# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Paul Plieger'
_publ_contact_author_email       P.G.PLIEGER@MASSEY.AC.NZ

_publ_section_title              
;
Anion-induced contraction of helical receptors
;
loop_
_publ_author_name
'Paul Plieger'
'Lauren A. Ferguson'
'Ross Forgan'
'Geoffrey Jameson'
'Quintin W. Knapp'
'Simon Parsons'
;
P.Tasker
;
'Marco Wenzel'
'Fraser White'

# Attachment '719944_new.cif'

data_lfb_gj
_database_code_depnum_ccdc_archive 'CCDC 719944'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H106 B4 Cu2 F16 N10 O8'
_chemical_formula_weight         1665.95

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'
B B 0.0013 0.0007 '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'
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
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.6568(12)
_cell_length_b                   19.259(3)
_cell_length_c                   20.910(3)
_cell_angle_alpha                87.723(5)
_cell_angle_beta                 75.455(3)
_cell_angle_gamma                79.962(3)
_cell_volume                     4090.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4541
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      22.53

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1740
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_type   Multiscan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-2004/1

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22739
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.1248
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         23.26
_reflns_number_total             11456
_reflns_number_gt                5966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

The intensity statistics (<E^2^ - 1> = 0.783) betrayed the possibility of
either acentricity or twinning. XPREP indicated a possible monoclinic
C-centered cell with a figure of merit of 0.327 deg but with very much
poorer merging statistics (R(int) = 0.21) than those for triclinic. When
refinement in P-1 died at R1 ~ 0.20, twinning
(twin law: -1 0 0/0 -1 0/-1 0 1) was included,
lowering R1 to ~0.12 (minor twin component fraction 0.302(2)). Because of
rather high overall Debye-Waller factor (for example U~equiv~ for Cu atoms
are > 0.05 A^2^), data did not extend to high resolution, and refinement was
limited to data with resolution of only 0.90 A. Three of the five BF~4~^-^
sites are disordered, including one about a centre of inversion, and one
present both disordered and in half overall occupancy. Because of limited
data, restraints were applied to the anisotropic atomic displacement
parameters of all carbon, nitrogen, oxygen, fluorine and boron atoms. In
addition, free variables were assigned to distances and angles of BF~4~^-^
groups and to bond distances of terminal atoms in the ligand in the
acetonitrile solvate species. While more complex models could be invoked
for disorder of several BF~4~^-^ groups, leading to less eccentric atomic
displacement parameters, the absence of significant residual electron
density around these groups and the extra parameters needed did not justify
such invocation. That crystal quality left something to be
desired was evident in the number of poorly equivalent reflections (>200)
and that the solvate model was incomplete was evident in two void volumes
of ~65 A^3^ with more than 70 electrons smeared throughout each. Because of
relatively small size of void volumes and the presence of twinning, the
X-ray diffraction data were not SQUEEZEd. Accordingly, a small number (85)
reflections that showed very poor agreement between F~obs~ and F~calc~ were
omitted from least-squares refinement, leading to a small improvcement in
R1 and wR2. The final value for R1 of 0.106 reflects, in large part, the
incomplete description of solvate species. The two crystallographically
independent copper ions show statistically insignificant differences in the
bond parameters -- no restraints were applied to the geometry around the
copper ions. Thus, the various restraints and data-handling practices
employed do not appear to have led to bias in the metrical details of
interest.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11456
_refine_ls_number_parameters     1094
_refine_ls_number_restraints     1892
_refine_ls_R_factor_all          0.1769
_refine_ls_R_factor_gt           0.1034
_refine_ls_wR_factor_ref         0.2949
_refine_ls_wR_factor_gt          0.2433
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_restrained_S_all      0.903
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.97398(14) 0.20080(8) 0.73276(8) 0.0490(4) Uani 1 1 d . . .
Cu1 Cu 0.31200(14) 0.29630(8) 0.73993(8) 0.0522(5) Uani 1 1 d . . .
O1 O 0.3650(8) 0.3752(4) 0.6922(4) 0.053(2) Uani 1 1 d U . .
C1 C 0.3694(12) 0.4381(6) 0.7158(6) 0.050(2) Uani 1 1 d U . .
C2 C 0.3116(13) 0.4574(6) 0.7835(7) 0.0550(19) Uani 1 1 d U . .
C21 C 0.2460(13) 0.4157(7) 0.8333(7) 0.058(2) Uani 1 1 d U . .
H21A H 0.2055 0.4350 0.8750 0.070 Uiso 1 1 calc R . .
N2 N 0.2414(11) 0.3498(6) 0.8214(5) 0.060(2) Uani 1 1 d DU . .
