 0.85555(13) 0.0247(6) Uani 1 1 d . A .
C11 C 0.9639(3) 0.5394(3) 0.90216(13) 0.0235(6) Uani 1 1 d . . .
C12 C 0.9165(3) 0.3418(3) 0.79777(13) 0.0253(6) Uani 1 1 d . . .
C13 C 0.6561(3) 0.2523(3) 0.73881(13) 0.0213(6) Uani 1 1 d . . .
C14 C 0.6586(4) 0.2665(4) 0.67361(16) 0.0193(7) Uiso 0.80 1 d PD A 1
H14 H 0.7264 0.3434 0.6633 0.023 Uiso 0.80 1 calc PR A 1
C15 C 0.5604(4) 0.1667(4) 0.62258(17) 0.0203(7) Uiso 0.80 1 d PD A 1
H15 H 0.5633 0.1760 0.5768 0.024 Uiso 0.80 1 calc PR A 1
C16 C 0.4561(4) 0.0495(4) 0.69988(17) 0.0260(8) Uiso 0.80 1 d PD A 1
H16 H 0.3831 -0.0250 0.7092 0.031 Uiso 0.80 1 calc PR A 1
C17 C 0.5511(4) 0.1438(4) 0.75364(18) 0.0259(8) Uiso 0.80 1 d PD A 1
H17 H 0.5451 0.1350 0.7993 0.031 Uiso 0.80 1 calc PR A 1
C140 C 0.5943(18) 0.2920(17) 0.6822(7) 0.028(3) Uiso 0.20 1 d PD A 2
H140 H 0.6198 0.3875 0.6776 0.034 Uiso 0.20 1 calc PR A 2
C150 C 0.4954(17) 0.1918(15) 0.6326(7) 0.024(3) Uiso 0.20 1 d PD A 2
H150 H 0.4488 0.2212 0.5949 0.029 Uiso 0.20 1 calc PR A 2
C160 C 0.5409(16) 0.0163(15) 0.6820(7) 0.026(3) Uiso 0.20 1 d PD A 2
H160 H 0.5283 -0.0827 0.6801 0.032 Uiso 0.20 1 calc PR A 2
C170 C 0.6410(18) 0.1086(16) 0.7348(8) 0.032(3) Uiso 0.20 1 d PD A 2
H170 H 0.6986 0.0740 0.7678 0.039 Uiso 0.20 1 calc PR A 2
N22 N -0.1391(2) -0.5200(2) 0.32719(11) 0.0183(5) Uani 1 1 d . C .
N23 N 0.1686(2) -0.2306(2) 0.48465(10) 0.0175(5) Uani 1 1 d . . .
N21 N -0.7232(5) -0.9357(4) 0.1222(2) 0.0342(9) Uani 0.65 1 d P C 1
O21 O -0.8478(4) -0.9846(4) 0.13835(19) 0.0517(11) Uani 0.65 1 d P C 1
O22 O -0.6928(5) -0.9590(4) 0.06278(18) 0.0368(8) Uani 0.65 1 d P C 1
N200 N -0.4898(9) -1.0161(8) 0.0723(4) 0.0374(19) Uani 0.35 1 d P D 2
O200 O -0.4524(8) -1.1331(7) 0.0580(4) 0.0507(19) Uani 0.35 1 d P D 2
O201 O -0.6056(9) -0.9861(7) 0.0443(3) 0.0409(17) Uani 0.35 1 d P D 2
O23 O 0.0649(2) -0.58184(19) 0.27596(9) 0.0247(4) Uani 1 1 d . . .
O24 O -0.3443(2) -0.4710(2) 0.38112(10) 0.0352(5) Uani 1 1 d . C .
C21 C -0.0742(3) -0.6018(3) 0.27699(13) 0.0207(6) Uani 1 1 d . . .
C22 C -0.1844(3) -0.7097(3) 0.22397(13) 0.0214(6) Uani 1 1 d . C .
C23 C -0.1254(3) -0.7918(3) 0.17357(14) 0.0257(6) Uani 1 1 d . . .
H23 H -0.0161 -0.7791 0.1728 0.031 Uiso 1 1 calc R . .
C24 C -0.2264(4) -0.8947(3) 0.12308(15) 0.0325(7) Uani 1 1 d . D .
H24 H -0.1849 -0.9537 0.0888 0.039 Uiso 1 1 calc R . .
C25 C -0.3829(4) -0.9115(3) 0.12248(15) 0.0312(7) Uani 1 1 d . . .
H25 H -0.4491 -0.9817 0.0873 0.037 Uiso 0.65 1 calc PR D 1
C26 C -0.4497(3) -0.8277(3) 0.17251(14) 0.0267(6) Uani 1 1 d . C .
C27 C -0.6101(3) -0.8392(3) 0.17792(15) 0.0302(7) Uani 1 1 d . . .
H27 H -0.6829 -0.9051 0.1435 0.036 Uiso 0.35 1 calc PR C 2
C28 C -0.6642(4) -0.7598(3) 0.23033(16) 0.0344(7) Uani 1 1 d . C .
H28 H -0.7731 -0.7709 0.2322 0.041 Uiso 1 1 calc R . .
C29 C -0.5609(3) -0.6621(3) 0.28134(15) 0.0316(7) Uani 1 1 d . . .
H29 H -0.5994 -0.6075 0.3182 0.038 Uiso 1 1 calc R C .
C30 C -0.4045(3) -0.6442(3) 0.27872(13) 0.0236(6) Uani 1 1 d . C .
C31 C -0.3463(3) -0.7264(3) 0.22503(13) 0.0214(6) Uani 1 1 d . . .
C32 C -0.2982(3) -0.5393(3) 0.33356(13) 0.0229(6) Uani 1 1 d . . .
C33 C -0.0344(3) -0.4202(3) 0.38148(12) 0.0185(5) Uani 1 1 d . . .
C34 C 0.0685(3) -0.4676(3) 0.42268(13) 0.0209(6) Uani 1 1 d . A .
H34 H 0.0700 -0.5661 0.4163 0.025 Uiso 1 1 calc R . .
C35 C 0.1692(3) -0.3700(3) 0.47322(13) 0.0200(6) Uani 1 1 d . A .
H35 H 0.2420 -0.4025 0.5011 0.024 Uiso 1 1 calc R . .
C36 C 0.0648(3) -0.1867(3) 0.44565(13) 0.0190(5) Uani 1 1 d . A .
H36 H 0.0618 -0.0882 0.4543 0.023 Uiso 1 1 calc R . .
C37 C -0.0385(3) -0.2777(3) 0.39326(13) 0.0193(6) Uani 1 1 d . A .
H37 H -0.1106 -0.2430 0.3660 0.023 Uiso 1 1 calc R . .
O40 O 0.1395(2) -0.01899(18) 0.59721(9) 0.0216(4) Uani 1 1 d . . .
O41 O 0.1549(2) -0.2009(2) 0.64485(9) 0.0275(4) Uani 1 1 d . . .
C40 C 0.0941(3) -0.0999(3) 0.63634(13) 0.0219(6) Uani 1 1 d . A .
C41 C -0.0383(4) -0.0652(3) 0.67461(16) 0.0352(7) Uani 1 1 d . . .
H41A H -0.0989 -0.1528 0.6823 0.042 Uiso 1 1 calc R A .
H41B H -0.1057 -0.0204 0.6478 0.042 Uiso 1 1 calc R . .
H41C H 0.0033 0.0001 0.7186 0.042 Uiso 1 1 calc R . .
O50 O 0.4728(2) -0.20342(18) 0.54584(9) 0.0222(4) Uani 1 1 d . . .
O51 O 0.6659(2) -0.06002(19) 0.51596(9) 0.0247(4) Uani 1 1 d . . .
C50 C 0.6115(3) -0.1703(3) 0.53252(12) 0.0196(6) Uani 1 1 d . A .
C51 C 0.7087(3) -0.2810(3) 0.53650(15) 0.0281(6) Uani 1 1 d . . .
H51A H 0.6735 -0.3615 0.4973 0.034 Uiso 1 1 calc R A .
H51B H 0.6979 -0.3136 0.5788 0.034 Uiso 1 1 calc R . .
H51C H 0.8181 -0.2401 0.5359 0.034 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O50 1.9310(18) . y
Cu1 O40 1.9632(19) . y
Cu1 N23 2.021(2) . y
Cu1 N3 2.023(2) . y
Cu1 O51 2.2819(19) 2_656 y
N1 O1 1.216(5) . ?
N1 O2 1.218(5) . ?
N1 C7 1.469(5) . ?
O10 N20 1.221(9) . ?
N20 O11 1.235(9) . ?
N20 C5 1.411(7) . ?
N2 C12 1.390(4) . ?
N2 C1 1.391(3) . ?
N2 C13 1.432(3) . ?
N3 C150 1.298(14) . ?
N3 C160 1.310(14) . ?
N3 C15 1.328(4) . ?
N3 C16 1.352(4) . ?
O3 C1 1.207(3) . ?
O4 C12 1.199(3) . ?
C1 C2 1.475(4) . ?
C2 C3 1.365(4) . ?
C2 C11 1.402(4) . ?
C3 C4 1.397(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.354(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(4) . ?
C6 C11 1.424(4) . ?
C7 C8 1.352(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.401(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.360(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.406(4) . ?
C10 C12 1.481(4) . ?
C13 C14 1.355(4) . ?
C13 C140 1.376(15) . ?
C13 C170 1.377(15) . ?
C13 C17 1.387(4) . ?
C14 C15 1.377(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.374(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C140 C150 1.37(2) . ?
C140 H140 0.9500 . ?
C150 H150 0.9500 . ?
C160 C170 1.37(2) . ?
C160 H160 0.9500 . ?
C170 H170 0.9500 . ?
N22 C21 1.389(3) . ?
N22 C32 1.401(3) . ?
N22 C33 1.439(3) . ?
N23 C36 1.332(3) . ?
N23 C35 1.339(3) . ?
N21 O21 1.222(5) . ?
N21 O22 1.238(5) . ?
N21 C27 1.478(4) . ?
N200 O201 1.226(11) . ?
N200 O200 1.231(10) . ?
N200 C25 1.425(8) . ?
O23 C21 1.208(3) . ?
O24 C32 1.200(3) . ?
C21 C22 1.483(4) . ?
C22 C23 1.364(4) . ?
C22 C31 1.408(4) . ?
C23 C24 1.397(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.357(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.406(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.413(4) . ?
C26 C31 1.421(4) . ?
C27 C28 1.355(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.364(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.405(4) . ?
C30 C32 1.474(4) . ?
C33 C34 1.372(4) . ?
C33 C37 1.375(4) . ?
C34 C35 1.373(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.378(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
O40 C40 1.274(3) . ?
O41 C40 1.235(3) . ?
C40 C41 1.505(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
O50 C50 1.276(3) . ?
O51 C50 1.229(3) . ?
O51 Cu1 2.2819(19) 2_656 ?
C50 C51 1.499(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O50 Cu1 O40 156.39(8) . . y
O50 Cu1 N23 89.51(8) . . y
O40 Cu1 N23 89.71(8) . . y
O50 Cu1 N3 91.48(9) . . y
O40 Cu1 N3 88.99(9) . . y
N23 Cu1 N3 178.61(9) . . y
O50 Cu1 O51 108.96(8) . 2_656 y
O40 Cu1 O51 94.57(8) . 2_656 y
N23 Cu1 O51 87.20(8) . 2_656 y
N3 Cu1 O51 93.40(8) . 2_656 y
O1 N1 O2 123.9(4) . . ?
O1 N1 C7 117.1(4) . . ?
O2 N1 C7 119.0(4) . . ?
O10 N20 O11 121.1(7) . . ?
O10 N20 C5 120.2(6) . . ?
O11 N20 C5 118.6(7) . . ?
C12 N2 C1 125.1(2) . . ?
C12 N2 C13 117.3(2) . . ?
C1 N2 C13 117.6(2) . . ?
C150 N3 C160 117.5(9) . . ?
C150 N3 C15 30.4(6) . . ?
C160 N3 C15 104.0(7) . . ?
C150 N3 C16 108.2(6) . . ?
C160 N3 C16 41.2(6) . . ?
C15 N3 C16 117.5(3) . . ?
C150 N3 Cu1 121.9(6) . . ?
C160 N3 Cu1 120.0(7) . . ?
C15 N3 Cu1 122.7(2) . . ?
C16 N3 Cu1 119.7(2) . . ?
O3 C1 N2 121.1(2) . . ?
O3 C1 C2 122.5(3) . . ?
N2 C1 C2 116.4(2) . . ?
C3 C2 C11 120.3(3) . . ?
C3 C2 C1 118.5(3) . . ?
C11 C2 C1 121.2(2) . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 N20 116.5(4) . . ?
C6 C5 N20 121.8(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
N20 C5 H5 2.7 . . ?
C5 C6 C7 126.5(3) . . ?
C5 C6 C11 117.3(3) . . ?
C7 C6 C11 116.2(3) . . ?
C8 C7 C6 123.0(3) . . ?
C8 C7 N1 116.6(3) . . ?
C6 C7 N1 120.4(3) . . ?
C8 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
N1 C7 H7 2.1 . . ?
C7 C8 C9 119.9(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.0(3) . . ?
C9 C10 C12 118.7(3) . . ?
C11 C10 C12 120.2(3) . . ?
C2 C11 C10 120.0(2) . . ?
C2 C11 C6 120.0(3) . . ?
C10 C11 C6 120.0(3) . . ?
O4 C12 N2 120.6(3) . . ?
O4 C12 C10 122.4(3) . . ?
N2 C12 C10 117.0(2) . . ?
C14 C13 C140 28.8(6) . . ?
C14 C13 C170 104.8(7) . . ?
C140 C13 C170 116.5(9) . . ?
C14 C13 C17 120.3(3) . . ?
C140 C13 C17 109.9(7) . . ?
C170 C13 C17 42.1(6) . . ?
C14 C13 N2 120.0(3) . . ?
C140 C13 N2 122.1(7) . . ?
C170 C13 N2 120.0(7) . . ?
C17 C13 N2 119.6(3) . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.2(3) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N3 C16 C17 122.8(3) . . ?
N3 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C16 C17 C13 117.6(3) . . ?
C16 C17 H17 121.2 . . ?
C13 C17 H17 121.2 . . ?
C150 C140 C13 118.8(13) . . ?
C150 C140 H140 120.6 . . ?
C13 C140 H140 120.6 . . ?
N3 C150 C140 123.5(13) . . ?
N3 C150 H150 118.2 . . ?
C140 C150 H150 118.2 . . ?
N3 C160 C170 123.1(13) . . ?
N3 C160 H160 118.5 . . ?
C170 C160 H160 118.5 . . ?
C160 C170 C13 118.6(13) . . ?
C160 C170 H170 120.7 . . ?
C13 C170 H170 120.7 . . ?