O23 O 0.1676(9) 0.3207(5) 0.8762(5) 0.076(3) Uani 1 1 d DU . .
H23A H 0.1614 0.2804 0.8675 0.091 Uiso 1 1 calc R . .
C3 C 0.3292(14) 0.5267(7) 0.8030(7) 0.062(2) Uani 1 1 d U . .
H3A H 0.2932 0.5403 0.8468 0.075 Uiso 1 1 calc R . .
C4 C 0.3918(14) 0.5709(7) 0.7634(7) 0.066(2) Uani 1 1 d DU . .
C41 C 0.4157(13) 0.6423(6) 0.7911(7) 0.075(3) Uani 1 1 d DU . .
C42 C 0.2833(14) 0.6785(8) 0.8304(9) 0.114(6) Uani 1 1 d DU . .
H42A H 0.2246 0.6893 0.8019 0.171 Uiso 1 1 calc R . .
H42B H 0.2930 0.7212 0.8493 0.171 Uiso 1 1 calc R . .
H42C H 0.2480 0.6478 0.8651 0.171 Uiso 1 1 calc R . .
C43 C 0.5102(18) 0.6255(10) 0.8359(8) 0.120(6) Uani 1 1 d DU . .
H43A H 0.5249 0.6686 0.8519 0.179 Uiso 1 1 calc R . .
H43B H 0.5923 0.5995 0.8113 0.179 Uiso 1 1 calc R . .
H43C H 0.4727 0.5977 0.8726 0.179 Uiso 1 1 calc R . .
C44 C 0.4768(16) 0.6895(7) 0.7359(7) 0.100(5) Uani 1 1 d DU . .
H44A H 0.4180 0.7030 0.7078 0.150 Uiso 1 1 calc R . .
H44B H 0.5588 0.6643 0.7104 0.150 Uiso 1 1 calc R . .
H44C H 0.4920 0.7310 0.7548 0.150 Uiso 1 1 calc R . .
C5 C 0.4531(13) 0.5488(7) 0.6985(7) 0.059(2) Uani 1 1 d U . .
H5A H 0.5034 0.5777 0.6701 0.071 Uiso 1 1 calc R . .
C6 C 0.4396(13) 0.4832(6) 0.6753(6) 0.0538(19) Uani 1 1 d U . .
C61 C 0.5095(14) 0.4603(7) 0.6054(6) 0.058(2) Uani 1 1 d U . .
H61A H 0.5478 0.4989 0.5817 0.070 Uiso 1 1 calc R . .
H61B H 0.4466 0.4482 0.5831 0.070 Uiso 1 1 calc R . .
N3 N 0.6175(11) 0.3967(5) 0.6048(5) 0.063(2) Uani 1 1 d DU . .
H3B H 0.5786 0.3634 0.6305 0.076 Uiso 1 1 calc R . .
C31 C 0.7217(15) 0.4126(9) 0.6356(8) 0.085(5) Uani 1 1 d DU . .
H31A H 0.6820 0.4303 0.6796 0.128 Uiso 1 1 calc R . .
H31B H 0.7666 0.4473 0.6097 0.128 Uiso 1 1 calc R . .
H31C H 0.7835 0.3703 0.6373 0.128 Uiso 1 1 calc R . .
C63 C 0.6702(16) 0.3652(7) 0.5353(7) 0.083(3) Uani 1 1 d DU . .
H63A H 0.5960 0.3547 0.5207 0.100 Uiso 1 1 calc R . .
H63B H 0.7058 0.4013 0.5063 0.100 Uiso 1 1 calc R . .
C64 C 0.7671(16) 0.3038(7) 0.5259(7) 0.100(3) Uani 1 1 d DU . .
H64A H 0.7488 0.2735 0.5641 0.120 Uiso 1 1 calc R . .
H64B H 0.8524 0.3170 0.5224 0.120 Uiso 1 1 calc R . .
C65 C 0.772(2) 0.2636(8) 0.4647(7) 0.108(3) Uani 1 1 d DU . .
H65A H 0.7470 0.2967 0.4320 0.130 Uiso 1 1 calc R . .
H65B H 0.8616 0.2404 0.4464 0.130 Uiso 1 1 calc R . .
O1A O 0.9588(8) 0.1186(4) 0.6882(4) 0.048(2) Uani 1 1 d U . .
C1A C 0.9320(14) 0.0590(7) 0.7151(7) 0.061(2) Uani 1 1 d U . .
C2A C 0.9292(14) 0.0410(7) 0.7788(7) 0.061(2) Uani 1 1 d U . .
C21A C 0.9527(13) 0.0873(7) 0.8272(7) 0.056(2) Uani 1 1 d U . .
H21B H 0.9579 0.0687 0.8683 0.067 Uiso 1 1 calc R . .
N2A N 0.9659(10) 0.1498(6) 0.8164(5) 0.054(2) Uani 1 1 d DU . .
O23A O 0.9866(9) 0.1856(5) 0.8679(4) 0.065(2) Uani 1 1 d DU . .
H23B H 1.0006 0.2251 0.8556 0.077 Uiso 1 1 calc R . .
C3A C 0.8968(14) -0.0256(7) 0.8061(8) 0.068(2) Uani 1 1 d U . .
H3AA H 0.8948 -0.0363 0.8501 0.081 Uiso 1 1 calc R . .
C4A C 0.8684(15) -0.0736(7) 0.7656(8) 0.074(2) Uani 1 1 d DU . .
C41A C 0.8486(14) -0.1495(7) 0.7922(7) 0.083(3) Uani 1 1 d DU . .
C42A C 0.946(2) -0.2023(11) 0.7467(11) 0.190(10) Uani 1 1 d DU . .
H42D H 1.0318 -0.1903 0.7394 0.285 Uiso 1 1 calc R . .
H42E H 0.9220 -0.2021 0.7053 0.285 Uiso 1 1 calc R . .
H42F H 0.9454 -0.2483 0.7660 0.285 Uiso 1 1 calc R . .
C43A C 0.7098(18) -0.1514(13) 0.7945(12) 0.179(9) Uani 1 1 d DU . .
H43D H 0.6538 -0.1224 0.8303 0.268 Uiso 1 1 calc R . .
H43E H 0.6940 -0.1991 0.8011 0.268 Uiso 1 1 calc R . .
H43F H 0.6912 -0.1340 0.7536 0.268 Uiso 1 1 calc R . .
C44A C 0.873(2) -0.1581(11) 0.8611(9) 0.147(7) Uani 1 1 d DU . .
H44D H 0.9660 -0.1703 0.8574 0.220 Uiso 1 1 calc R . .
H44E H 0.8296 -0.1949 0.8840 0.220 Uiso 1 1 calc R . .
H44F H 0.8394 -0.1147 0.8852 0.220 Uiso 1 1 calc R . .
C5A C 0.8685(14) -0.0561(7) 0.7014(8) 0.069(2) Uani 1 1 d U . .
H5AA H 0.8478 -0.0878 0.6749 0.083 Uiso 1 1 calc R . .
C6A C 0.8992(14) 0.0092(7) 0.6748(7) 0.064(2) Uani 1 1 d U . .
C61A C 0.8947(15) 0.0300(7) 0.6078(7) 0.069(2) Uani 1 1 d U . .
H61C H 0.8821 -0.0099 0.5845 0.083 Uiso 1 1 calc R . .
H61D H 0.9780 0.0434 0.5848 0.083 Uiso 1 1 calc R . .
N3A N 0.7877(12) 0.0893(6) 0.6070(6) 0.076(2) Uani 1 1 d DU . .
H3AB H 0.7956 0.1239 0.6334 0.091 Uiso 1 1 calc R . .
C31A C 0.6584(15) 0.0682(10) 0.6344(9) 0.101(5) Uani 1 1 d DU . .
H31D H 0.6538 0.0505 0.6784 0.152 Uiso 1 1 calc R . .
H31E H 0.6471 0.0320 0.6071 0.152 Uiso 1 1 calc R . .
H31F H 0.5902 0.1083 0.6356 0.152 Uiso 1 1 calc R . .
C63A C 0.7963(17) 0.1199(8) 0.5376(8) 0.091(3) Uani 1 1 d DU . .
H63C H 0.8769 0.1393 0.5230 0.109 Uiso 1 1 calc R . .
H63D H 0.8002 0.0823 0.5073 0.109 Uiso 1 1 calc R . .
C64A C 0.6843(17) 0.1752(8) 0.5349(8) 0.106(3) Uani 1 1 d DU . .
H64C H 0.6062 0.1534 0.5431 0.127 Uiso 1 1 calc R . .
H64D H 0.6718 0.2079 0.5709 0.127 Uiso 1 1 calc R . .
C65A C 0.6919(19) 0.2145(8) 0.4758(8) 0.114(3) Uani 1 1 d DU . .
H65C H 0.7209 0.1816 0.4390 0.137 Uiso 1 1 calc R . .
H65D H 0.6038 0.2381 0.4756 0.137 Uiso 1 1 calc R . .