C21 N22 C32 124.7(2) . . ?
C21 N22 C33 117.7(2) . . ?
C32 N22 C33 117.1(2) . . ?
C36 N23 C35 118.1(2) . . ?
C36 N23 Cu1 119.30(17) . . ?
C35 N23 Cu1 122.59(17) . . ?
O21 N21 O22 123.4(4) . . ?
O21 N21 C27 115.8(4) . . ?
O22 N21 C27 120.8(4) . . ?
O201 N200 O200 124.1(7) . . ?
O201 N200 C25 120.7(7) . . ?
O200 N200 C25 115.1(7) . . ?
O23 C21 N22 121.0(2) . . ?
O23 C21 C22 122.3(2) . . ?
N22 C21 C22 116.6(2) . . ?
C23 C22 C31 120.6(2) . . ?
C23 C22 C21 118.5(3) . . ?
C31 C22 C21 120.9(2) . . ?
C22 C23 C24 119.8(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 120.8(3) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 121.7(3) . . ?
C24 C25 N200 122.5(4) . . ?
C26 C25 N200 115.8(4) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
N200 C25 H25 3.5 . . ?
C25 C26 C27 126.3(3) . . ?
C25 C26 C31 117.3(3) . . ?
C27 C26 C31 116.3(3) . . ?
C28 C27 C26 122.5(3) . . ?
C28 C27 N21 118.9(3) . . ?
C26 C27 N21 118.5(3) . . ?
C28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
N21 C27 H27 3.1 . . ?
C27 C28 C29 120.2(3) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 120.3(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 120.3(3) . . ?
C29 C30 C32 118.9(3) . . ?
C31 C30 C32 120.8(2) . . ?
C30 C31 C22 119.7(2) . . ?
C30 C31 C26 120.4(3) . . ?
C22 C31 C26 119.9(2) . . ?
O24 C32 N22 120.8(2) . . ?
O24 C32 C30 122.2(3) . . ?
N22 C32 C30 116.9(2) . . ?
C34 C33 C37 119.6(2) . . ?
C34 C33 N22 120.0(2) . . ?
C37 C33 N22 120.5(2) . . ?
C33 C34 C35 118.8(2) . . ?
C33 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
N23 C35 C34 122.4(2) . . ?
N23 C35 H35 118.8 . . ?
C34 C35 H35 118.8 . . ?
N23 C36 C37 122.9(2) . . ?
N23 C36 H36 118.5 . . ?
C37 C36 H36 118.5 . . ?
C33 C37 C36 118.2(2) . . ?
C33 C37 H37 120.9 . . ?
C36 C37 H37 120.9 . . ?
C40 O40 Cu1 106.69(16) . . ?
O41 C40 O40 123.4(3) . . ?
O41 C40 C41 119.9(3) . . ?
O40 C40 C41 116.7(2) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C50 O50 Cu1 128.80(17) . . ?
C50 O51 Cu1 152.38(17) . 2_656 ?
O51 C50 O50 125.4(2) . . ?
O51 C50 C51 120.2(3) . . ?
O50 C50 C51 114.4(2) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 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
O50 Cu1 N3 C150 125.2(8) . . . . ?
O40 Cu1 N3 C150 -78.4(8) . . . . ?
N23 Cu1 N3 C150 -100(4) . . . . ?
O51 Cu1 N3 C150 16.1(8) 2_656 . . . ?
O50 Cu1 N3 C160 -45.7(7) . . . . ?
O40 Cu1 N3 C160 110.7(7) . . . . ?
N23 Cu1 N3 C160 90(4) . . . . ?
O51 Cu1 N3 C160 -154.8(7) 2_656 . . . ?
O50 Cu1 N3 C15 89.0(2) . . . . ?
O40 Cu1 N3 C15 -114.6(2) . . . . ?
N23 Cu1 N3 C15 -136(3) . . . . ?
O51 Cu1 N3 C15 -20.1(2) 2_656 . . . ?
O50 Cu1 N3 C16 -93.5(2) . . . . ?
O40 Cu1 N3 C16 62.8(2) . . . . ?
N23 Cu1 N3 C16 42(4) . . . . ?
O51 Cu1 N3 C16 157.4(2) 2_656 . . . ?
C12 N2 C1 O3 -179.9(3) . . . . ?
C13 N2 C1 O3 -0.2(4) . . . . ?
C12 N2 C1 C2 -0.4(4) . . . . ?
C13 N2 C1 C2 179.3(2) . . . . ?
O3 C1 C2 C3 -2.4(4) . . . . ?
N2 C1 C2 C3 178.0(3) . . . . ?
O3 C1 C2 C11 176.7(3) . . . . ?
N2 C1 C2 C11 -2.8(4) . . . . ?
C11 C2 C3 C4 -1.0(5) . . . . ?
C1 C2 C3 C4 178.2(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C3 C4 C5 C6 1.0(5) . . . . ?
C3 C4 C5 N20 -178.4(4) . . . . ?
O10 N20 C5 C4 143.4(6) . . . . ?
O11 N20 C5 C4 -34.2(9) . . . . ?
O10 N20 C5 C6 -36.0(9) . . . . ?
O11 N20 C5 C6 146.4(6) . . . . ?
C4 C5 C6 C7 176.8(3) . . . . ?
N20 C5 C6 C7 -3.8(6) . . . . ?
C4 C5 C6 C11 -0.6(4) . . . . ?
N20 C5 C6 C11 178.7(4) . . . . ?
C5 C6 C7 C8 -176.2(3) . . . . ?
C11 C6 C7 C8 1.3(4) . . . . ?
C5 C6 C7 N1 4.9(5) . . . . ?
C11 C6 C7 N1 -177.6(3) . . . . ?
O1 N1 C7 C8 33.6(5) . . . . ?
O2 N1 C7 C8 -146.1(4) . . . . ?
O1 N1 C7 C6 -147.4(4) . . . . ?
O2 N1 C7 C6 32.9(5) . . . . ?
C6 C7 C8 C9 -1.2(5) . . . . ?
N1 C7 C8 C9 177.8(3) . . . . ?
C7 C8 C9 C10 -0.2(5) . . . . ?
C8 C9 C10 C11 1.4(4) . . . . ?
C8 C9 C10 C12 -179.4(3) . . . . ?
C3 C2 C11 C10 -176.7(3) . . . . ?
C1 C2 C11 C10 4.1(4) . . . . ?
C3 C2 C11 C6 1.4(4) . . . . ?
C1 C2 C11 C6 -177.8(3) . . . . ?
C9 C10 C11 C2 176.9(3) . . . . ?
C12 C10 C11 C2 -2.2(4) . . . . ?
C9 C10 C11 C6 -1.2(4) . . . . ?
C12 C10 C11 C6 179.6(2) . . . . ?
C5 C6 C11 C2 -0.5(4) . . . . ?
C7 C6 C11 C2 -178.3(3) . . . . ?
C5 C6 C11 C10 177.6(3) . . . . ?
C7 C6 C11 C10 -0.1(4) . . . . ?
C1 N2 C12 O4 -178.2(3) . . . . ?
C13 N2 C12 O4 2.1(4) . . . . ?
C1 N2 C12 C10 2.1(4) . . . . ?
C13 N2 C12 C10 -177.6(2) . . . . ?
C9 C10 C12 O4 0.4(4) . . . . ?
C11 C10 C12 O4 179.6(3) . . . . ?
C9 C10 C12 N2 -179.9(3) . . . . ?
C11 C10 C12 N2 -0.8(4) . . . . ?
C12 N2 C13 C14 -72.5(4) . . . . ?
C1 N2 C13 C14 107.8(3) . . . . ?
C12 N2 C13 C140 -106.2(8) . . . . ?
C1 N2 C13 C140 74.1(8) . . . . ?
C12 N2 C13 C170 59.8(8) . . . . ?
C1 N2 C13 C170 -119.9(7) . . . . ?
C12 N2 C13 C17 108.7(3) . . . . ?
C1 N2 C13 C17 -71.0(3) . . . . ?
C140 C13 C14 C15 -79.1(14) . . . . ?
C170 C13 C14 C15 39.4(8) . . . . ?
C17 C13 C14 C15 -3.3(5) . . . . ?
N2 C13 C14 C15 178.0(3) . . . . ?
C150 N3 C15 C14 81.1(13) . . . . ?
C160 N3 C15 C14 -39.9(8) . . . . ?
C16 N3 C15 C14 2.0(5) . . . . ?
Cu1 N3 C15 C14 179.5(3) . . . . ?
C13 C14 C15 N3 0.9(5) . . . . ?
C150 N3 C16 C17 -34.2(8) . . . . ?
C160 N3 C16 C17 77.0(10) . . . . ?
C15 N3 C16 C17 -2.6(5) . . . . ?
Cu1 N3 C16 C17 179.8(3) . . . . ?
N3 C16 C17 C13 0.3(5) . . . . ?
C14 C13 C17 C16 2.7(5) . . . . ?
C140 C13 C17 C16 32.5(8) . . . . ?
C170 C13 C17 C16 -75.4(10) . . . . ?
N2 C13 C17 C16 -178.6(3) . . . . ?
C14 C13 C140 C150 85.3(17) . . . . ?
C170 C13 C140 C150 13.7(18) . . . . ?
C17 C13 C140 C150 -31.7(14) . . . . ?
N2 C13 C140 C150 -179.8(9) . . . . ?
C160 N3 C150 C140 -7.9(18) . . . . ?
C15 N3 C150 C140 -77.7(16) . . . . ?
C16 N3 C150 C140 35.8(15) . . . . ?
Cu1 N3 C150 C140 -179.1(10) . . . . ?
C13 C140 C150 N3 -3(2) . . . . ?
C150 N3 C160 C170 8.7(18) . . . . ?
C15 N3 C160 C170 38.1(13) . . . . ?
C16 N3 C160 C170 -77.8(13) . . . . ?
Cu1 N3 C160 C170 -180.0(10) . . . . ?
N3 C160 C170 C13 1.8(19) . . . . ?
C14 C13 C170 C160 -41.1(13) . . . . ?
C140 C13 C170 C160 -12.9(17) . . . . ?
C17 C13 C170 C160 78.0(13) . . . . ?
N2 C13 C170 C160 -179.7(9) . . . . ?
O50 Cu1 N23 C36 -148.2(2) . . . . ?
O40 Cu1 N23 C36 55.41(19) . . . . ?
N3 Cu1 N23 C36 77(4) . . . . ?
O51 Cu1 N23 C36 -39.18(19) 2_656 . . . ?
O50 Cu1 N23 C35 32.3(2) . . . . ?
O40 Cu1 N23 C35 -124.1(2) . . . . ?
N3 Cu1 N23 C35 -103(3) . . . . ?
O51 Cu1 N23 C35 141.3(2) 2_656 . . . ?
C32 N22 C21 O23 -177.6(2) . . . . ?
C33 N22 C21 O23 -5.9(4) . . . . ?
C32 N22 C21 C22 4.7(4) . . . . ?
C33 N22 C21 C22 176.4(2) . . . . ?
O23 C21 C22 C23 2.0(4) . . . . ?
N22 C21 C22 C23 179.7(2) . . . . ?
O23 C21 C22 C31 -177.3(3) . . . . ?
N22 C21 C22 C31 0.3(4) . . . . ?
C31 C22 C23 C24 -0.9(4) . . . . ?
C21 C22 C23 C24 179.7(3) . . . . ?
C22 C23 C24 C25 1.8(5) . . . . ?
C23 C24 C25 C26 -0.6(5) . . . . ?
C23 C24 C25 N200 -179.3(5) . . . . ?
O201 N200 C25 C24 -134.7(7) . . . . ?
O200 N200 C25 C24 42.0(9) . . . . ?
O201 N200 C25 C26 46.4(9) . . . . ?
O200 N200 C25 C26 -136.9(6) . . . . ?
C24 C25 C26 C27 -177.9(3) . . . . ?
N200 C25 C26 C27 1.0(6) . . . . ?
C24 C25 C26 C31 -1.5(4) . . . . ?
N200 C25 C26 C31 177.4(4) . . . . ?
C25 C26 C27 C28 175.8(3) . . . . ?
C31 C26 C27 C28 -0.6(4) . . . . ?
C25 C26 C27 N21 -7.7(5) . . . . ?
C31 C26 C27 N21 175.8(3) . . . . ?
O21 N21 C27 C28 -30.5(5) . . . . ?
O22 N21 C27 C28 146.6(4) . . . . ?
O21 N21 C27 C26 153.0(4) . . . . ?
O22 N21 C27 C26 -30.0(5) . . . . ?
C26 C27 C28 C29 0.2(5) . . . . ?
N21 C27 C28 C29 -176.2(3) . . . . ?
C27 C28 C29 C30 0.7(5) . . . . ?
C28 C29 C30 C31 -1.2(4) . . . . ?
C28 C29 C30 C32 179.8(3) . . . . ?
C29 C30 C31 C22 -178.2(3) . . . . ?
C32 C30 C31 C22 0.8(4) . . . . ?
C29 C30 C31 C26 0.8(4) . . . . ?
C32 C30 C31 C26 179.7(2) . . . . ?
C23 C22 C31 C30 177.8(3) . . . . ?
C21 C22 C31 C30 -2.9(4) . . . . ?
C23 C22 C31 C26 -1.1(4) . . . . ?
C21 C22 C31 C26 178.2(2) . . . . ?
C25 C26 C31 C30 -176.6(3) . . . . ?
C27 C26 C31 C30 0.2(4) . . . . ?
C25 C26 C31 C22 2.3(4) . . . . ?
C27 C26 C31 C22 179.1(3) . . . . ?
C21 N22 C32 O24 174.6(3) . . . . ?
C33 N22 C32 O24 2.8(4) . . . . ?
C21 N22 C32 C30 -6.7(4) . . . . ?
C33 N22 C32 C30 -178.5(2) . . . . ?
C29 C30 C32 O24 1.4(4) . . . . ?
C31 C30 C32 O24 -177.6(3) . . . . ?
C29 C30 C32 N22 -177.2(3) . . . . ?
C31 C30 C32 N22 3.8(4) . . . . ?
C21 N22 C33 C34 -59.8(3) . . . . ?
C32 N22 C33 C34 112.6(3) . . . . ?
C21 N22 C33 C37 121.4(3) . . . . ?
C32 N22 C33 C37 -66.3(3) . . . . ?
C37 C33 C34 C35 -2.5(4) . . . . ?
N22 C33 C34 C35 178.7(2) . . . . ?
C36 N23 C35 C34 0.7(4) . . . . ?
Cu1 N23 C35 C34 -179.7(2) . . . . ?
C33 C34 C35 N23 1.3(4) . . . . ?
C35 N23 C36 C37 -1.7(4) . . . . ?
Cu1 N23 C36 C37 178.7(2) . . . . ?
C34 C33 C37 C36 1.5(4) . . . . ?
N22 C33 C37 C36 -179.6(2) . . . . ?
N23 C36 C37 C33 0.6(4) . . . . ?
O50 Cu1 O40 C40 -3.1(3) . . . . ?
N23 Cu1 O40 C40 85.04(17) . . . . ?
N3 Cu1 O40 C40 -94.46(17) . . . . ?
O51 Cu1 O40 C40 172.21(16) 2_656 . . . ?
Cu1 O40 C40 O41 -1.1(3) . . . . ?
Cu1 O40 C40 C41 177.4(2) . . . . ?
O40 Cu1 O50 C50 -147.3(2) . . . . ?
N23 Cu1 O50 C50 124.5(2) . . . . ?
N3 Cu1 O50 C50 -56.4(2) . . . . ?
O51 Cu1 O50 C50 37.7(2) 2_656 . . . ?
Cu1 O51 C50 O50 -69.4(5) 2_656 . . . ?
Cu1 O51 C50 C51 108.8(4) 2_656 . . . ?
Cu1 O50 C50 O51 -10.7(4) . . . . ?
Cu1 O50 C50 C51 171.01(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 958088'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jak044

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H32 Cl2 Cu N8 O18'
_chemical_formula_weight         1047.18

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.707(3)
_cell_length_b                   8.1250(16)
_cell_length_c                   16.943(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.55(3)
_cell_angle_gamma                90.00
_cell_volume                     2132.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    5733
_cell_measurement_theta_min      2.5065
_cell_measurement_theta_max      31.2818

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1070
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7948
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   Crystalclear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      108(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 Saturn 724'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17603
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3940
_reflns_number_gt                3706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. No disorder, no solvent.
 All non-H ANIS. H calc and ride except OH which was found and fixed.
;

_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)+(0.0819P)²+0.5627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3940
_refine_ls_number_parameters     315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.1296
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.0000 0.01362(16) Uani 1 2 d S . .
O1 O -0.13419(14) -0.4343(2) 0.19169(14) 0.0439(5) Uani 1 1 d . . .
O2 O -0.14510(11) -0.2132(2) 0.25913(10) 0.0312(4) Uani 1 1 d . . .
O3 O 0.23231(10) -0.0848(2) 0.08279(10) 0.0249(4) Uani 1 1 d . . .
O4 O 0.08796(10) 0.3998(2) 0.03811(11) 0.0283(4) Uani 1 1 d . . .
N1 N -0.11410(13) -0.2928(3) 0.20958(12) 0.0247(4) Uani 1 1 d . . .
N2 N 0.16193(11) 0.1611(2) 0.06393(10) 0.0161(4) Uani 1 1 d . . .
N3 N 0.38932(11) 0.3932(2) 0.02057(10) 0.0159(4) Uani 1 1 d . . .
C1 C 0.16725(15) -0.0070(2) 0.08544(14) 0.0166(5) Uani 1 1 d . . .
C2 C 0.09067(13) -0.0788(3) 0.11287(13) 0.0169(5) Uani 1 1 d . . .
C3 C 0.09439(14) -0.2410(3) 0.13670(13) 0.0199(5) Uani 1 1 d . . .
H3 H 0.1443 -0.3051 0.1334 0.024 Uiso 1 1 calc R . .
C4 C 0.02438(15) -0.3108(3) 0.16577(13) 0.0219(5) Uani 1 1 d . . .
H4 H 0.0257 -0.4234 0.1809 0.026 Uiso 1 1 calc R . .
C5 C -0.04600(14) -0.2159(3) 0.17226(13) 0.0195(5) Uani 1 1 d . . .
C6 C -0.05500(14) -0.0493(3) 0.14639(13) 0.0171(4) Uani 1 1 d . . .
C7 C -0.12918(14) 0.0496(3) 0.14691(14) 0.0198(5) Uani 1 1 d . . .
H7 H -0.1767 0.0074 0.1687 0.024 Uiso 1 1 calc R . .
C8 C -0.13264(14) 0.2065(3) 0.11606(14) 0.0227(5) Uani 1 1 d . . .
H8 H -0.1835 0.2703 0.1150 0.027 Uiso 1 1 calc R . .
C9 C -0.06200(14) 0.2737(3) 0.08609(14) 0.0213(5) Uani 1 1 d . . .
H9 H -0.0652 0.3822 0.0649 0.026 Uiso 1 1 calc R . .
C10 C 0.01188(13) 0.1820(3) 0.08754(13) 0.0173(5) Uani 1 1 d . . .
C11 C 0.01631(14) 0.0171(3) 0.11568(13) 0.0156(5) Uani 1 1 d . . .
C12 C 0.08774(14) 0.2586(3) 0.06087(13) 0.0183(5) Uani 1 1 d . . .
C13 C 0.23944(13) 0.2401(3) 0.04827(13) 0.0165(4) Uani 1 1 d . . .
C14 C 0.28156(14) 0.1846(3) -0.01196(13) 0.0183(5) Uani 1 1 d . . .
H14 H 0.2596 0.0941 -0.0446 0.022 Uiso 1 1 calc R . .
C15 C 0.35623(14) 0.2636(3) -0.02366(13) 0.0176(5) Uani 1 1 d . . .
H15 H 0.3856 0.2249 -0.0648 0.021 Uiso 1 1 calc R . .
C16 C 0.34742(14) 0.4460(3) 0.07902(13) 0.0193(5) Uani 1 1 d . . .
H16 H 0.3700 0.5374 0.1107 0.023 Uiso 1 1 calc R . .
C17 C 0.27278(14) 0.3722(3) 0.09460(13) 0.0189(5) Uani 1 1 d . . .
H17 H 0.2448 0.4116 0.1365 0.023 Uiso 1 1 calc R . .
N20 N 0.54790(13) 0.5050(2) 0.11894(12) 0.0177(4) Uani 1 1 d . . .
C20 C 0.58578(16) 0.5154(2) 0.18143(15) 0.0172(5) Uani 1 1 d . . .
C21 C 0.63648(17) 0.5303(3) 0.26133(15) 0.0247(5) Uani 1 1 d . . .
H21A H 0.6587 0.4218 0.2798 0.030 Uiso 1 1 calc R . .
H21B H 0.5999 0.5734 0.2981 0.030 Uiso 1 1 calc R . .
H21C H 0.6849 0.6056 0.2598 0.030 Uiso 1 1 calc R . .
O30 O 0.44421(11) 0.75510(19) 0.00780(9) 0.0243(4) Uani 1 1 d . . .
H30X H 0.4120 0.7773 -0.0344 0.029 Uiso 1 1 d . . .
C30 C 0.43959(15) 0.8654(3) 0.07167(14) 0.0251(5) Uani 1 1 d . . .
H30A H 0.4690 0.8171 0.1219 0.030 Uiso 1 1 calc R . .
H30B H 0.3789 0.8860 0.0756 0.030 Uiso 1 1 calc R . .
H30C H 0.4676 0.9694 0.0618 0.030 Uiso 1 1 calc R . .
Cl1 Cl 0.35780(4) 0.93101(7) -0.20258(3) 0.02049(18) Uani 1 1 d . . .
O11 O 0.35835(15) 1.1052(2) -0.20793(12) 0.0429(5) Uani 1 1 d . . .
O12 O 0.43822(11) 0.8632(2) -0.21446(12) 0.0358(5) Uani 1 1 d . . .
O13 O 0.34018(11) 0.8849(3) -0.12461(10) 0.0349(5) Uani 1 1 d . . .
O14 O 0.28971(11) 0.8665(2) -0.26173(10) 0.0310(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 2.0241(17) 3_665 y
Cu1 N3 2.0241(17) . y
Cu1 N20 2.031(2) 3_665 y
Cu1 N20 2.031(2) . y
Cu1 O30 2.2627(16) . y
Cu1 O30 2.2627(16) 3_665 y
O1 N1 1.217(3) . ?
O2 N1 1.223(3) . ?
O3 C1 1.209(3) . ?
O4 C12 1.211(3) . ?
N1 C5 1.469(3) . ?
N2 C12 1.403(3) . ?
N2 C1 1.412(3) . ?
N2 C13 1.440(3) . ?
N3 C15 1.346(3) . ?
N3 C16 1.347(3) . ?
C1 C2 1.479(3) . ?
C2 C3 1.376(3) . ?
C2 C11 1.411(3) . ?
C3 C4 1.398(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.422(3) . ?
C6 C7 1.417(3) . ?
C6 C11 1.417(3) . ?
C7 C8 1.375(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.405(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.420(3) . ?
C10 C12 1.480(3) . ?
C13 C17 1.380(3) . ?
C13 C14 1.381(3) . ?
C14 C15 1.380(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.381(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N20 C20 1.128(3) . ?
C20 C21 1.457(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O30 C30 1.416(3) . ?
O30 H30X 0.8243 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
Cl1 O11 1.419(2) . ?
Cl1 O12 1.4226(18) . ?
Cl1 O14 1.4378(18) . ?
Cl1 O13 1.4434(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N3 180.0 3_665 . y
N3 Cu1 N20 91.43(8) 3_665 3_665 y
N3 Cu1 N20 88.57(8) . 3_665 y
N3 Cu1 N20 88.57(8) 3_665 . y
N3 Cu1 N20 91.43(8) . . y
N20 Cu1 N20 180.0 3_665 . y
N3 Cu1 O30 88.25(7) 3_665 . y
N3 Cu1 O30 91.75(7) . . y
N20 Cu1 O30 89.59(6) 3_665 . y
N20 Cu1 O30 90.41(6) . . y
N3 Cu1 O30 91.75(7) 3_665 3_665 y
N3 Cu1 O30 88.25(7) . 3_665 y
N20 Cu1 O30 90.41(6) 3_665 3_665 y
N20 Cu1 O30 89.59(6) . 3_665 y
O30 Cu1 O30 180.0 . 3_665 y
O1 N1 O2 123.7(2) . . ?
O1 N1 C5 118.1(2) . . ?
O2 N1 C5 118.1(2) . . ?
C12 N2 C1 124.68(18) . . ?
C12 N2 C13 117.62(17) . . ?
C1 N2 C13 117.61(18) . . ?
C15 N3 C16 117.90(18) . . ?
C15 N3 Cu1 120.18(14) . . ?
C16 N3 Cu1 121.91(15) . . ?
O3 C1 N2 120.7(2) . . ?
O3 C1 C2 122.82(19) . . ?
N2 C1 C2 116.50(19) . . ?
C3 C2 C11 120.9(2) . . ?
C3 C2 C1 118.20(19) . . ?
C11 C2 C1 120.89(19) . . ?
C2 C3 C4 119.6(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.6(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 123.5(2) . . ?
C4 C5 N1 116.8(2) . . ?
C6 C5 N1 119.7(2) . . ?
C7 C6 C11 119.2(2) . . ?
C7 C6 C5 125.3(2) . . ?
C11 C6 C5 115.5(2) . . ?
C8 C7 C6 120.3(2) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.9(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C10 C9 C8 119.8(2) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 120.7(2) . . ?
C9 C10 C12 119.1(2) . . ?
C11 C10 C12 120.17(19) . . ?
C2 C11 C6 120.8(2) . . ?
C2 C11 C10 120.3(2) . . ?
C6 C11 C10 119.0(2) . . ?
O4 C12 N2 120.1(2) . . ?
O4 C12 C10 122.8(2) . . ?
N2 C12 C10 117.18(18) . . ?
C17 C13 C14 119.4(2) . . ?
C17 C13 N2 119.65(19) . . ?
C14 C13 N2 120.93(19) . . ?
C15 C14 C13 118.5(2) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
N3 C15 C14 122.88(19) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N3 C16 C17 122.4(2) . . ?
N3 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C13 C17 C16 118.9(2) . . ?
C13 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C20 N20 Cu1 169.52(19) . . ?
N20 C20 C21 178.6(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C30 O30 Cu1 133.93(14) . . ?
C30 O30 H30X 115.0 . . ?
Cu1 O30 H30X 109.7 . . ?
O30 C30 H30A 109.5 . . ?
O30 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O30 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O11 Cl1 O12 111.25(12) . . ?
O11 Cl1 O14 109.34(11) . . ?
O12 Cl1 O14 109.60(11) . . ?
O11 Cl1 O13 108.75(12) . . ?
O12 Cl1 O13 109.79(11) . . ?
O14 Cl1 O13 108.05(11) . . ?

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
N3 Cu1 N3 C15 141(5) 3_665 . . . ?
N20 Cu1 N3 C15 45.96(17) 3_665 . . . ?
N20 Cu1 N3 C15 -134.04(17) . . . . ?
O30 Cu1 N3 C15 135.50(17) . . . . ?
O30 Cu1 N3 C15 -44.50(17) 3_665 . . . ?
N3 Cu1 N3 C16 -40(5) 3_665 . . . ?
N20 Cu1 N3 C16 -135.30(18) 3_665 . . . ?
N20 Cu1 N3 C16 44.70(18) . . . . ?
O30 Cu1 N3 C16 -45.75(17) . . . . ?
O30 Cu1 N3 C16 134.25(17) 3_665 . . . ?
C12 N2 C1 O3 176.3(2) . . . . ?
C13 N2 C1 O3 -7.3(3) . . . . ?
C12 N2 C1 C2 -5.3(3) . . . . ?
C13 N2 C1 C2 171.17(18) . . . . ?
O3 C1 C2 C3 0.4(3) . . . . ?
N2 C1 C2 C3 -178.0(2) . . . . ?
O3 C1 C2 C11 179.4(2) . . . . ?
N2 C1 C2 C11 1.0(3) . . . . ?
C11 C2 C3 C4 -1.4(3) . . . . ?
C1 C2 C3 C4 177.6(2) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C3 C4 C5 C6 3.9(3) . . . . ?
C3 C4 C5 N1 -174.9(2) . . . . ?
O1 N1 C5 C4 -41.9(3) . . . . ?
O2 N1 C5 C4 135.4(2) . . . . ?
O1 N1 C5 C6 139.2(2) . . . . ?
O2 N1 C5 C6 -43.5(3) . . . . ?
C4 C5 C6 C7 175.4(2) . . . . ?
N1 C5 C6 C7 -5.8(3) . . . . ?
C4 C5 C6 C11 -2.5(3) . . . . ?
N1 C5 C6 C11 176.26(19) . . . . ?
C11 C6 C7 C8 1.7(3) . . . . ?
C5 C6 C7 C8 -176.2(2) . . . . ?
C6 C7 C8 C9 -2.2(3) . . . . ?
C7 C8 C9 C10 -0.1(3) . . . . ?
C8 C9 C10 C11 2.9(3) . . . . ?
C8 C9 C10 C12 -175.9(2) . . . . ?
C3 C2 C11 C6 2.7(3) . . . . ?
C1 C2 C11 C6 -176.3(2) . . . . ?
C3 C2 C11 C10 -177.2(2) . . . . ?
C1 C2 C11 C10 3.8(3) . . . . ?
C7 C6 C11 C2 -178.8(2) . . . . ?
C5 C6 C11 C2 -0.8(3) . . . . ?
C7 C6 C11 C10 1.1(3) . . . . ?
C5 C6 C11 C10 179.12(19) . . . . ?
C9 C10 C11 C2 176.5(2) . . . . ?
C12 C10 C11 C2 -4.7(3) . . . . ?
C9 C10 C11 C6 -3.4(3) . . . . ?
C12 C10 C11 C6 175.4(2) . . . . ?
C1 N2 C12 O4 -176.5(2) . . . . ?
C13 N2 C12 O4 7.0(3) . . . . ?
C1 N2 C12 C10 4.4(3) . . . . ?
C13 N2 C12 C10 -172.02(18) . . . . ?
C9 C10 C12 O4 0.5(3) . . . . ?
C11 C10 C12 O4 -178.3(2) . . . . ?
C9 C10 C12 N2 179.52(19) . . . . ?
C11 C10 C12 N2 0.8(3) . . . . ?
C12 N2 C13 C17 57.6(3) . . . . ?
C1 N2 C13 C17 -119.1(2) . . . . ?
C12 N2 C13 C14 -123.2(2) . . . . ?
C1 N2 C13 C14 60.1(3) . . . . ?
C17 C13 C14 C15 0.1(3) . . . . ?
N2 C13 C14 C15 -179.15(19) . . . . ?
C16 N3 C15 C14 0.5(3) . . . . ?
Cu1 N3 C15 C14 179.31(16) . . . . ?
C13 C14 C15 N3 -0.6(3) . . . . ?
C15 N3 C16 C17 0.0(3) . . . . ?
Cu1 N3 C16 C17 -178.73(16) . . . . ?
C14 C13 C17 C16 0.4(3) . . . . ?
N2 C13 C17 C16 179.67(19) . . . . ?
N3 C16 C17 C13 -0.5(3) . . . . ?
N3 Cu1 N20 C20 -7.5(9) 3_665 . . . ?
N3 Cu1 N20 C20 172.5(9) . . . . ?
N20 Cu1 N20 C20 76(39) 3_665 . . . ?
O30 Cu1 N20 C20 -95.8(9) . . . . ?
O30 Cu1 N20 C20 84.2(9) 3_665 . . . ?
Cu1 N20 C20 C21 2(11) . . . . ?
N3 Cu1 O30 C30 -92.9(2) 3_665 . . . ?
N3 Cu1 O30 C30 87.1(2) . . . . ?
N20 Cu1 O30 C30 175.7(2) 3_665 . . . ?
N20 Cu1 O30 C30 -4.3(2) . . . . ?
O30 Cu1 O30 C30 -130(12) 3_665 . . . ?

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
O30 H30X O13 0.82 1.95 2.756(2) 165.9 .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.114
_database_code_depnum_ccdc_archive 'CCDC 958089'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jak048_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H16 Br N3 O4'
_chemical_formula_weight         490.31

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'
Br Br -0.2901 2.4595 '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                   29.276(6)
_cell_length_b                   9.6019(19)
_cell_length_c                   15.263(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.34(3)
_cell_angle_gamma                90.00
_cell_volume                     4174.8(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    6045
_cell_measurement_theta_min      1.4491
_cell_measurement_theta_max      31.3101

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_absorpt_coefficient_mu    2.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_T_max  0.6444
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      108(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 Saturn 724'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16553
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3649
_reflns_number_gt                2760
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0833P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3649
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.1943
_refine_ls_wR_factor_gt          0.1729
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5292(3) 1.7239(7) 0.6612(5) 0.0553(17) Uani 1 1 d . . .
N2 N 0.38672(17) 1.2350(5) 0.4719(3) 0.0283(11) Uani 1 1 d . . .
N3 N 0.28358(18) 0.9848(5) 0.3156(3) 0.0328(12) Uani 1 1 d . . .
O1 O 0.5296(3) 1.8438(7) 0.6212(5) 0.0464(18) Uani 0.65 1 d P A 1
O2 O 0.5544(4) 1.6913(9) 0.7291(5) 0.065(3) Uani 0.65 1 d P A 1
O10 O 0.5173(7) 1.8296(19) 0.6993(15) 0.095(7) Uani 0.35 1 d P A 2
O20 O 0.5724(5) 1.6756(15) 0.6768(11) 0.049(4) Uani 0.35 1 d P A 2
O3 O 0.34565(16) 1.4295(4) 0.4168(3) 0.0417(11) Uani 1 1 d . . .
O4 O 0.42362(16) 1.0401(4) 0.5377(3) 0.0420(11) Uani 1 1 d . . .
C1 C 0.3800(2) 1.3800(6) 0.4664(4) 0.0299(13) Uani 1 1 d . . .
C2 C 0.4193(2) 1.4651(6) 0.5210(4) 0.0332(15) Uani 1 1 d . . .
C3 C 0.4150(2) 1.6068(7) 0.5133(4) 0.0401(16) Uani 1 1 d . A .
H3 H 0.3877 1.6478 0.4766 0.048 Uiso 1 1 calc R . .
C4 C 0.4523(3) 1.6909(7) 0.5614(4) 0.0423(17) Uani 1 1 d . . .
H4 H 0.4502 1.7895 0.5579 0.051 Uiso 1 1 calc R A .
C5 C 0.4915(3) 1.6284(8) 0.6129(4) 0.0427(17) Uani 1 1 d . A .
C6 C 0.4982(2) 1.4829(7) 0.6239(4) 0.0380(16) Uani 1 1 d . . .
C7 C 0.5377(2) 1.4126(8) 0.6747(4) 0.0447(18) Uani 1 1 d . A .
H7 H 0.5637 1.4655 0.7066 0.054 Uiso 1 1 calc R . .
C8 C 0.5398(2) 1.2700(8) 0.6794(4) 0.0472(18) Uani 1 1 d . . .
H8 H 0.5670 1.2253 0.7141 0.057 Uiso 1 1 calc R A .
C9 C 0.5018(2) 1.1907(7) 0.6331(4) 0.0434(17) Uani 1 1 d . A .
H9 H 0.5032 1.0920 0.6371 0.052 Uiso 1 1 calc R . .
C10 C 0.4625(2) 1.2538(7) 0.5818(4) 0.0340(15) Uani 1 1 d . . .
C11 C 0.4598(2) 1.4004(7) 0.5744(3) 0.0320(14) Uani 1 1 d . A .
C12 C 0.4239(2) 1.1642(7) 0.5318(4) 0.0318(14) Uani 1 1 d . A .
C13 C 0.3510(2) 1.1495(6) 0.4174(3) 0.0267(13) Uani 1 1 d . . .
C14 C 0.3630(2) 1.0528(6) 0.3604(4) 0.0346(15) Uani 1 1 d . . .
H14 H 0.3947 1.0424 0.3562 0.041 Uiso 1 1 calc R . .
C15 C 0.3281(2) 0.9713(6) 0.3093(4) 0.0374(15) Uani 1 1 d . . .
H15 H 0.3358 0.9045 0.2691 0.045 Uiso 1 1 calc R . .
C16 C 0.2713(2) 1.0776(6) 0.3712(4) 0.0341(14) Uani 1 1 d . . .
H16 H 0.2394 1.0853 0.3743 0.041 Uiso 1 1 calc R . .
C17 C 0.3046(2) 1.1621(6) 0.4238(4) 0.0319(14) Uani 1 1 d . . .
H17 H 0.2960 1.2277 0.4638 0.038 Uiso 1 1 calc R . .
C18 C 0.2463(2) 0.8950(7) 0.2593(4) 0.0428(17) Uani 1 1 d . . .
H18A H 0.2598 0.8422 0.2156 0.051 Uiso 1 1 calc R . .
H18B H 0.2208 0.9547 0.2249 0.051 Uiso 1 1 calc R . .
C19 C 0.2263(2) 0.7945(6) 0.3165(4) 0.0313(14) Uani 1 1 d . . .
C20 C 0.2547(2) 0.6930(6) 0.3687(4) 0.0357(15) Uani 1 1 d . . .
H20 H 0.2873 0.6899 0.3702 0.043 Uiso 1 1 calc R . .
C21 C 0.2358(2) 0.5982(7) 0.4175(4) 0.0389(16) Uani 1 1 d . . .
H21 H 0.2553 0.5310 0.4536 0.047 Uiso 1 1 calc R . .
C22 C 0.1882(2) 0.6005(7) 0.4142(4) 0.0424(16) Uani 1 1 d . . .
H22 H 0.1749 0.5331 0.4465 0.051 Uiso 1 1 calc R . .
C23 C 0.1599(2) 0.7011(7) 0.3637(4) 0.0431(17) Uani 1 1 d . . .
H23 H 0.1274 0.7043 0.3629 0.052 Uiso 1 1 calc R . .
C24 C 0.1788(2) 0.7970(6) 0.3146(4) 0.0350(15) Uani 1 1 d . . .
H24 H 0.1592 0.8648 0.2793 0.042 Uiso 1 1 calc R . .
Br1 Br 0.15530(2) 0.19511(7) 0.33914(4) 0.0391(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 O2 1.168(10) . ?
N1 O10 1.258(18) . ?
N1 O1 1.304(9) . ?
N1 O20 1.316(15) . ?
N1 C5 1.492(9) . ?
N2 C1 1.406(7) . ?
N2 C12 1.421(7) . ?
N2 C13 1.434(7) . ?
N3 C15 1.336(8) . ?
N3 C16 1.336(8) . ?
N3 C18 1.496(7) . ?
O3 C1 1.208(7) . ?
O4 C12 1.195(7) . ?
C1 C2 1.499(8) . ?
C2 C3 1.369(9) . ?
C2 C11 1.416(8) . ?
C3 C4 1.419(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.416(10) . ?
C6 C7 1.408(9) . ?
C6 C11 1.439(8) . ?
C7 C8 1.372(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.413(9) . ?
C10 C12 1.485(8) . ?
C13 C14 1.373(8) . ?
C13 C17 1.391(8) . ?
C14 C15 1.377(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.375(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.509(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C24 1.382(9) . ?
C19 C20 1.404(8) . ?
C20 C21 1.373(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?