O1B O 0.9695(9) 0.2853(5) 0.7769(4) 0.065(3) Uani 1 1 d U . .
C1B C 0.9778(13) 0.3502(7) 0.7501(8) 0.061(2) Uani 1 1 d U . .
C2B C 1.0214(12) 0.3605(6) 0.6831(7) 0.0555(19) Uani 1 1 d U . .
C21B C 1.0546(12) 0.3046(6) 0.6352(7) 0.055(2) Uani 1 1 d U . .
H21C H 1.0937 0.3152 0.5918 0.066 Uiso 1 1 calc R . .
N2B N 1.0348(10) 0.2422(5) 0.6475(5) 0.053(2) Uani 1 1 d DU . .
O23B O 1.0721(11) 0.1978(5) 0.5912(4) 0.074(3) Uani 1 1 d DU . .
H23C H 1.0610 0.1576 0.6026 0.089 Uiso 1 1 calc R . .
C3B C 1.0327(12) 0.4292(6) 0.6557(8) 0.062(2) Uani 1 1 d U . .
H3BA H 1.0644 0.4353 0.6105 0.075 Uiso 1 1 calc R . .
C4B C 0.9926(13) 0.4889(6) 0.7010(8) 0.067(2) Uani 1 1 d DU . .
C41B C 0.9983(12) 0.5638(6) 0.6732(7) 0.071(3) Uani 1 1 d DU . .
C42B C 1.0762(17) 0.6003(9) 0.7101(9) 0.114(6) Uani 1 1 d DU . .
H42G H 1.1645 0.5749 0.7025 0.170 Uiso 1 1 calc R . .
H42H H 1.0350 0.6012 0.7565 0.170 Uiso 1 1 calc R . .
H42I H 1.0780 0.6477 0.6943 0.170 Uiso 1 1 calc R . .
C43B C 1.0588(16) 0.5659(9) 0.5985(7) 0.109(5) Uani 1 1 d DU . .
H43G H 1.1479 0.5413 0.5887 0.164 Uiso 1 1 calc R . .
H43H H 1.0578 0.6141 0.5845 0.164 Uiso 1 1 calc R . .
H43I H 1.0086 0.5438 0.5757 0.164 Uiso 1 1 calc R . .
C44B C 0.8575(13) 0.6057(9) 0.6853(9) 0.098(5) Uani 1 1 d DU . .
H44G H 0.8604 0.6525 0.6682 0.147 Uiso 1 1 calc R . .
H44H H 0.8172 0.6080 0.7319 0.147 Uiso 1 1 calc R . .
H44I H 0.8070 0.5826 0.6634 0.147 Uiso 1 1 calc R . .
C5B C 0.9437(14) 0.4766(7) 0.7640(8) 0.067(2) Uani 1 1 d U . .
H5BA H 0.9156 0.5156 0.7921 0.080 Uiso 1 1 calc R . .
C6B C 0.9294(14) 0.4078(7) 0.7940(8) 0.070(2) Uani 1 1 d U . .
C61B C 0.8711(16) 0.3993(8) 0.8590(8) 0.080(2) Uani 1 1 d U . .
H61E H 0.8535 0.4443 0.8817 0.096 Uiso 1 1 calc R . .
H61F H 0.9305 0.3667 0.8788 0.096 Uiso 1 1 calc R . .
N3B N 0.7398(13) 0.3706(7) 0.8678(7) 0.094(3) Uani 1 1 d DU . .
H3BB H 0.7602 0.3347 0.8380 0.113 Uiso 1 1 calc R . .
C31B C 0.6408(17) 0.4235(10) 0.8441(9) 0.107(6) Uani 1 1 d DU . .
H31G H 0.5621 0.4042 0.8480 0.161 Uiso 1 1 calc R . .
H31H H 0.6762 0.4347 0.7987 0.161 Uiso 1 1 calc R . .
H31I H 0.6206 0.4656 0.8705 0.161 Uiso 1 1 calc R . .
C63B C 0.6935(17) 0.3360(10) 0.9339(9) 0.105(3) Uani 1 1 d DU . .
H63E H 0.7640 0.2995 0.9408 0.126 Uiso 1 1 calc R . .
H63F H 0.6760 0.3710 0.9685 0.126 Uiso 1 1 calc R . .
C64B C 0.5750(17) 0.3045(10) 0.9403(8) 0.115(3) Uani 1 1 d DU . .
H64E H 0.5862 0.2742 0.9026 0.137 Uiso 1 1 calc R . .
H64F H 0.4998 0.3413 0.9415 0.137 Uiso 1 1 calc R . .
C65B C 0.5516(17) 0.2620(10) 1.0029(8) 0.120(3) Uani 1 1 d DU . .