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 N1 O10 89.5(12) . . ?
O2 N1 O1 125.4(8) . . ?
O10 N1 O1 62.4(11) . . ?
O2 N1 O20 50.2(8) . . ?
O10 N1 O20 123.9(12) . . ?
O1 N1 O20 106.5(10) . . ?
O2 N1 C5 121.2(7) . . ?
O10 N1 C5 118.2(11) . . ?
O1 N1 C5 113.4(7) . . ?
O20 N1 C5 116.3(8) . . ?
C1 N2 C12 126.0(5) . . ?
C1 N2 C13 117.3(5) . . ?
C12 N2 C13 116.6(5) . . ?
C15 N3 C16 121.4(5) . . ?
C15 N3 C18 119.8(5) . . ?
C16 N3 C18 118.8(6) . . ?
O3 C1 N2 120.8(5) . . ?
O3 C1 C2 123.8(5) . . ?
N2 C1 C2 115.3(5) . . ?
C3 C2 C11 122.2(6) . . ?
C3 C2 C1 116.8(6) . . ?
C11 C2 C1 120.9(5) . . ?
C2 C3 C4 118.5(7) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 119.3(6) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 125.1(6) . . ?
C4 C5 N1 116.1(6) . . ?
C6 C5 N1 118.8(7) . . ?
C7 C6 C5 127.7(6) . . ?
C7 C6 C11 118.0(6) . . ?
C5 C6 C11 114.3(6) . . ?
C8 C7 C6 121.9(6) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 119.7(6) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.8(6) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.6(6) . . ?
C9 C10 C12 118.5(6) . . ?
C11 C10 C12 120.9(6) . . ?
C10 C11 C2 120.5(5) . . ?
C10 C11 C6 118.9(6) . . ?
C2 C11 C6 120.6(6) . . ?
O4 C12 N2 120.5(5) . . ?
O4 C12 C10 123.7(6) . . ?
N2 C12 C10 115.7(5) . . ?
C14 C13 C17 120.1(5) . . ?
C14 C13 N2 119.7(5) . . ?
C17 C13 N2 120.2(5) . . ?
C13 C14 C15 118.6(6) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N3 C15 C14 120.9(6) . . ?
N3 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
N3 C16 C17 120.4(6) . . ?
N3 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C13 118.6(6) . . ?
C16 C17 H17 120.7 . . ?
C13 C17 H17 120.7 . . ?
N3 C18 C19 111.4(5) . . ?
N3 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
N3 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C24 C19 C20 119.1(6) . . ?
C24 C19 C18 120.0(5) . . ?
C20 C19 C18 120.9(6) . . ?
C21 C20 C19 120.5(6) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 120.0(6) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C23 120.0(6) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.2(7) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C19 120.3(6) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?

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
C12 N2 C1 O3 -175.5(6) . . . . ?
C13 N2 C1 O3 -0.9(8) . . . . ?
C12 N2 C1 C2 8.3(8) . . . . ?
C13 N2 C1 C2 -177.1(5) . . . . ?
O3 C1 C2 C3 0.4(9) . . . . ?
N2 C1 C2 C3 176.5(5) . . . . ?
O3 C1 C2 C11 -176.7(6) . . . . ?
N2 C1 C2 C11 -0.6(8) . . . . ?
C11 C2 C3 C4 -0.7(9) . . . . ?
C1 C2 C3 C4 -177.7(5) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C3 C4 C5 C6 -0.9(10) . . . . ?
C3 C4 C5 N1 179.8(6) . . . . ?
O2 N1 C5 C4 151.2(9) . . . . ?
O10 N1 C5 C4 42.8(16) . . . . ?
O1 N1 C5 C4 -27.2(9) . . . . ?
O20 N1 C5 C4 -151.2(10) . . . . ?
O2 N1 C5 C6 -28.1(12) . . . . ?
O10 N1 C5 C6 -136.5(14) . . . . ?
O1 N1 C5 C6 153.5(7) . . . . ?
O20 N1 C5 C6 29.5(12) . . . . ?
C4 C5 C6 C7 179.1(6) . . . . ?
N1 C5 C6 C7 -1.7(10) . . . . ?
C4 C5 C6 C11 0.8(9) . . . . ?
N1 C5 C6 C11 -180.0(5) . . . . ?
C5 C6 C7 C8 -179.7(7) . . . . ?
C11 C6 C7 C8 -1.4(10) . . . . ?
C6 C7 C8 C9 -0.2(11) . . . . ?
C7 C8 C9 C10 0.8(11) . . . . ?
C8 C9 C10 C11 0.4(10) . . . . ?
C8 C9 C10 C12 178.1(6) . . . . ?
C9 C10 C11 C2 179.5(6) . . . . ?
C12 C10 C11 C2 1.9(8) . . . . ?
C9 C10 C11 C6 -2.1(9) . . . . ?
C12 C10 C11 C6 -179.7(5) . . . . ?
C3 C2 C11 C10 178.9(6) . . . . ?
C1 C2 C11 C10 -4.1(8) . . . . ?
C3 C2 C11 C6 0.6(9) . . . . ?
C1 C2 C11 C6 177.5(5) . . . . ?
C7 C6 C11 C10 2.6(8) . . . . ?
C5 C6 C11 C10 -179.0(5) . . . . ?
C7 C6 C11 C2 -179.1(6) . . . . ?
C5 C6 C11 C2 -0.6(8) . . . . ?
C1 N2 C12 O4 171.9(6) . . . . ?
C13 N2 C12 O4 -2.7(9) . . . . ?
C1 N2 C12 C10 -10.3(8) . . . . ?
C13 N2 C12 C10 175.0(5) . . . . ?
C9 C10 C12 O4 4.8(10) . . . . ?
C11 C10 C12 O4 -177.5(6) . . . . ?
C9 C10 C12 N2 -172.9(6) . . . . ?
C11 C10 C12 N2 4.8(8) . . . . ?
C1 N2 C13 C14 126.4(6) . . . . ?
C12 N2 C13 C14 -58.5(7) . . . . ?
C1 N2 C13 C17 -55.2(7) . . . . ?
C12 N2 C13 C17 119.9(6) . . . . ?
C17 C13 C14 C15 1.1(9) . . . . ?
N2 C13 C14 C15 179.5(5) . . . . ?
C16 N3 C15 C14 0.1(9) . . . . ?
C18 N3 C15 C14 179.9(5) . . . . ?
C13 C14 C15 N3 -0.6(9) . . . . ?
C15 N3 C16 C17 -0.1(8) . . . . ?
C18 N3 C16 C17 -179.9(5) . . . . ?
N3 C16 C17 C13 0.5(8) . . . . ?
C14 C13 C17 C16 -1.0(8) . . . . ?
N2 C13 C17 C16 -179.4(5) . . . . ?
C15 N3 C18 C19 112.9(6) . . . . ?
C16 N3 C18 C19 -67.3(7) . . . . ?
N3 C18 C19 C24 121.0(6) . . . . ?
N3 C18 C19 C20 -62.3(8) . . . . ?
C24 C19 C20 C21 -0.5(8) . . . . ?
C18 C19 C20 C21 -177.2(6) . . . . ?
C19 C20 C21 C22 1.3(9) . . . . ?
C20 C21 C22 C23 -2.0(9) . . . . ?
C21 C22 C23 C24 1.9(10) . . . . ?
C22 C23 C24 C19 -1.0(9) . . . . ?
C20 C19 C24 C23 0.3(9) . . . . ?
C18 C19 C24 C23 177.1(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 958090'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jak160br

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H19 Br N4 O4'
_chemical_formula_weight         531.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   7.2517(15)
_cell_length_b                   25.162(5)
_cell_length_c                   12.801(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.23(3)
_cell_angle_gamma                90.00
_cell_volume                     2282.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4316
_cell_measurement_theta_min      1.6186
_cell_measurement_theta_max      31.4792

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(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 Saturn 724'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8104
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3866
_reflns_number_gt                3359
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.1016P)²+9.5812P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3866
_refine_ls_number_parameters     319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0885
_refine_ls_wR_factor_ref         0.2315
_refine_ls_wR_factor_gt          0.2217
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_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
Br1 Br 0.97525(10) 0.18830(3) 0.52530(5) 0.0396(3) Uani 1 1 d . . .
C4 C 0.4743(15) 0.0628(5) 0.8124(7) 0.071(3) Uani 1 1 d . . .
H4 H 0.5217 0.0678 0.8868 0.085 Uiso 1 1 calc R . .
C5 C 0.3936(16) 0.0158(5) 0.7755(9) 0.075(3) Uani 1 1 d . . .
N1 N 0.343(3) -0.0265(6) 0.8495(9) 0.130(6) Uani 1 1 d . . .
O1 O 0.484(2) -0.0381(6) 0.9195(9) 0.164(5) Uani 1 1 d . . .
O2 O 0.1842(17) -0.0505(5) 0.8323(11) 0.144(6) Uani 1 1 d . . .
C6 C 0.3275(13) 0.0039(4) 0.6659(7) 0.056(2) Uani 1 1 d . . .
C7 C 0.2563(13) -0.0456(4) 0.6246(11) 0.071(3) Uani 1 1 d . . .
H7 H 0.2466 -0.0740 0.6720 0.086 Uiso 1 1 calc R . .
N2 N 0.3618(8) 0.1284(2) 0.4484(4) 0.0309(13) Uani 1 1 d . . .
N3 N 0.4838(8) 0.2461(2) 0.3084(4) 0.0305(13) Uani 1 1 d . . .
O3 O 0.4860(7) 0.1842(2) 0.5870(4) 0.0389(12) Uani 1 1 d . . .
O4 O 0.2555(9) 0.0727(2) 0.3103(4) 0.0561(16) Uani 1 1 d . . .
C1 C 0.4267(10) 0.1403(3) 0.5584(5) 0.0331(15) Uani 1 1 d . . .
C2 C 0.4187(10) 0.0958(3) 0.6324(6) 0.0392(17) Uani 1 1 d . . .
C3 C 0.4874(12) 0.1044(4) 0.7389(6) 0.053(2) Uani 1 1 d . . .
H3A H 0.5428 0.1375 0.7635 0.064 Uiso 1 1 calc R . .
C8 C 0.2008(13) -0.0531(4) 0.5162(10) 0.066(3) Uani 1 1 d . . .
H8A H 0.1511 -0.0866 0.4894 0.079 Uiso 1 1 calc R . .
C9 C 0.2164(12) -0.0129(3) 0.4457(8) 0.053(2) Uani 1 1 d . . .
H9A H 0.1797 -0.0190 0.3710 0.063 Uiso 1 1 calc R . .
C10 C 0.2853(10) 0.0366(3) 0.4830(7) 0.0419(18) Uani 1 1 d . . .
C11 C 0.3437(11) 0.0457(3) 0.5933(7) 0.0453(19) Uani 1 1 d . . .
C12 C 0.2981(11) 0.0787(3) 0.4066(6) 0.0398(17) Uani 1 1 d . . .
C13 C 0.3448(10) 0.1721(3) 0.3747(5) 0.0327(16) Uani 1 1 d . . .
C14 C 0.1721(10) 0.1837(3) 0.3094(5) 0.0352(16) Uani 1 1 d . . .
H14A H 0.0642 0.1625 0.3111 0.042 Uiso 1 1 calc R . .
C15 C 0.1604(11) 0.2271(3) 0.2412(5) 0.0364(16) Uani 1 1 d . . .
H15A H 0.0442 0.2355 0.1941 0.044 Uiso 1 1 calc R . .
C16 C 0.3176(10) 0.2582(3) 0.2419(5) 0.0356(16) Uani 1 1 d . . .
H16A H 0.3093 0.2881 0.1958 0.043 Uiso 1 1 calc R . .
C17 C 0.5022(10) 0.2035(3) 0.3743(5) 0.0310(15) Uani 1 1 d . . .
H17A H 0.6204 0.1952 0.4195 0.037 Uiso 1 1 calc R . .
C18 C 0.6508(10) 0.2815(3) 0.3108(6) 0.0355(16) Uani 1 1 d . . .
H18A H 0.7677 0.2625 0.3452 0.043 Uiso 1 1 calc R . .
H18B H 0.6600 0.2906 0.2369 0.043 Uiso 1 1 calc R . .
C19 C 0.6321(10) 0.3308(3) 0.3712(5) 0.0343(16) Uani 1 1 d . . .
C20 C 0.5423(12) 0.3756(3) 0.3213(6) 0.048(2) Uani 1 1 d . . .
H20A H 0.4951 0.3754 0.2462 0.057 Uiso 1 1 calc R . .
C21 C 0.5206(13) 0.4211(3) 0.3801(7) 0.053(2) Uani 1 1 d . . .
H21A H 0.4570 0.4513 0.3452 0.064 Uiso 1 1 calc R . .
C22 C 0.5914(14) 0.4221(3) 0.4884(7) 0.056(2) Uani 1 1 d . . .
H22A H 0.5758 0.4529 0.5285 0.067 Uiso 1 1 calc R . .
C23 C 0.6845(15) 0.3788(4) 0.5388(7) 0.062(2) Uani 1 1 d . . .
H23A H 0.7351 0.3798 0.6136 0.074 Uiso 1 1 calc R . .
C24 C 0.7050(13) 0.3329(3) 0.4802(6) 0.049(2) Uani 1 1 d . . .
H24A H 0.7697 0.3030 0.5156 0.059 Uiso 1 1 calc R . .
N100 N 0.2967(15) -0.1643(4) 0.8003(8) 0.082(3) Uani 1 1 d . A 1
C100 C 0.2956(14) -0.1725(4) 0.8887(8) 0.062(2) Uani 1 1 d . A 1
C101 C 0.2904(19) -0.1832(5) 1.0011(9) 0.080(3) Uani 1 1 d . A 1
H10A H 0.2041 -0.1582 1.0247 0.096 Uiso 1 1 calc R A 1
H10B H 0.4173 -0.1790 1.0456 0.096 Uiso 1 1 calc R A 1
H10C H 0.2463 -0.2196 1.0079 0.096 Uiso 1 1 calc R A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C4 C5 1.358(16) . ?
C4 C3 1.425(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.414(16) . ?
C5 N1 1.521(16) . ?
N1 O1 1.245(18) . ?
N1 O2 1.28(2) . ?
C6 C7 1.409(15) . ?
C6 C11 1.424(11) . ?
C7 C8 1.374(16) . ?
C7 H7 0.9500 . ?
N2 C12 1.401(9) . ?
N2 C1 1.419(8) . ?
N2 C13 1.436(8) . ?
N3 C17 1.354(8) . ?
N3 C16 1.355(9) . ?
N3 C18 1.499(9) . ?
O3 C1 1.214(9) . ?
O4 C12 1.215(9) . ?
C1 C2 1.475(10) . ?
C2 C3 1.366(11) . ?
C2 C11 1.420(11) . ?
C3 H3A 0.9500 . ?
C8 C9 1.377(13) . ?
C8 H8A 0.9500 . ?
C9 C10 1.387(12) . ?
C9 H9A 0.9500 . ?
C10 C11 1.405(12) . ?
C10 C12 1.458(11) . ?
C13 C14 1.382(10) . ?
C13 C17 1.388(10) . ?
C14 C15 1.391(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.381(10) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
C18 C19 1.484(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C24 1.384(10) . ?
C19 C20 1.388(11) . ?
C20 C21 1.397(12) . ?
C20 H20A 0.9500 . ?
C21 C22 1.373(13) . ?
C21 H21A 0.9500 . ?
C22 C23 1.369(13) . ?
C22 H22A 0.9500 . ?
C23 C24 1.401(12) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
N100 C100 1.152(13) . ?
C100 C101 1.473(15) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C4 C3 119.6(9) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 124.0(8) . . ?
C4 C5 N1 122.4(11) . . ?
C6 C5 N1 113.2(12) . . ?
O1 N1 O2 126.0(15) . . ?
O1 N1 C5 109.9(17) . . ?
O2 N1 C5 123.5(12) . . ?
C7 C6 C5 125.4(9) . . ?
C7 C6 C11 118.8(9) . . ?
C5 C6 C11 115.7(9) . . ?
C8 C7 C6 120.5(9) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C12 N2 C1 125.5(6) . . ?
C12 N2 C13 117.3(6) . . ?
C1 N2 C13 117.1(6) . . ?
C17 N3 C16 121.9(6) . . ?
C17 N3 C18 119.0(6) . . ?
C16 N3 C18 119.1(6) . . ?
O3 C1 N2 120.8(6) . . ?
O3 C1 C2 123.9(6) . . ?
N2 C1 C2 115.3(6) . . ?
C3 C2 C11 121.5(8) . . ?
C3 C2 C1 117.7(8) . . ?
C11 C2 C1 120.8(7) . . ?
C2 C3 C4 118.8(10) . . ?
C2 C3 H3A 120.6 . . ?
C4 C3 H3A 120.6 . . ?
C7 C8 C9 120.8(9) . . ?
C7 C8 H8A 119.6 . . ?
C9 C8 H8A 119.6 . . ?
C8 C9 C10 120.6(10) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C9 C10 C11 120.2(8) . . ?
C9 C10 C12 119.3(8) . . ?
C11 C10 C12 120.5(7) . . ?
C10 C11 C2 120.7(7) . . ?
C10 C11 C6 119.1(8) . . ?
C2 C11 C6 120.2(8) . . ?
O4 C12 N2 119.3(7) . . ?
O4 C12 C10 123.6(7) . . ?
N2 C12 C10 117.1(7) . . ?
C14 C13 C17 121.2(6) . . ?
C14 C13 N2 119.9(6) . . ?
C17 C13 N2 118.8(6) . . ?
C13 C14 C15 118.2(7) . . ?
C13 C14 H14A 120.9 . . ?
C15 C14 H14A 120.9 . . ?
C16 C15 C14 120.1(7) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
N3 C16 C15 119.9(6) . . ?
N3 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
N3 C17 C13 118.7(6) . . ?
N3 C17 H17A 120.7 . . ?
C13 C17 H17A 120.7 . . ?
C19 C18 N3 110.2(5) . . ?
C19 C18 H18A 109.6 . . ?
N3 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
N3 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C24 C19 C20 118.3(7) . . ?
C24 C19 C18 120.0(7) . . ?
C20 C19 C18 121.7(6) . . ?
C19 C20 C21 120.9(7) . . ?
C19 C20 H20A 119.6 . . ?
C21 C20 H20A 119.6 . . ?
C22 C21 C20 119.8(8) . . ?
C22 C21 H21A 120.1 . . ?
C20 C21 H21A 120.1 . . ?
C23 C22 C21 120.2(8) . . ?
C23 C22 H22A 119.9 . . ?
C21 C22 H22A 119.9 . . ?
C22 C23 C24 120.0(8) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C19 C24 C23 120.7(8) . . ?
C19 C24 H24A 119.7 . . ?
C23 C24 H24A 119.7 . . ?
N100 C100 C101 179.0(13) . . ?

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
C3 C4 C5 C6 3.1(15) . . . . ?
C3 C4 C5 N1 -168.7(10) . . . . ?
C4 C5 N1 O1 -54.8(15) . . . . ?
C6 C5 N1 O1 132.6(11) . . . . ?
C4 C5 N1 O2 133.2(14) . . . . ?
C6 C5 N1 O2 -39.4(16) . . . . ?
C4 C5 C6 C7 175.0(9) . . . . ?
N1 C5 C6 C7 -12.5(13) . . . . ?
C4 C5 C6 C11 -2.3(13) . . . . ?
N1 C5 C6 C11 170.2(9) . . . . ?
C5 C6 C7 C8 -178.1(9) . . . . ?
C11 C6 C7 C8 -1.0(12) . . . . ?
C12 N2 C1 O3 177.3(7) . . . . ?
C13 N2 C1 O3 -8.4(10) . . . . ?
C12 N2 C1 C2 -1.9(10) . . . . ?
C13 N2 C1 C2 172.4(6) . . . . ?
O3 C1 C2 C3 -2.0(11) . . . . ?
N2 C1 C2 C3 177.1(6) . . . . ?
O3 C1 C2 C11 178.6(7) . . . . ?
N2 C1 C2 C11 -2.3(10) . . . . ?
C11 C2 C3 C4 -3.1(12) . . . . ?
C1 C2 C3 C4 177.5(7) . . . . ?
C5 C4 C3 C2 -0.3(13) . . . . ?
C6 C7 C8 C9 1.1(14) . . . . ?
C7 C8 C9 C10 -1.2(13) . . . . ?
C8 C9 C10 C11 1.3(12) . . . . ?
C8 C9 C10 C12 -179.3(7) . . . . ?
C9 C10 C11 C2 178.5(7) . . . . ?
C12 C10 C11 C2 -1.0(11) . . . . ?
C9 C10 C11 C6 -1.2(11) . . . . ?
C12 C10 C11 C6 179.4(7) . . . . ?
C3 C2 C11 C10 -175.7(7) . . . . ?
C1 C2 C11 C10 3.6(11) . . . . ?
C3 C2 C11 C6 4.0(11) . . . . ?
C1 C2 C11 C6 -176.7(7) . . . . ?
C7 C6 C11 C10 1.0(11) . . . . ?
C5 C6 C11 C10 178.5(7) . . . . ?
C7 C6 C11 C2 -178.6(7) . . . . ?
C5 C6 C11 C2 -1.2(11) . . . . ?
C1 N2 C12 O4 -176.1(7) . . . . ?
C13 N2 C12 O4 9.6(10) . . . . ?
C1 N2 C12 C10 4.5(10) . . . . ?
C13 N2 C12 C10 -169.8(6) . . . . ?
C9 C10 C12 O4 -1.8(12) . . . . ?
C11 C10 C12 O4 177.6(7) . . . . ?
C9 C10 C12 N2 177.6(7) . . . . ?
C11 C10 C12 N2 -2.9(10) . . . . ?
C12 N2 C13 C14 53.8(9) . . . . ?
C1 N2 C13 C14 -120.9(7) . . . . ?
C12 N2 C13 C17 -129.1(7) . . . . ?
C1 N2 C13 C17 56.1(8) . . . . ?
C17 C13 C14 C15 1.3(10) . . . . ?
N2 C13 C14 C15 178.3(6) . . . . ?
C13 C14 C15 C16 -1.7(10) . . . . ?
C17 N3 C16 C15 0.8(10) . . . . ?
C18 N3 C16 C15 -177.7(6) . . . . ?
C14 C15 C16 N3 0.6(10) . . . . ?
C16 N3 C17 C13 -1.2(9) . . . . ?
C18 N3 C17 C13 177.4(6) . . . . ?
C14 C13 C17 N3 0.1(9) . . . . ?
N2 C13 C17 N3 -177.0(5) . . . . ?
C17 N3 C18 C19 -102.5(7) . . . . ?
C16 N3 C18 C19 76.1(7) . . . . ?
N3 C18 C19 C24 90.4(8) . . . . ?
N3 C18 C19 C20 -89.5(8) . . . . ?
C24 C19 C20 C21 -2.1(12) . . . . ?
C18 C19 C20 C21 177.9(7) . . . . ?
C19 C20 C21 C22 1.1(13) . . . . ?
C20 C21 C22 C23 0.5(14) . . . . ?
C21 C22 C23 C24 -1.1(15) . . . . ?
C20 C19 C24 C23 1.5(12) . . . . ?
C18 C19 C24 C23 -178.4(8) . . . . ?
C22 C23 C24 C19 0.0(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.482
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 958091'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jakoac

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H36 Cu2 N8 O16'
_chemical_formula_weight         1083.91

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                   8.7390(17)
_cell_length_b                   9.0880(18)
_cell_length_c                   17.536(4)
_cell_angle_alpha                99.75(3)
_cell_angle_beta                 94.30(3)
_cell_angle_gamma                118.30(3)
_cell_volume                     1189.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    3098
_cell_measurement_theta_min      2.6120
_cell_measurement_theta_max      30.5940