H65E H 0.6093 0.2167 0.9961 0.144 Uiso 1 1 calc R . .
H65F H 0.5706 0.2866 1.0380 0.144 Uiso 1 1 calc R . .
O1C O 0.2854(9) 0.2137(4) 0.7899(5) 0.062(2) Uani 1 1 d U . .
C1C C 0.2913(14) 0.1492(8) 0.7716(8) 0.070(2) Uani 1 1 d U . .
C2C C 0.3033(13) 0.1316(7) 0.7052(8) 0.066(2) Uani 1 1 d U . .
C21C C 0.3247(12) 0.1801(7) 0.6517(8) 0.063(2) Uani 1 1 d U . .
H21D H 0.3326 0.1635 0.6095 0.076 Uiso 1 1 calc R . .
N2C N 0.3339(10) 0.2453(5) 0.6575(6) 0.057(2) Uani 1 1 d DU . .
O23C O 0.3598(11) 0.2791(5) 0.5995(5) 0.080(3) Uani 1 1 d DU . .
H23D H 0.3629 0.3204 0.6060 0.096 Uiso 1 1 calc R . .
C3C C 0.3132(13) 0.0580(7) 0.6918(9) 0.074(2) Uani 1 1 d U . .
H3CA H 0.3269 0.0434 0.6483 0.088 Uiso 1 1 calc R . .
C4C C 0.3028(14) 0.0075(7) 0.7425(9) 0.079(2) Uani 1 1 d DU . .
C41C C 0.3151(13) -0.0724(7) 0.7230(8) 0.087(3) Uani 1 1 d DU . .
C42C C 0.2391(17) -0.0804(9) 0.6742(8) 0.113(6) Uani 1 1 d DU . .
H42J H 0.2778 -0.1227 0.6489 0.170 Uiso 1 1 calc R . .
H42K H 0.2405 -0.0405 0.6451 0.170 Uiso 1 1 calc R . .
H42L H 0.1499 -0.0831 0.6968 0.170 Uiso 1 1 calc R . .
C43C C 0.2636(19) -0.1144(9) 0.7846(8) 0.127(6) Uani 1 1 d DU . .
H43J H 0.2801 -0.1637 0.7736 0.191 Uiso 1 1 calc R . .
H43K H 0.1708 -0.0989 0.8010 0.191 Uiso 1 1 calc R . .
H43L H 0.3078 -0.1072 0.8179 0.191 Uiso 1 1 calc R . .
C44C C 0.4635(13) -0.0996(9) 0.6954(9) 0.112(6) Uani 1 1 d DU . .
H44J H 0.4752 -0.1384 0.6658 0.168 Uiso 1 1 calc R . .
H44K H 0.5028 -0.1151 0.7312 0.168 Uiso 1 1 calc R . .
H44L H 0.5048 -0.0623 0.6721 0.168 Uiso 1 1 calc R . .
C5C C 0.2929(14) 0.0267(8) 0.8040(9) 0.080(2) Uani 1 1 d U . .
H5CA H 0.2903 -0.0069 0.8372 0.096 Uiso 1 1 calc R . .
C6C C 0.2868(15) 0.0942(8) 0.8183(9) 0.081(2) Uani 1 1 d U . .
C61C C 0.2961(16) 0.1131(9) 0.8882(9) 0.091(3) Uani 1 1 d U . .
H61G H 0.2336 0.1553 0.9043 0.110 Uiso 1 1 calc R . .
H61H H 0.2751 0.0749 0.9185 0.110 Uiso 1 1 calc R . .
N3C N 0.4338(14) 0.1250(7) 0.8844(7) 0.100(3) Uani 1 1 d DU . .
H3CB H 0.4505 0.1598 0.8543 0.120 Uiso 1 1 calc R . .
C31C C 0.5373(16) 0.0630(9) 0.8619(10) 0.103(5) Uani 1 1 d DU . .
H31J H 0.5315 0.0472 0.8199 0.154 Uiso 1 1 calc R . .
H31K H 0.5255 0.0258 0.8936 0.154 Uiso 1 1 calc R . .
H31L H 0.6222 0.0758 0.8575 0.154 Uiso 1 1 calc R . .
C63C C 0.440(2) 0.1519(9) 0.9494(9) 0.112(3) Uani 1 1 d DU . .
H63G H 0.4092 0.1181 0.9828 0.134 Uiso 1 1 calc R . .
H63H H 0.5318 0.1514 0.9478 0.134 Uiso 1 1 calc R . .
C64C C 0.3693(17) 0.2204(9) 0.9722(9) 0.119(3) Uani 1 1 d DU . .