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             554
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7275
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_process_details   CrystalClear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      108(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 Saturn 724'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7727
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         24.49
_reflns_number_total             3766
_reflns_number_gt                3259
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1806P)²+2.2193P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3766
_refine_ls_number_parameters     356
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.1200
_refine_ls_wR_factor_ref         0.3505
_refine_ls_wR_factor_gt          0.3304
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.209
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.94926(15) 1.02789(15) 0.06723(6) 0.0540(6) Uani 1 1 d . . .
O3 O 0.4345(10) 0.6171(10) 0.2286(4) 0.075(2) Uani 1 1 d . . .
O4 O 0.9562(9) 0.9263(8) 0.4070(4) 0.0563(16) Uani 1 1 d . C .
N2 N 0.6895(10) 0.7805(9) 0.3235(4) 0.0472(17) Uani 1 1 d . C .
N3 N 0.8547(11) 1.0505(10) 0.1816(4) 0.0546(19) Uani 1 1 d . . .
C1 C 0.5287(14) 0.6240(13) 0.2876(5) 0.058(2) Uani 1 1 d . . .
C2 C 0.4840(13) 0.4760(13) 0.3246(5) 0.055(2) Uani 1 1 d . C .
C3 C 0.3317(13) 0.3190(13) 0.2889(6) 0.060(2) Uani 1 1 d . . .
H3 H 0.2612 0.3086 0.2421 0.072 Uiso 1 1 calc R . .
C4 C 0.2840(14) 0.1768(12) 0.3230(5) 0.059(2) Uani 1 1 d . C .
H4 H 0.1807 0.0708 0.2988 0.071 Uiso 1 1 calc R . .
C5 C 0.3841(12) 0.1882(12) 0.3907(5) 0.055(2) Uani 1 1 d . . .
H5 H 0.3477 0.0902 0.4124 0.065 Uiso 0.50 1 calc PR A 2
C6 C 0.5421(12) 0.3451(11) 0.4292(5) 0.049(2) Uani 1 1 d . C .
C7 C 0.6595(13) 0.3687(13) 0.4970(5) 0.055(2) Uani 1 1 d . . .
H7 H 0.6291 0.2767 0.5224 0.065 Uiso 0.50 1 calc PR B 1
C8 C 0.8174(13) 0.5223(13) 0.5272(6) 0.059(2) Uani 1 1 d . C .
H8 H 0.8935 0.5324 0.5719 0.070 Uiso 1 1 calc R . .
C9 C 0.8649(15) 0.6637(13) 0.4915(5) 0.059(2) Uani 1 1 d . . .
H9 H 0.9714 0.7691 0.5124 0.071 Uiso 1 1 calc R C .
C10 C 0.7531(13) 0.6451(12) 0.4256(5) 0.051(2) Uani 1 1 d . C .
C11 C 0.5930(12) 0.4878(11) 0.3928(4) 0.046(2) Uani 1 1 d . . .
C12 C 0.8119(13) 0.7947(13) 0.3866(5) 0.052(2) Uani 1 1 d . . .
C13 C 0.7394(11) 0.9237(11) 0.2877(5) 0.0443(19) Uani 1 1 d . . .
C14 C 0.7456(13) 1.0768(13) 0.3254(5) 0.056(2) Uani 1 1 d . C .
H14 H 0.7064 1.0852 0.3743 0.067 Uiso 1 1 calc R . .
C15 C 0.8098(13) 1.2150(12) 0.2901(5) 0.055(2) Uani 1 1 d . . .
H15 H 0.8169 1.3204 0.3143 0.066 Uiso 1 1 calc R C .
C16 C 0.8624(12) 1.1950(11) 0.2194(5) 0.049(2) Uani 1 1 d . C .
H16 H 0.9076 1.2903 0.1956 0.059 Uiso 1 1 calc R . .
C17 C 0.7948(12) 0.9140(11) 0.2151(5) 0.048(2) Uani 1 1 d . C .
H17 H 0.7904 0.8110 0.1891 0.058 Uiso 1 1 calc R . .
N1 N 0.340(2) 0.032(2) 0.4236(9) 0.057(4) Uani 0.50 1 d P C 1
O2 O 0.3408(17) 0.0463(18) 0.4963(8) 0.054(3) Uani 0.50 1 d P C 1
O1 O 0.2900(19) -0.1127(18) 0.3761(8) 0.064(3) Uani 0.50 1 d P C 1
N10 N 0.622(3) 0.241(2) 0.5393(10) 0.063(4) Uani 0.50 1 d P C 2
O11 O 0.468(2) 0.141(2) 0.5404(11) 0.074(4) Uani 0.50 1 d P C 2
O10 O 0.749(3) 0.232(2) 0.5716(10) 0.091(5) Uani 0.50 1 d P C 2
O61 O 0.8371(10) 0.7729(8) 0.0503(4) 0.067(2) Uani 1 1 d . . .
C61 C 0.8424(16) 0.6703(15) -0.0096(6) 0.069(3) Uani 1 1 d . . .
C62 C 0.7382(19) 0.4782(15) -0.0146(7) 0.090(4) Uani 1 1 d . . .
H62A H 0.8192 0.4319 -0.0140 0.107 Uiso 1 1 calc R . .
H62B H 0.6512 0.4209 -0.0635 0.107 Uiso 1 1 calc R . .
H62C H 0.6773 0.4580 0.0304 0.107 Uiso 1 1 calc R . .
C63 C 0.7118(16) 0.9556(16) -0.0753(6) 0.072(3) Uani 1 1 d . . .
C64 C 0.5322(17) 0.912(2) -0.1163(8) 0.093(4) Uani 1 1 d . . .
H64A H 0.5438 0.9514 -0.1653 0.111 Uiso 1 1 calc R . .
H64B H 0.4829 0.9690 -0.0820 0.111 Uiso 1 1 calc R . .
H64C H 0.4535 0.7873 -0.1282 0.111 Uiso 1 1 calc R . .
O51 O 1.1765(9) 1.0544(9) 0.1147(3) 0.0594(17) Uani 1 1 d . . .
O41 O 1.0749(10) 1.2765(9) 0.0659(4) 0.0675(19) Uani 1 1 d . . .
O71 O 0.7340(9) 0.9879(11) 0.0016(4) 0.071(2) Uani 1 1 d . . .
C100 C -0.0221(19) 0.6350(17) 0.2233(8) 0.079(3) Uani 1 1 d D . .
N100 N -0.150(2) 0.5706(16) 0.2448(8) 0.104(4) Uani 1 1 d . D .
C101 C 0.115(3) 0.687(3) 0.1762(12) 0.079(5) Uiso 0.65 1 d P D 1
H10A H 0.0744 0.7099 0.1283 0.095 Uiso 0.65 1 calc PR D 1
H10B H 0.1439 0.5950 0.1619 0.095 Uiso 0.65 1 calc PR D 1
H10C H 0.2211 0.7915 0.2065 0.095 Uiso 0.65 1 calc PR D 1
C110 C 0.159(3) 0.756(5) 0.216(3) 0.099(12) Uiso 0.35 1 d PD D 2
H11A H 0.2213 0.8389 0.2669 0.119 Uiso 0.35 1 calc PR D 2
H11B H 0.1560 0.8181 0.1760 0.119 Uiso 0.35 1 calc PR D 2
H11C H 0.2215 0.6932 0.2013 0.119 Uiso 0.35 1 calc PR D 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
Cu1 O71 1.970(7) . y
Cu1 O51 1.981(6) . y
Cu1 O41 1.996(7) . y
Cu1 O61 1.997(7) . y
Cu1 N3 2.240(8) . y
Cu1 Cu1 2.634(2) 2_775 y
O3 C1 1.246(11) . ?
O4 C12 1.227(12) . ?
N2 C12 1.424(11) . ?
N2 C13 1.435(11) . ?
N2 C1 1.436(13) . ?
N3 C16 1.335(11) . ?
N3 C17 1.355(11) . ?
C1 C2 1.489(14) . ?
C2 C3 1.404(14) . ?
C2 C11 1.429(12) . ?
C3 C4 1.411(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.436(13) . ?
C5 N1 1.516(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(12) . ?
C6 C11 1.436(12) . ?
C7 C8 1.396(14) . ?
C7 N10 1.408(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.422(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.427(13) . ?
C10 C12 1.512(13) . ?
C13 C17 1.398(12) . ?
C13 C14 1.411(12) . ?
C14 C15 1.387(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.367(13) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N1 O2 1.258(19) . ?
N1 O1 1.28(2) . ?
N10 O11 1.22(2) . ?
N10 O10 1.25(2) . ?
O61 C61 1.301(12) . ?
C61 O41 1.291(13) 2_775 ?
C61 C62 1.521(15) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 O51 1.266(12) 2_775 ?
C63 O71 1.309(12) . ?
C63 C64 1.511(15) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
O51 C63 1.266(12) 2_775 ?
O41 C61 1.291(13) 2_775 ?
C100 N100 1.119(16) . ?
C100 C101 1.45(2) . ?
C100 C110 1.470(10) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C110 H11A 0.9800 . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O71 Cu1 O51 169.5(2) . . y
O71 Cu1 O41 91.8(3) . . y
O51 Cu1 O41 89.0(3) . . y
O71 Cu1 O61 87.1(3) . . y
O51 Cu1 O61 90.2(3) . . y
O41 Cu1 O61 169.8(3) . . y
O71 Cu1 N3 95.4(3) . . y
O51 Cu1 N3 94.9(3) . . y
O41 Cu1 N3 98.3(3) . . y
O61 Cu1 N3 91.9(3) . . y
O71 Cu1 Cu1 85.25(19) . 2_775 y
O51 Cu1 Cu1 84.32(18) . 2_775 y
O41 Cu1 Cu1 86.8(2) . 2_775 y
O61 Cu1 Cu1 83.02(19) . 2_775 y
N3 Cu1 Cu1 174.8(2) . 2_775 y
C12 N2 C13 118.1(7) . . ?
C12 N2 C1 123.5(8) . . ?
C13 N2 C1 117.9(7) . . ?
C16 N3 C17 119.1(8) . . ?
C16 N3 Cu1 122.6(6) . . ?
C17 N3 Cu1 118.2(5) . . ?
O3 C1 N2 120.1(9) . . ?
O3 C1 C2 123.4(10) . . ?
N2 C1 C2 116.6(8) . . ?
C3 C2 C11 119.7(9) . . ?
C3 C2 C1 118.0(9) . . ?
C11 C2 C1 122.3(9) . . ?
C2 C3 C4 119.5(9) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 121.5(9) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 121.4(9) . . ?
C4 C5 N1 121.2(10) . . ?
C6 C5 N1 117.3(10) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
N1 C5 H5 4.9 . . ?
C7 C6 C11 117.0(8) . . ?
C7 C6 C5 126.0(8) . . ?
C11 C6 C5 116.9(8) . . ?
C8 C7 N10 115.3(11) . . ?
C8 C7 C6 122.3(9) . . ?
N10 C7 C6 122.4(12) . . ?
C8 C7 H7 118.9 . . ?
N10 C7 H7 3.8 . . ?
C6 C7 H7 118.9 . . ?
C7 C8 C9 120.3(9) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 118.9(9) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 121.6(9) . . ?
C9 C10 C12 117.5(9) . . ?
C11 C10 C12 120.7(8) . . ?
C10 C11 C2 119.0(8) . . ?
C10 C11 C6 120.0(7) . . ?
C2 C11 C6 121.0(8) . . ?
O4 C12 N2 119.1(8) . . ?
O4 C12 C10 123.8(8) . . ?
N2 C12 C10 117.1(9) . . ?
C17 C13 C14 119.3(8) . . ?
C17 C13 N2 118.3(7) . . ?
C14 C13 N2 122.3(8) . . ?
C15 C14 C13 118.9(8) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C16 C15 C14 118.0(8) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
N3 C16 C15 124.4(8) . . ?
N3 C16 H16 117.8 . . ?
C15 C16 H16 117.8 . . ?
N3 C17 C13 120.4(7) . . ?
N3 C17 H17 119.8 . . ?
C13 C17 H17 119.8 . . ?
O2 N1 O1 122.5(15) . . ?
O2 N1 C5 118.2(14) . . ?
O1 N1 C5 119.1(13) . . ?
O11 N10 O10 123.8(18) . . ?
O11 N10 C7 118.3(16) . . ?
O10 N10 C7 117.8(18) . . ?
C61 O61 Cu1 125.5(7) . . ?
O41 C61 O61 123.2(10) 2_775 . ?
O41 C61 C62 119.1(9) 2_775 . ?
O61 C61 C62 117.6(10) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O51 C63 O71 124.1(9) 2_775 . ?
O51 C63 C64 120.5(9) 2_775 . ?
O71 C63 C64 115.2(10) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 O51 Cu1 123.9(6) 2_775 . ?
C61 O41 Cu1 121.5(7) 2_775 . ?
C63 O71 Cu1 122.4(7) . . ?
N100 C100 C101 164.9(18) . . ?
N100 C100 C110 163(2) . . ?
C101 C100 C110 31.3(18) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
C100 C110 H11A 109.5 . . ?
C100 C110 H11B 109.5 . . ?
H11A C110 H11B 109.5 . . ?
C100 C110 H11C 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 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
O71 Cu1 N3 C16 -81.0(7) . . . . ?
O51 Cu1 N3 C16 101.3(7) . . . . ?
O41 Cu1 N3 C16 11.6(7) . . . . ?
O61 Cu1 N3 C16 -168.3(7) . . . . ?
Cu1 Cu1 N3 C16 -177.6(18) 2_775 . . . ?
O71 Cu1 N3 C17 102.0(7) . . . . ?
O51 Cu1 N3 C17 -75.7(7) . . . . ?
O41 Cu1 N3 C17 -165.4(7) . . . . ?
O61 Cu1 N3 C17 14.7(7) . . . . ?
Cu1 Cu1 N3 C17 5(3) 2_775 . . . ?
C12 N2 C1 O3 -174.4(8) . . . . ?
C13 N2 C1 O3 -2.2(13) . . . . ?
C12 N2 C1 C2 5.8(12) . . . . ?
C13 N2 C1 C2 177.9(7) . . . . ?
O3 C1 C2 C3 2.9(14) . . . . ?
N2 C1 C2 C3 -177.3(8) . . . . ?
O3 C1 C2 C11 -179.1(9) . . . . ?
N2 C1 C2 C11 0.7(13) . . . . ?
C11 C2 C3 C4 2.8(14) . . . . ?
C1 C2 C3 C4 -179.1(8) . . . . ?
C2 C3 C4 C5 -0.2(15) . . . . ?
C3 C4 C5 C6 -0.5(15) . . . . ?
C3 C4 C5 N1 -175.3(10) . . . . ?
C4 C5 C6 C7 -176.8(9) . . . . ?
N1 C5 C6 C7 -1.8(14) . . . . ?
C4 C5 C6 C11 -1.4(13) . . . . ?
N1 C5 C6 C11 173.6(9) . . . . ?
C11 C6 C7 C8 -0.3(13) . . . . ?
C5 C6 C7 C8 175.1(8) . . . . ?
C11 C6 C7 N10 178.0(11) . . . . ?
C5 C6 C7 N10 -6.6(16) . . . . ?
N10 C7 C8 C9 -177.0(10) . . . . ?
C6 C7 C8 C9 1.3(14) . . . . ?
C7 C8 C9 C10 -1.0(13) . . . . ?
C8 C9 C10 C11 -0.3(13) . . . . ?
C8 C9 C10 C12 -177.0(8) . . . . ?
C9 C10 C11 C2 -179.5(8) . . . . ?
C12 C10 C11 C2 -3.0(12) . . . . ?
C9 C10 C11 C6 1.4(13) . . . . ?
C12 C10 C11 C6 177.9(7) . . . . ?
C3 C2 C11 C10 176.1(8) . . . . ?
C1 C2 C11 C10 -1.9(13) . . . . ?
C3 C2 C11 C6 -4.8(13) . . . . ?
C1 C2 C11 C6 177.2(8) . . . . ?
C7 C6 C11 C10 -1.1(12) . . . . ?
C5 C6 C11 C10 -176.9(8) . . . . ?
C7 C6 C11 C2 179.9(8) . . . . ?
C5 C6 C11 C2 4.1(12) . . . . ?
C13 N2 C12 O4 -1.5(11) . . . . ?
C1 N2 C12 O4 170.6(8) . . . . ?
C13 N2 C12 C10 177.5(7) . . . . ?
C1 N2 C12 C10 -10.4(11) . . . . ?
C9 C10 C12 O4 4.5(13) . . . . ?
C11 C10 C12 O4 -172.2(8) . . . . ?
C9 C10 C12 N2 -174.4(8) . . . . ?
C11 C10 C12 N2 8.9(11) . . . . ?
C12 N2 C13 C17 102.5(9) . . . . ?
C1 N2 C13 C17 -70.0(10) . . . . ?
C12 N2 C13 C14 -73.2(11) . . . . ?
C1 N2 C13 C14 114.2(9) . . . . ?
C17 C13 C14 C15 -1.2(13) . . . . ?
N2 C13 C14 C15 174.4(8) . . . . ?
C13 C14 C15 C16 0.7(14) . . . . ?
C17 N3 C16 C15 -1.5(14) . . . . ?
Cu1 N3 C16 C15 -178.5(7) . . . . ?
C14 C15 C16 N3 0.7(14) . . . . ?
C16 N3 C17 C13 0.9(13) . . . . ?
Cu1 N3 C17 C13 178.0(6) . . . . ?
C14 C13 C17 N3 0.4(13) . . . . ?
N2 C13 C17 N3 -175.4(8) . . . . ?
C4 C5 N1 O2 -134.7(14) . . . . ?
C6 C5 N1 O2 50.3(17) . . . . ?
C4 C5 N1 O1 40(2) . . . . ?
C6 C5 N1 O1 -135.2(14) . . . . ?
C8 C7 N10 O11 148.3(15) . . . . ?
C6 C7 N10 O11 -30(2) . . . . ?
C8 C7 N10 O10 -34(2) . . . . ?
C6 C7 N10 O10 148.0(15) . . . . ?
O71 Cu1 O61 C61 85.3(9) . . . . ?
O51 Cu1 O61 C61 -84.5(9) . . . . ?
O41 Cu1 O61 C61 1(2) . . . . ?
N3 Cu1 O61 C61 -179.4(9) . . . . ?
Cu1 Cu1 O61 C61 -0.3(9) 2_775 . . . ?
Cu1 O61 C61 O41 1.0(17) . . . 2_775 ?
Cu1 O61 C61 C62 -176.1(8) . . . . ?
O71 Cu1 O51 C63 10(2) . . . 2_775 ?
O41 Cu1 O51 C63 -85.0(9) . . . 2_775 ?
O61 Cu1 O51 C63 84.8(9) . . . 2_775 ?
N3 Cu1 O51 C63 176.7(9) . . . 2_775 ?
Cu1 Cu1 O51 C63 1.9(9) 2_775 . . 2_775 ?
O71 Cu1 O41 C61 -86.0(9) . . . 2_775 ?
O51 Cu1 O41 C61 83.5(9) . . . 2_775 ?
O61 Cu1 O41 C61 -2(2) . . . 2_775 ?
N3 Cu1 O41 C61 178.3(8) . . . 2_775 ?
Cu1 Cu1 O41 C61 -0.8(8) 2_775 . . 2_775 ?
O51 C63 O71 Cu1 0.6(17) 2_775 . . . ?
C64 C63 O71 Cu1 174.5(8) . . . . ?
O51 Cu1 O71 C63 -9(2) . . . . ?
O41 Cu1 O71 C63 85.1(9) . . . . ?
O61 Cu1 O71 C63 -84.7(9) . . . . ?
N3 Cu1 O71 C63 -176.3(9) . . . . ?
Cu1 Cu1 O71 C63 -1.5(9) 2_775 . . . ?

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        24.49
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.142
_database_code_depnum_ccdc_archive 'CCDC 958092'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jaktrif

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H30 Cu F3 N10 O15 S'
_chemical_formula_weight         1211.48

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.966(2)
_cell_length_b                   14.668(3)
_cell_length_c                   15.581(3)
_cell_angle_alpha                109.59(3)
_cell_angle_beta                 103.35(3)
_cell_angle_gamma                93.41(3)
_cell_volume                     2478.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    121(2)
_cell_measurement_reflns_used    9443
_cell_measurement_theta_min      1.4393
_cell_measurement_theta_max      31.3867