H64G H 0.2776 0.2167 0.9909 0.143 Uiso 1 1 calc R . .
H64H H 0.3730 0.2516 0.9344 0.143 Uiso 1 1 calc R . .
C65C C 0.4174(17) 0.2520(10) 1.0210(8) 0.122(3) Uani 1 1 d DU . .
H65G H 0.3625 0.2976 1.0331 0.147 Uiso 1 1 calc R . .
H65H H 0.4052 0.2228 1.0603 0.147 Uiso 1 1 calc R . .
B1 B 0.2775(14) 0.3986(7) 0.4797(7) 0.067(4) Uani 1 1 d DU . .
F11 F 0.2325(12) 0.4628(5) 0.4588(6) 0.141(4) Uani 1 1 d DU . .
F12 F 0.3823(12) 0.3674(6) 0.4348(6) 0.146(5) Uani 1 1 d DU . .
F13 F 0.3051(9) 0.4032(6) 0.5386(5) 0.110(3) Uani 1 1 d DU . .
F14 F 0.1775(10) 0.3592(5) 0.4874(5) 0.113(3) Uani 1 1 d DU . .
B2 B 0.6352(13) 0.2384(7) 0.7472(6) 0.027(2) Uani 0.711(17) 1 d PDU A 1
F21 F 0.7364(10) 0.2537(8) 0.7698(6) 0.107(6) Uani 0.711(17) 1 d PDU A 1
F24 F 0.6207(18) 0.1708(7) 0.7611(11) 0.143(8) Uani 0.711(17) 1 d PDU A 1
F23 F 0.5224(12) 0.2814(7) 0.7761(7) 0.109(6) Uani 0.711(17) 1 d PDU A 1
F22 F 0.662(2) 0.2428(11) 0.6808(5) 0.133(6) Uani 0.711(17) 1 d PDU A 1
B2A B 0.650(3) 0.2472(15) 0.7323(12) 0.027(2) Uani 0.289(17) 1 d PDU A 2
F21A F 0.766(3) 0.2255(14) 0.6878(13) 0.085(11) Uani 0.289(17) 1 d PDU A 2
F22A F 0.554(3) 0.259(2) 0.6994(19) 0.16(2) Uani 0.289(17) 1 d PDU A 2
F23A F 0.652(4) 0.3088(15) 0.7612(17) 0.141(18) Uani 0.289(17) 1 d PDU A 2
F24A F 0.629(4) 0.1961(17) 0.7777(14) 0.099(14) Uani 0.289(17) 1 d PDU A 2
B3 B 0.7271(19) 0.0360(10) 0.9952(9) 0.116(8) Uani 1 1 d DU . .
F32 F 0.7444(14) 0.0887(7) 0.9507(7) 0.171(6) Uani 1 1 d DU . .
F31 F 0.6557(17) 0.0621(8) 1.0554(7) 0.197(7) Uani 1 1 d DU . .
F34 F 0.666(2) -0.0107(10) 0.9758(10) 0.273(11) Uani 1 1 d DU . .
F33 F 0.8468(19) 0.0031(13) 1.0002(13) 0.348(14) Uani 1 1 d DU . .
B4 B 0.322(3) 0.4691(15) 0.9965(14) 0.121(3) Uani 0.25 1 d PDU B 1
F41 F 0.443(3) 0.479(2) 1.000(2) 0.122(4) Uani 0.25 1 d PDU . 1
F42 F 0.333(5) 0.4185(18) 0.9509(19) 0.099(7) Uani 0.25 1 d PDU B 1
F43 F 0.253(3) 0.5295(14) 0.9784(15) 0.068(10) Uani 0.25 1 d PDU B 1
F44 F 0.257(3) 0.448(2) 1.0565(14) 0.096(9) Uani 0.25 1 d PDU B 1
B4A B 0.326(3) 0.4705(15) 0.9921(13) 0.121(3) Uani 0.25 1 d PDU C 2
F44A F 0.311(4) 0.459(2) 1.0565(12) 0.096(9) Uani 0.25 1 d PDU C 2
F41A F 0.413(4) 0.513(2) 0.9694(19) 0.140(17) Uani 0.25 1 d PDU C 2
F42A F 0.347(5) 0.4132(18) 0.957(2) 0.099(7) Uani 0.25 1 d PDU C 2
F43A F 0.201(3) 0.509(2) 0.9841(19) 0.087(13) Uani 0.25 1 d PDU C 2
B5 B 0.406(3) 0.0154(14) 0.5087(13) 0.184(7) Uani 0.50 1 d PDU . .