_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Crystalclear

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      121(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 Saturn 724'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28442
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8359
_reflns_number_gt                7752
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0678P)²+5.1219P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8359
_refine_ls_number_parameters     778
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.1888
_refine_ls_wR_factor_gt          0.1845
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.184
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.29200(5) 0.51777(4) 0.33423(5) 0.0429(2) Uani 1 1 d . . .
N1 N -0.6805(5) 0.3110(4) -0.0086(4) 0.0731(16) Uani 1 1 d D . .
O1 O -0.7187(8) 0.2430(9) -0.0905(7) 0.107(4) Uani 0.55 1 d PD A 1
O2 O -0.7414(7) 0.3393(7) 0.0424(6) 0.064(2) Uani 0.55 1 d PD A 1
O10 O -0.7162(10) 0.2279(8) -0.0213(11) 0.093(4) Uani 0.45 1 d PD A 2
O20 O -0.7435(9) 0.3793(8) -0.0014(11) 0.094(4) Uani 0.45 1 d PD A 2
N2 N -0.1437(4) 0.5247(3) 0.1473(3) 0.0486(11) Uani 1 1 d . . .
N3 N 0.1725(3) 0.5633(3) 0.2505(3) 0.0441(10) Uani 1 1 d . . .
O3 O -0.1249(3) 0.3744(3) 0.0494(3) 0.0560(9) Uani 1 1 d . . .
O4 O -0.1613(4) 0.6716(3) 0.2517(4) 0.0834(15) Uani 1 1 d . . .
C1 C -0.1889(4) 0.4282(4) 0.0841(4) 0.0443(12) Uani 1 1 d . . .
C2 C -0.3152(4) 0.3988(3) 0.0651(3) 0.0423(11) Uani 1 1 d . . .
C3 C -0.3643(5) 0.3053(4) 0.0069(4) 0.0561(14) Uani 1 1 d . A .
H3 H -0.3176 0.2588 -0.0188 0.067 Uiso 1 1 calc R . .
C4 C -0.4857(6) 0.2790(4) -0.0142(4) 0.0637(16) Uani 1 1 d . . .
H4 H -0.5205 0.2142 -0.0544 0.076 Uiso 1 1 calc R A .
C5 C -0.5531(5) 0.3441(5) 0.0215(4) 0.0550(14) Uani 1 1 d . A .
C6 C -0.5100(5) 0.4416(4) 0.0834(4) 0.0520(14) Uani 1 1 d . . .
C7 C -0.5726(5) 0.5158(5) 0.1233(5) 0.0636(17) Uani 1 1 d . A .
H7 H -0.6547 0.5014 0.1098 0.076 Uiso 1 1 calc R . .
C8 C -0.5185(6) 0.6075(5) 0.1806(5) 0.0760(19) Uani 1 1 d . . .
H8 H -0.5637 0.6560 0.2048 0.091 Uiso 1 1 calc R A .
C9 C -0.4012(6) 0.6312(5) 0.2041(5) 0.0654(16) Uani 1 1 d . A .
H9 H -0.3651 0.6952 0.2457 0.078 Uiso 1 1 calc R . .
C10 C -0.3348(5) 0.5626(4) 0.1675(4) 0.0505(13) Uani 1 1 d . . .
C11 C -0.3850(4) 0.4668(4) 0.1052(4) 0.0453(12) Uani 1 1 d . A .
C12 C -0.2087(5) 0.5913(4) 0.1929(4) 0.0545(14) Uani 1 1 d . A .
C13 C -0.0211(4) 0.5601(4) 0.1681(4) 0.0513(13) Uani 1 1 d . . .
C14 C 0.0118(5) 0.6310(5) 0.1350(5) 0.0730(19) Uani 1 1 d . . .
H14 H -0.0433 0.6512 0.0931 0.088 Uiso 1 1 calc R . .
C15 C 0.1271(5) 0.6713(5) 0.1647(5) 0.077(2) Uani 1 1 d . . .
H15 H 0.1533 0.7218 0.1454 0.093 Uiso 1 1 calc R . .
C16 C 0.2044(5) 0.6369(4) 0.2233(4) 0.0602(15) Uani 1 1 d . . .
H16 H 0.2835 0.6664 0.2453 0.072 Uiso 1 1 calc R . .
C17 C 0.0594(4) 0.5275(3) 0.2238(4) 0.0440(12) Uani 1 1 d . . .
H17 H 0.0344 0.4776 0.2443 0.053 Uiso 1 1 calc R . .
N21 N 0.0749(4) -0.2777(3) -0.1839(3) 0.0444(10) Uani 1 1 d D . .
O21 O 0.1308(3) -0.3384(2) -0.2239(2) 0.0494(9) Uani 1 1 d D . .
O22 O -0.0322(3) -0.2900(3) -0.1976(3) 0.0516(9) Uani 1 1 d D . .
N22 N 0.3111(3) 0.1402(3) 0.1492(3) 0.0370(9) Uani 1 1 d . . .
N23 N 0.3806(3) 0.4068(3) 0.2840(3) 0.0379(9) Uani 1 1 d . . .
O23 O 0.4287(4) 0.1213(3) 0.0511(3) 0.0797(15) Uani 1 1 d . . .
O24 O 0.2050(3) 0.1516(2) 0.2553(2) 0.0415(8) Uani 1 1 d . . .
C21 C 0.3450(5) 0.0887(4) 0.0676(4) 0.0474(12) Uani 1 1 d . . .
C22 C 0.2721(4) -0.0055(3) 0.0047(3) 0.0378(10) Uani 1 1 d . . .
C23 C 0.3009(5) -0.0568(4) -0.0764(4) 0.0482(12) Uani 1 1 d . . .
H23 H 0.3655 -0.0313 -0.0916 0.058 Uiso 1 1 calc R . .
C24 C 0.2343(5) -0.1476(4) -0.1373(3) 0.0448(12) Uani 1 1 d . . .
H24 H 0.2536 -0.1838 -0.1937 0.054 Uiso 1 1 calc R . .
C25 C 0.1415(4) -0.1828(3) -0.1145(3) 0.0370(10) Uani 1 1 d . . .
C26 C 0.1071(4) -0.1346(3) -0.0315(3) 0.0343(10) Uani 1 1 d . . .
C27 C 0.0161(4) -0.1708(3) -0.0022(3) 0.0380(11) Uani 1 1 d . . .
H27 H -0.0296 -0.2324 -0.0406 0.046 Uiso 1 1 calc R . .
C28 C -0.0068(4) -0.1178(3) 0.0808(4) 0.0422(11) Uani 1 1 d . . .
H28 H -0.0691 -0.1428 0.0988 0.051 Uiso 1 1 calc R . .
C29 C 0.0605(4) -0.0265(3) 0.1404(4) 0.0396(11) Uani 1 1 d . . .
H29 H 0.0432 0.0095 0.1978 0.048 Uiso 1 1 calc R . .
C30 C 0.1512(4) 0.0102(3) 0.1149(3) 0.0315(9) Uani 1 1 d . . .
C31 C 0.1766(4) -0.0426(3) 0.0292(3) 0.0344(10) Uani 1 1 d . . .
C32 C 0.2217(4) 0.1054(3) 0.1802(3) 0.0360(10) Uani 1 1 d . . .
C33 C 0.3794(4) 0.2350(3) 0.2089(3) 0.0374(10) Uani 1 1 d . . .
C34 C 0.4978(4) 0.2444(4) 0.2449(4) 0.0451(12) Uani 1 1 d . . .
H34 H 0.5372 0.1889 0.2335 0.054 Uiso 1 1 calc R . .
C35 C 0.5572(4) 0.3376(4) 0.2983(4) 0.0497(13) Uani 1 1 d . . .
H35 H 0.6393 0.3476 0.3220 0.060 Uiso 1 1 calc R . .
C36 C 0.4967(4) 0.4159(4) 0.3170(4) 0.0472(12) Uani 1 1 d . . .
H36 H 0.5388 0.4791 0.3549 0.057 Uiso 1 1 calc R . .
C37 C 0.3238(4) 0.3168(3) 0.2284(3) 0.0367(10) Uani 1 1 d . . .
H37 H 0.2425 0.3090 0.2016 0.044 Uiso 1 1 calc R . .
N41 N 0.1474(4) -0.1894(3) 0.4399(4) 0.0579(12) Uani 1 1 d . . .
N42 N 0.1158(3) 0.2564(2) 0.4612(3) 0.0323(8) Uani 1 1 d . . .
N43 N 0.2082(3) 0.4793(3) 0.4225(3) 0.0394(9) Uani 1 1 d . . .
O41 O 0.2385(4) -0.2245(3) 0.4495(4) 0.0923(16) Uani 1 1 d . . .
O42 O 0.0514(4) -0.2362(3) 0.4238(3) 0.0640(11) Uani 1 1 d . . .
O43 O 0.2908(3) 0.2735(2) 0.5634(3) 0.0483(9) Uani 1 1 d . . .
O44 O -0.0622(3) 0.2431(2) 0.3632(2) 0.0478(9) Uani 1 1 d . . .
C41 C 0.2037(4) 0.2196(3) 0.5096(3) 0.0373(10) Uani 1 1 d . . .
C42 C 0.1845(4) 0.1128(3) 0.4889(3) 0.0368(10) Uani 1 1 d . . .
C43 C 0.2680(5) 0.0735(4) 0.5366(4) 0.0468(12) Uani 1 1 d . . .
H43 H 0.3350 0.1144 0.5823 0.056 Uiso 1 1 calc R . .
C44 C 0.2528(5) -0.0278(4) 0.5169(4) 0.0500(13) Uani 1 1 d . . .
H44 H 0.3099 -0.0560 0.5491 0.060 Uiso 1 1 calc R . .
C45 C 0.1570(5) -0.0850(3) 0.4523(4) 0.0456(12) Uani 1 1 d . . .
C46 C 0.0655(4) -0.0504(3) 0.4017(3) 0.0399(11) Uani 1 1 d . . .
C47 C -0.0376(5) -0.1058(3) 0.3353(4) 0.0458(12) Uani 1 1 d . . .
H47 H -0.0490 -0.1749 0.3184 0.055 Uiso 1 1 calc R . .
C48 C -0.1219(5) -0.0626(4) 0.2947(4) 0.0485(13) Uani 1 1 d . . .
H48 H -0.1912 -0.1017 0.2507 0.058 Uiso 1 1 calc R . .
C49 C -0.1069(4) 0.0388(3) 0.3174(4) 0.0439(11) Uani 1 1 d . . .
H49 H -0.1671 0.0685 0.2907 0.053 Uiso 1 1 calc R . .
C50 C -0.0049(4) 0.0957(3) 0.3784(3) 0.0377(10) Uani 1 1 d . . .
C51 C 0.0824(4) 0.0538(3) 0.4228(3) 0.0359(10) Uani 1 1 d . . .
C52 C 0.0101(4) 0.2028(3) 0.3985(3) 0.0379(10) Uani 1 1 d . . .
C53 C 0.1370(4) 0.3595(3) 0.4765(3) 0.0333(10) Uani 1 1 d . . .
C54 C 0.1158(4) 0.4307(3) 0.5534(3) 0.0406(11) Uani 1 1 d . . .
H54 H 0.0860 0.4139 0.5985 0.049 Uiso 1 1 calc R . .
C55 C 0.1399(4) 0.5271(3) 0.5616(4) 0.0434(12) Uani 1 1 d . . .
H55 H 0.1257 0.5784 0.6126 0.052 Uiso 1 1 calc R . .
C56 C 0.1843(4) 0.5482(3) 0.4956(4) 0.0414(11) Uani 1 1 d . . .
H56 H 0.1989 0.6148 0.5018 0.050 Uiso 1 1 calc R . .
C57 C 0.1840(4) 0.3860(3) 0.4142(3) 0.0366(10) Uani 1 1 d . . .
H57 H 0.2000 0.3360 0.3631 0.044 Uiso 1 1 calc R . .
N60 N 0.4143(4) 0.6318(3) 0.4211(3) 0.0525(11) Uani 1 1 d . . .
C60 C 0.4652(4) 0.7024(4) 0.4761(4) 0.0437(11) Uani 1 1 d . . .
C61 C 0.5282(5) 0.7950(4) 0.5486(4) 0.0524(13) Uani 1 1 d . . .
H61A H 0.5480 0.8401 0.5182 0.063 Uiso 1 1 calc R . .
H61B H 0.5996 0.7828 0.5861 0.063 Uiso 1 1 calc R . .
H61C H 0.4792 0.8240 0.5900 0.063 Uiso 1 1 calc R . .
S1 S 0.50598(15) 0.94840(11) 0.23866(11) 0.0607(4) Uani 1 1 d . . .
O100 O 0.5741(4) 0.8711(3) 0.2408(3) 0.0723(13) Uani 1 1 d . . .
O101 O 0.4310(5) 0.9371(4) 0.1486(3) 0.0967(18) Uani 1 1 d . . .
O102 O 0.5680(4) 1.0447(3) 0.2923(3) 0.0687(12) Uani 1 1 d . . .
C100 C 0.4042(5) 0.9335(4) 0.3042(5) 0.0613(16) Uani 1 1 d . . .
F100 F 0.4570(3) 0.9465(3) 0.3942(3) 0.0762(11) Uani 1 1 d . . .
F101 F 0.3298(3) 0.9996(2) 0.3106(2) 0.0665(9) Uani 1 1 d . . .
F102 F 0.3404(4) 0.8468(3) 0.2662(4) 0.1107(17) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 2.008(4) . y
Cu1 N60 2.011(4) . y
Cu1 N23 2.030(4) . y
Cu1 N43 2.075(4) . y
N1 O2 1.189(8) . ?
N1 O10 1.202(9) . ?
N1 O20 1.280(10) . ?
N1 O1 1.287(9) . ?
N1 C5 1.486(7) . ?
N2 C12 1.394(7) . ?
N2 C1 1.412(6) . ?
N2 C13 1.451(6) . ?
N3 C17 1.338(6) . ?
N3 C16 1.350(7) . ?
O3 C1 1.216(6) . ?
O4 C12 1.226(6) . ?
C1 C2 1.479(7) . ?
C2 C3 1.369(7) . ?
C2 C11 1.416(7) . ?
C3 C4 1.412(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.347(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.413(8) . ?
C6 C7 1.412(8) . ?
C6 C11 1.450(7) . ?
C7 C8 1.359(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.358(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.412(7) . ?
C10 C12 1.467(7) . ?
C13 C17 1.363(7) . ?
C13 C14 1.381(8) . ?
C14 C15 1.376(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N21 O21 1.233(5) . ?
N21 O22 1.241(5) . ?
N21 C25 1.484(6) . ?
N22 C32 1.407(6) . ?
N22 C21 1.408(6) . ?
N22 C33 1.453(6) . ?
N23 C37 1.346(6) . ?
N23 C36 1.347(6) . ?
O23 C21 1.201(6) . ?
O24 C32 1.210(6) . ?
C21 C22 1.478(6) . ?
C22 C23 1.370(7) . ?
C22 C31 1.419(6) . ?
C23 C24 1.409(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.365(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.417(7) . ?
C26 C27 1.414(6) . ?
C26 C31 1.434(6) . ?
C27 C28 1.366(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.413(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.412(7) . ?
C30 C32 1.486(6) . ?
C33 C34 1.378(7) . ?
C33 C37 1.385(6) . ?
C34 C35 1.384(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
N41 O42 1.229(6) . ?
N41 O41 1.232(6) . ?
N41 C45 1.471(6) . ?
N42 C41 1.393(6) . ?
N42 C52 1.403(6) . ?
N42 C53 1.447(5) . ?
N43 C57 1.338(5) . ?
N43 C56 1.347(6) . ?
O43 C41 1.211(6) . ?
O44 C52 1.209(6) . ?
C41 C42 1.482(6) . ?
C42 C43 1.378(7) . ?
C42 C51 1.413(7) . ?
C43 C44 1.404(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.349(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.420(7) . ?
C46 C47 1.407(7) . ?
C46 C51 1.442(6) . ?
C47 C48 1.368(8) . ?
C47 H47 0.9500 . ?
C48 C49 1.397(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.405(7) . ?
C50 C52 1.485(6) . ?
C53 C57 1.374(6) . ?
C53 C54 1.387(7) . ?
C54 C55 1.383(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.371(7) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
N60 C60 1.126(6) . ?
C60 C61 1.464(7) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
S1 O102 1.429(4) . ?
S1 O101 1.431(5) . ?
S1 O100 1.440(4) . ?
S1 C100 1.807(7) . ?
C100 F102 1.312(6) . ?
C100 F100 1.342(7) . ?
C100 F101 1.348(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N60 109.39(17) . . y
N3 Cu1 N23 123.34(17) . . y
N60 Cu1 N23 105.37(17) . . y
N3 Cu1 N43 106.00(16) . . y
N60 Cu1 N43 104.83(18) . . y
N23 Cu1 N43 106.52(15) . . y
O2 N1 O10 89.9(10) . . ?
O2 N1 O20 49.4(7) . . ?
O10 N1 O20 124.0(9) . . ?
O2 N1 O1 122.1(7) . . ?
O10 N1 O1 55.7(8) . . ?
O20 N1 O1 109.8(10) . . ?
O2 N1 C5 122.4(6) . . ?
O10 N1 C5 119.3(8) . . ?
O20 N1 C5 115.3(7) . . ?
O1 N1 C5 115.2(7) . . ?
C12 N2 C1 124.8(4) . . ?
C12 N2 C13 115.7(4) . . ?
C1 N2 C13 119.5(4) . . ?
C17 N3 C16 117.4(5) . . ?
C17 N3 Cu1 122.8(3) . . ?
C16 N3 Cu1 119.8(4) . . ?
O3 C1 N2 120.2(5) . . ?
O3 C1 C2 123.8(5) . . ?
N2 C1 C2 116.0(5) . . ?
C3 C2 C11 120.2(5) . . ?
C3 C2 C1 119.2(5) . . ?
C11 C2 C1 120.6(4) . . ?
C2 C3 C4 118.8(6) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 123.9(5) . . ?
C4 C5 N1 117.3(5) . . ?
C6 C5 N1 118.8(6) . . ?
C7 C6 C5 128.5(6) . . ?
C7 C6 C11 117.4(5) . . ?
C5 C6 C11 114.0(5) . . ?
C8 C7 C6 121.6(6) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 C7 121.5(6) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 119.9(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 121.8(5) . . ?