F51 F 0.275(2) 0.0306(17) 0.5254(17) 0.243(16) Uani 0.50 1 d PDU . .
F52 F 0.458(3) 0.0653(13) 0.5327(13) 0.180(7) Uani 0.50 1 d PDU . .
F53 F 0.444(3) -0.0476(12) 0.5328(14) 0.188(7) Uani 0.50 1 d PDU . .
F54 F 0.456(3) 0.0157(16) 0.4419(10) 0.184(7) Uani 0.50 1 d PDU . .
N100 N 0.867(3) 0.8687(18) 0.5579(17) 0.240(13) Uani 1 1 d DU . .
C100 C 0.772(3) 0.8436(19) 0.5555(17) 0.189(12) Uani 1 1 d DU . .
C101 C 0.680(2) 0.7995(13) 0.5470(12) 0.146(8) Uani 1 1 d DU . .
H10A H 0.6933 0.7560 0.5703 0.219 Uiso 1 1 calc R . .
H10B H 0.6930 0.7899 0.5009 0.219 Uiso 1 1 calc R . .
H10C H 0.5913 0.8237 0.5643 0.219 Uiso 1 1 calc R . .
N200 N 1.013(3) 0.2497(18) 0.0025(11) 0.195(9) Uani 1 1 d DU . .
C200 C 0.972(3) 0.1932(18) 0.0192(16) 0.182(11) Uani 1 1 d DU . .
C201 C 0.907(4) 0.1295(19) 0.0323(16) 0.212(13) Uani 1 1 d DU . .
H20A H 0.9625 0.0925 0.0494 0.318 Uiso 1 1 calc R . .
H20B H 0.8935 0.1140 -0.0082 0.318 Uiso 1 1 calc R . .
H20C H 0.8241 0.1410 0.0639 0.318 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu2 0.0466(9) 0.0406(8) 0.0582(10) -0.0066(8) -0.0141(8) 0.0002(6)
Cu1 0.0476(9) 0.0410(8) 0.0680(11) 0.0015(8) -0.0203(8) 0.0007(7)
O1 0.053(5) 0.044(5) 0.067(5) 0.007(4) -0.027(4) -0.006(4)
C1 0.058(4) 0.036(4) 0.059(4) -0.002(3) -0.026(3) -0.001(3)
C2 0.063(4) 0.042(3) 0.060(4) 0.002(3) -0.024(3) 0.002(3)
C21 0.062(4) 0.052(4) 0.058(4) 0.003(4) -0.019(4) 0.000(4)
N2 0.063(5) 0.054(4) 0.060(5) 0.011(4) -0.014(4) -0.002(4)
O23 0.075(7) 0.074(6) 0.066(6) 0.012(5) -0.003(5) -0.007(5)
C3 0.071(4) 0.047(4) 0.068(4) -0.003(4) -0.022(4) 0.002(4)
C4 0.075(4) 0.045(4) 0.075(4) -0.004(3) -0.021(4) -0.003(3)
C41 0.086(6) 0.050(5) 0.085(5) -0.009(5) -0.017(5) -0.002(5)
C42 0.114(10) 0.063(9) 0.147(13) -0.048(9) 0.011(9) -0.018(8)
C43 0.148(13) 0.100(12) 0.121(12) -0.033(9) -0.055(10) -0.012(10)
C44 0.120(11) 0.063(8) 0.122(11) -0.012(8) -0.026(9) -0.027(8)
C5 0.069(4) 0.040(4) 0.070(4) 0.001(3) -0.025(4) -0.005(4)
C6 0.063(4) 0.039(3) 0.063(4) 0.003(3) -0.027(3) -0.004(3)
C61 0.072(4) 0.044(4) 0.062(4) 0.007(4) -0.029(4) -0.006(4)
N3 0.082(4) 0.049(4) 0.059(4) 0.009(3) -0.022(4) -0.007(4)
C31 0.071(9) 0.085(10) 0.102(11) -0.008(8) -0.040(8) 0.013(7)
C63 0.104(5) 0.066(4) 0.068(4) 0.010(4) -0.010(4) -0.006(4)
C64 0.121(5) 0.085(5) 0.080(5) 0.001(4) -0.006(5) -0.011(4)
C65 0.132(6) 0.096(5) 0.086(5) -0.008(5) -0.006(5) -0.020(5)
O1A 0.057(5) 0.041(4) 0.040(5) -0.001(4) 0.001(4) -0.009(4)
C1A 0.065(4) 0.051(4) 0.065(4) -0.003(4) -0.014(4) -0.004(4)