C9 C10 C12 118.5(5) . . ?
C11 C10 C12 119.7(5) . . ?
C10 C11 C2 120.7(5) . . ?
C10 C11 C6 117.6(5) . . ?
C2 C11 C6 121.7(5) . . ?
O4 C12 N2 120.7(5) . . ?
O4 C12 C10 121.4(5) . . ?
N2 C12 C10 117.9(4) . . ?
C17 C13 C14 120.8(5) . . ?
C17 C13 N2 120.1(5) . . ?
C14 C13 N2 119.0(5) . . ?
C15 C14 C13 117.7(5) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
C14 C15 C16 118.8(5) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
N3 C16 C15 123.0(5) . . ?
N3 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
N3 C17 C13 122.2(5) . . ?
N3 C17 H17 118.9 . . ?
C13 C17 H17 118.9 . . ?
O21 N21 O22 125.0(4) . . ?
O21 N21 C25 117.0(4) . . ?
O22 N21 C25 118.0(4) . . ?
C32 N22 C21 125.5(4) . . ?
C32 N22 C33 117.7(4) . . ?
C21 N22 C33 116.6(4) . . ?
C37 N23 C36 117.1(4) . . ?
C37 N23 Cu1 120.7(3) . . ?
C36 N23 Cu1 121.3(3) . . ?
O23 C21 N22 120.6(4) . . ?
O23 C21 C22 122.9(5) . . ?
N22 C21 C22 116.5(4) . . ?
C23 C22 C31 121.2(4) . . ?
C23 C22 C21 118.2(4) . . ?
C31 C22 C21 120.6(4) . . ?
C22 C23 C24 119.7(5) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C25 C24 C23 119.2(5) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 124.3(4) . . ?
C24 C25 N21 115.4(4) . . ?
C26 C25 N21 120.3(4) . . ?
C27 C26 C25 126.3(4) . . ?
C27 C26 C31 118.4(4) . . ?
C25 C26 C31 115.2(4) . . ?
C28 C27 C26 120.6(4) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 121.3(4) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C30 C29 C28 119.7(4) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 120.4(4) . . ?
C29 C30 C32 118.3(4) . . ?
C31 C30 C32 121.3(4) . . ?
C30 C31 C22 120.0(4) . . ?
C30 C31 C26 119.6(4) . . ?
C22 C31 C26 120.4(4) . . ?
O24 C32 N22 120.8(4) . . ?
O24 C32 C30 123.5(4) . . ?
N22 C32 C30 115.7(4) . . ?
C34 C33 C37 120.1(4) . . ?
C34 C33 N22 121.0(4) . . ?
C37 C33 N22 118.9(4) . . ?
C33 C34 C35 117.5(5) . . ?
C33 C34 H34 121.3 . . ?
C35 C34 H34 121.3 . . ?
C36 C35 C34 119.7(5) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
N23 C36 C35 123.0(4) . . ?
N23 C36 H36 118.5 . . ?
C35 C36 H36 118.5 . . ?
N23 C37 C33 122.5(4) . . ?
N23 C37 H37 118.7 . . ?
C33 C37 H37 118.7 . . ?
O42 N41 O41 123.4(5) . . ?
O42 N41 C45 119.5(5) . . ?
O41 N41 C45 117.1(5) . . ?
C41 N42 C52 126.2(4) . . ?
C41 N42 C53 116.4(3) . . ?
C52 N42 C53 117.3(4) . . ?
C57 N43 C56 117.0(4) . . ?
C57 N43 Cu1 121.8(3) . . ?
C56 N43 Cu1 121.0(3) . . ?
O43 C41 N42 120.4(4) . . ?
O43 C41 C42 123.6(4) . . ?
N42 C41 C42 116.0(4) . . ?
C43 C42 C51 121.4(4) . . ?
C43 C42 C41 118.1(4) . . ?
C51 C42 C41 120.5(4) . . ?
C42 C43 C44 119.2(5) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
C45 C44 C43 119.8(5) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C44 C45 C46 124.7(4) . . ?
C44 C45 N41 115.4(5) . . ?
C46 C45 N41 119.8(5) . . ?
C47 C46 C45 127.4(4) . . ?
C47 C46 C51 117.9(5) . . ?
C45 C46 C51 114.7(4) . . ?
C48 C47 C46 121.6(4) . . ?
C48 C47 H47 119.2 . . ?
C46 C47 H47 119.2 . . ?
C47 C48 C49 120.4(5) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C50 C49 C48 120.2(5) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C49 C50 C51 120.7(4) . . ?
C49 C50 C52 118.9(4) . . ?
C51 C50 C52 120.4(4) . . ?
C50 C51 C42 120.8(4) . . ?
C50 C51 C46 119.1(4) . . ?
C42 C51 C46 120.1(4) . . ?
O44 C52 N42 120.6(4) . . ?
O44 C52 C50 123.4(4) . . ?
N42 C52 C50 116.0(4) . . ?
C57 C53 C54 120.2(4) . . ?
C57 C53 N42 117.9(4) . . ?
C54 C53 N42 121.9(4) . . ?
C55 C54 C53 117.1(5) . . ?
C55 C54 H54 121.4 . . ?
C53 C54 H54 121.4 . . ?
C56 C55 C54 119.6(5) . . ?
C56 C55 H55 120.2 . . ?
C54 C55 H55 120.2 . . ?
N43 C56 C55 123.3(4) . . ?
N43 C56 H56 118.3 . . ?
C55 C56 H56 118.3 . . ?
N43 C57 C53 122.7(4) . . ?
N43 C57 H57 118.7 . . ?
C53 C57 H57 118.7 . . ?
C60 N60 Cu1 166.6(5) . . ?
N60 C60 C61 178.2(6) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O102 S1 O101 115.0(3) . . ?
O102 S1 O100 114.3(3) . . ?
O101 S1 O100 116.0(3) . . ?
O102 S1 C100 103.7(3) . . ?
O101 S1 C100 102.4(3) . . ?
O100 S1 C100 102.8(3) . . ?
F102 C100 F100 107.4(5) . . ?
F102 C100 F101 106.6(5) . . ?
F100 C100 F101 104.5(5) . . ?
F102 C100 S1 112.5(5) . . ?
F100 C100 S1 112.4(4) . . ?
F101 C100 S1 112.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N60 Cu1 N3 C17 -143.9(4) . . . . ?
N23 Cu1 N3 C17 91.5(4) . . . . ?
N43 Cu1 N3 C17 -31.4(4) . . . . ?
N60 Cu1 N3 C16 32.4(5) . . . . ?
N23 Cu1 N3 C16 -92.2(5) . . . . ?
N43 Cu1 N3 C16 144.9(4) . . . . ?
C12 N2 C1 O3 -178.2(5) . . . . ?
C13 N2 C1 O3 2.0(7) . . . . ?
C12 N2 C1 C2 1.2(7) . . . . ?
C13 N2 C1 C2 -178.5(4) . . . . ?
O3 C1 C2 C3 1.5(8) . . . . ?
N2 C1 C2 C3 -177.9(5) . . . . ?
O3 C1 C2 C11 -177.4(5) . . . . ?
N2 C1 C2 C11 3.2(7) . . . . ?
C11 C2 C3 C4 1.7(8) . . . . ?
C1 C2 C3 C4 -177.3(5) . . . . ?
C2 C3 C4 C5 0.2(9) . . . . ?
C3 C4 C5 C6 -1.3(9) . . . . ?
C3 C4 C5 N1 177.0(5) . . . . ?
O2 N1 C5 C4 146.6(8) . . . . ?
O10 N1 C5 C4 35.8(12) . . . . ?
O20 N1 C5 C4 -156.9(10) . . . . ?
O1 N1 C5 C4 -27.5(11) . . . . ?
O2 N1 C5 C6 -35.0(10) . . . . ?
O10 N1 C5 C6 -145.8(10) . . . . ?
O20 N1 C5 C6 21.5(11) . . . . ?
O1 N1 C5 C6 150.9(9) . . . . ?
C4 C5 C6 C7 178.7(6) . . . . ?
N1 C5 C6 C7 0.4(8) . . . . ?
C4 C5 C6 C11 0.5(8) . . . . ?
N1 C5 C6 C11 -177.8(5) . . . . ?
C5 C6 C7 C8 -178.7(6) . . . . ?
C11 C6 C7 C8 -0.5(8) . . . . ?
C6 C7 C8 C9 -1.7(10) . . . . ?
C7 C8 C9 C10 1.8(11) . . . . ?
C8 C9 C10 C11 0.2(10) . . . . ?
C8 C9 C10 C12 178.9(6) . . . . ?
C9 C10 C11 C2 177.1(5) . . . . ?
C12 C10 C11 C2 -1.6(8) . . . . ?
C9 C10 C11 C6 -2.2(8) . . . . ?
C12 C10 C11 C6 179.1(5) . . . . ?
C3 C2 C11 C10 178.1(5) . . . . ?
C1 C2 C11 C10 -2.9(7) . . . . ?
C3 C2 C11 C6 -2.6(7) . . . . ?
C1 C2 C11 C6 176.4(4) . . . . ?
C7 C6 C11 C10 2.3(7) . . . . ?
C5 C6 C11 C10 -179.2(5) . . . . ?
C7 C6 C11 C2 -177.0(5) . . . . ?
C5 C6 C11 C2 1.4(7) . . . . ?
C1 N2 C12 O4 175.1(6) . . . . ?
C13 N2 C12 O4 -5.2(8) . . . . ?
C1 N2 C12 C10 -5.6(8) . . . . ?
C13 N2 C12 C10 174.2(5) . . . . ?
C9 C10 C12 O4 6.3(9) . . . . ?
C11 C10 C12 O4 -175.0(6) . . . . ?
C9 C10 C12 N2 -173.1(5) . . . . ?
C11 C10 C12 N2 5.7(8) . . . . ?
C12 N2 C13 C17 107.2(6) . . . . ?
C1 N2 C13 C17 -73.0(7) . . . . ?
C12 N2 C13 C14 -69.2(8) . . . . ?
C1 N2 C13 C14 110.6(6) . . . . ?
C17 C13 C14 C15 -3.7(11) . . . . ?
N2 C13 C14 C15 172.7(6) . . . . ?
C13 C14 C15 C16 2.0(12) . . . . ?
C17 N3 C16 C15 -4.4(9) . . . . ?
Cu1 N3 C16 C15 179.1(6) . . . . ?
C14 C15 C16 N3 2.0(12) . . . . ?
C16 N3 C17 C13 2.7(8) . . . . ?
Cu1 N3 C17 C13 179.0(4) . . . . ?
C14 C13 C17 N3 1.4(9) . . . . ?
N2 C13 C17 N3 -175.0(5) . . . . ?
N3 Cu1 N23 C37 -58.4(4) . . . . ?
N60 Cu1 N23 C37 175.2(3) . . . . ?
N43 Cu1 N23 C37 64.2(4) . . . . ?
N3 Cu1 N23 C36 132.7(4) . . . . ?
N60 Cu1 N23 C36 6.4(4) . . . . ?
N43 Cu1 N23 C36 -104.6(4) . . . . ?
C32 N22 C21 O23 -173.8(5) . . . . ?
C33 N22 C21 O23 2.4(8) . . . . ?
C32 N22 C21 C22 6.6(7) . . . . ?
C33 N22 C21 C22 -177.2(4) . . . . ?
O23 C21 C22 C23 -0.9(8) . . . . ?
N22 C21 C22 C23 178.7(5) . . . . ?
O23 C21 C22 C31 177.6(6) . . . . ?
N22 C21 C22 C31 -2.8(7) . . . . ?
C31 C22 C23 C24 0.6(8) . . . . ?
C21 C22 C23 C24 179.1(5) . . . . ?
C22 C23 C24 C25 0.2(8) . . . . ?
C23 C24 C25 C26 -0.9(7) . . . . ?
C23 C24 C25 N21 178.6(4) . . . . ?
O21 N21 C25 C24 36.6(6) . . . . ?
O22 N21 C25 C24 -143.2(5) . . . . ?
O21 N21 C25 C26 -143.9(4) . . . . ?
O22 N21 C25 C26 36.4(6) . . . . ?
C24 C25 C26 C27 -176.1(5) . . . . ?
N21 C25 C26 C27 4.4(7) . . . . ?
C24 C25 C26 C31 0.8(7) . . . . ?
N21 C25 C26 C31 -178.7(4) . . . . ?
C25 C26 C27 C28 178.5(4) . . . . ?
C31 C26 C27 C28 1.7(6) . . . . ?
C26 C27 C28 C29 -1.0(7) . . . . ?
C27 C28 C29 C30 -0.2(7) . . . . ?
C28 C29 C30 C31 0.6(7) . . . . ?
C28 C29 C30 C32 -178.7(4) . . . . ?
C29 C30 C31 C22 -178.3(4) . . . . ?
C32 C30 C31 C22 0.9(6) . . . . ?
C29 C30 C31 C26 0.2(6) . . . . ?
C32 C30 C31 C26 179.4(4) . . . . ?
C23 C22 C31 C30 177.8(4) . . . . ?
C21 C22 C31 C30 -0.7(7) . . . . ?
C23 C22 C31 C26 -0.7(7) . . . . ?
C21 C22 C31 C26 -179.2(4) . . . . ?
C27 C26 C31 C30 -1.3(6) . . . . ?
C25 C26 C31 C30 -178.5(4) . . . . ?
C27 C26 C31 C22 177.2(4) . . . . ?
C25 C26 C31 C22 0.0(6) . . . . ?
C21 N22 C32 O24 173.9(5) . . . . ?
C33 N22 C32 O24 -2.3(6) . . . . ?
C21 N22 C32 C30 -6.3(7) . . . . ?
C33 N22 C32 C30 177.5(4) . . . . ?
C29 C30 C32 O24 1.4(7) . . . . ?
C31 C30 C32 O24 -177.9(4) . . . . ?
C29 C30 C32 N22 -178.4(4) . . . . ?
C31 C30 C32 N22 2.3(6) . . . . ?
C32 N22 C33 C34 120.4(5) . . . . ?
C21 N22 C33 C34 -56.1(6) . . . . ?
C32 N22 C33 C37 -60.3(6) . . . . ?
C21 N22 C33 C37 123.2(5) . . . . ?
C37 C33 C34 C35 -1.6(7) . . . . ?
N22 C33 C34 C35 177.7(4) . . . . ?
C33 C34 C35 C36 2.9(8) . . . . ?
C37 N23 C36 C35 -1.7(8) . . . . ?
Cu1 N23 C36 C35 167.5(4) . . . . ?
C34 C35 C36 N23 -1.3(9) . . . . ?
C36 N23 C37 C33 3.2(7) . . . . ?
Cu1 N23 C37 C33 -166.1(4) . . . . ?
C34 C33 C37 N23 -1.6(7) . . . . ?
N22 C33 C37 N23 179.1(4) . . . . ?
N3 Cu1 N43 C57 109.9(4) . . . . ?
N60 Cu1 N43 C57 -134.5(4) . . . . ?
N23 Cu1 N43 C57 -23.1(4) . . . . ?
N3 Cu1 N43 C56 -75.5(4) . . . . ?
N60 Cu1 N43 C56 40.1(4) . . . . ?
N23 Cu1 N43 C56 151.5(3) . . . . ?
C52 N42 C41 O43 -178.8(4) . . . . ?
C53 N42 C41 O43 2.2(7) . . . . ?
C52 N42 C41 C42 2.8(7) . . . . ?
C53 N42 C41 C42 -176.3(4) . . . . ?
O43 C41 C42 C43 3.0(7) . . . . ?
N42 C41 C42 C43 -178.6(4) . . . . ?
O43 C41 C42 C51 -177.8(5) . . . . ?
N42 C41 C42 C51 0.6(6) . . . . ?
C51 C42 C43 C44 2.0(8) . . . . ?
C41 C42 C43 C44 -178.8(5) . . . . ?
C42 C43 C44 C45 -0.4(8) . . . . ?
C43 C44 C45 C46 -1.3(8) . . . . ?
C43 C44 C45 N41 -177.6(5) . . . . ?
O42 N41 C45 C44 144.0(5) . . . . ?
O41 N41 C45 C44 -33.6(8) . . . . ?
O42 N41 C45 C46 -32.4(7) . . . . ?
O41 N41 C45 C46 149.9(6) . . . . ?
C44 C45 C46 C47 -178.3(5) . . . . ?
N41 C45 C46 C47 -2.2(8) . . . . ?
C44 C45 C46 C51 1.2(7) . . . . ?
N41 C45 C46 C51 177.3(4) . . . . ?
C45 C46 C47 C48 176.8(5) . . . . ?
C51 C46 C47 C48 -2.7(7) . . . . ?
C46 C47 C48 C49 0.9(8) . . . . ?
C47 C48 C49 C50 2.4(8) . . . . ?
C48 C49 C50 C51 -3.7(7) . . . . ?
C48 C49 C50 C52 177.9(4) . . . . ?
C49 C50 C51 C42 -176.8(4) . . . . ?
C52 C50 C51 C42 1.5(7) . . . . ?
C49 C50 C51 C46 1.8(7) . . . . ?
C52 C50 C51 C46 -179.9(4) . . . . ?
C43 C42 C51 C50 176.6(5) . . . . ?
C41 C42 C51 C50 -2.6(7) . . . . ?
C43 C42 C51 C46 -2.0(7) . . . . ?
C41 C42 C51 C46 178.8(4) . . . . ?
C47 C46 C51 C50 1.4(7) . . . . ?
C45 C46 C51 C50 -178.2(4) . . . . ?
C47 C46 C51 C42 -180.0(4) . . . . ?
C45 C46 C51 C42 0.4(6) . . . . ?
C41 N42 C52 O44 177.0(4) . . . . ?
C53 N42 C52 O44 -3.9(7) . . . . ?
C41 N42 C52 C50 -3.8(7) . . . . ?
C53 N42 C52 C50 175.2(4) . . . . ?
C49 C50 C52 O44 -1.0(7) . . . . ?
C51 C50 C52 O44 -179.3(5) . . . . ?
C49 C50 C52 N42 179.9(4) . . . . ?
C51 C50 C52 N42 1.6(6) . . . . ?
C41 N42 C53 C57 93.5(5) . . . . ?
C52 N42 C53 C57 -85.6(5) . . . . ?
C41 N42 C53 C54 -83.8(5) . . . . ?
C52 N42 C53 C54 97.1(5) . . . . ?
C57 C53 C54 C55 2.4(7) . . . . ?
N42 C53 C54 C55 179.6(4) . . . . ?
C53 C54 C55 C56 -0.9(7) . . . . ?
C57 N43 C56 C55 1.6(7) . . . . ?
Cu1 N43 C56 C55 -173.2(4) . . . . ?
C54 C55 C56 N43 -1.1(7) . . . . ?
C56 N43 C57 C53 -0.1(7) . . . . ?
Cu1 N43 C57 C53 174.7(3) . . . . ?
C54 C53 C57 N43 -1.9(7) . . . . ?
N42 C53 C57 N43 -179.2(4) . . . . ?
N3 Cu1 N60 C60 63(2) . . . . ?
N23 Cu1 N60 C60 -162.6(19) . . . . ?
N43 Cu1 N60 C60 -50(2) . . . . ?
Cu1 N60 C60 C61 6(21) . . . . ?
O102 S1 C100 F102 -178.3(4) . . . . ?
O101 S1 C100 F102 61.7(5) . . . . ?
O100 S1 C100 F102 -59.0(5) . . . . ?
O102 S1 C100 F100 -56.9(4) . . . . ?
O101 S1 C100 F100 -176.9(4) . . . . ?
O100 S1 C100 F100 62.5(4) . . . . ?
O102 S1 C100 F101 61.0(4) . . . . ?
O101 S1 C100 F101 -59.0(5) . . . . ?
O100 S1 C100 F101 -179.6(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 958093'