C2A 0.064(4) 0.051(4) 0.062(4) -0.004(3) -0.011(3) -0.002(3)
C21A 0.059(4) 0.053(4) 0.052(4) -0.005(4) -0.009(4) -0.003(4)
N2A 0.057(5) 0.053(4) 0.049(5) -0.013(4) -0.010(4) 0.000(4)
O23A 0.075(6) 0.065(6) 0.051(5) -0.002(4) -0.013(4) -0.009(5)
C3A 0.070(4) 0.055(4) 0.073(4) 0.001(4) -0.012(4) -0.004(4)
C4A 0.075(4) 0.057(4) 0.084(4) 0.001(4) -0.011(4) -0.009(4)
C41A 0.086(6) 0.059(5) 0.095(6) 0.007(5) -0.011(5) -0.010(5)
C42A 0.216(16) 0.101(11) 0.218(16) -0.018(13) 0.007(14) -0.016(12)
C43A 0.155(12) 0.167(16) 0.238(19) 0.082(15) -0.068(12) -0.080(12)
C44A 0.196(17) 0.103(13) 0.163(12) 0.050(10) -0.076(12) -0.048(12)
C5A 0.072(4) 0.053(4) 0.078(4) -0.004(4) -0.010(4) -0.010(4)
C6A 0.070(4) 0.050(4) 0.071(4) -0.008(3) -0.014(4) -0.010(3)
C61A 0.079(4) 0.053(4) 0.073(4) -0.012(4) -0.014(4) -0.014(4)
N3A 0.092(5) 0.061(4) 0.076(4) -0.015(4) -0.019(4) -0.014(4)
C31A 0.067(9) 0.124(13) 0.118(12) 0.007(10) -0.031(8) -0.021(9)
C63A 0.112(5) 0.077(5) 0.082(5) -0.015(4) -0.021(5) -0.011(4)
C64A 0.128(6) 0.094(5) 0.091(5) -0.012(5) -0.019(5) -0.011(5)
C65A 0.136(6) 0.102(5) 0.095(5) -0.010(5) -0.013(5) -0.014(5)
O1B 0.077(6) 0.056(5) 0.062(6) -0.011(4) -0.031(5) 0.013(5)
C1B 0.057(4) 0.047(4) 0.083(4) -0.015(4) -0.026(4) -0.001(3)
C2B 0.050(4) 0.041(3) 0.081(4) -0.014(3) -0.027(3) -0.003(3)
C21B 0.053(4) 0.042(4) 0.075(4) -0.013(4) -0.023(4) -0.008(4)
N2B 0.055(5) 0.039(4) 0.072(5) -0.017(4) -0.022(4) -0.015(4)
O23B 0.109(8) 0.064(6) 0.052(5) -0.015(5) -0.006(5) -0.041(5)
C3B 0.051(4) 0.047(4) 0.089(4) -0.009(4) -0.023(4) 0.002(4)
C4B 0.055(4) 0.047(3) 0.095(4) -0.011(4) -0.020(4) 0.003(3)
C41B 0.057(5) 0.049(5) 0.103(6) -0.006(5) -0.017(5) 0.004(4)
C42B 0.117(12) 0.062(9) 0.177(14) 0.017(10) -0.053(11) -0.035(9)
C43B 0.093(11) 0.079(10) 0.137(10) 0.015(9) -0.001(9) -0.010(8)
C44B 0.091(9) 0.076(10) 0.123(12) 0.011(9) -0.035(9) 0.005(8)
C5B 0.060(4) 0.049(4) 0.091(4) -0.020(4) -0.024(4) 0.005(4)
C6B 0.067(4) 0.055(4) 0.088(4) -0.019(4) -0.024(4) 0.000(3)
C61B 0.081(5) 0.068(4) 0.091(5) -0.021(4) -0.025(4) -0.004(4)
N3B 0.098(5) 0.087(5) 0.096(5) -0.017(4) -0.023(4) -0.008(4)
C31B 0.079(10) 0.136(13) 0.104(11) -0.009(10) -0.019(9) -0.016(9)
C63B 0.110(5) 0.101(5) 0.100(5) -0.014(5) -0.021(5) -0.013(5)
C64B 0.120(6) 0.110(5) 0.106(5) -0.004(5) -0.019(5) -0.012(5)
C65B 0.125(6) 0.118(6) 0.108(5) 0.004(5) -0.021(5) -0.010(5)
O1C 0.063(6) 0.037(4) 0.079(6) 0.019(4) -0.007(5) -0.003(4)
C1C 0.051(4) 0.058(4) 0.100(5) 0.014(4) -0.021(4) -0.006(4)
C2C 0.046(4) 0.053(4) 0.099(4) 0.005(4) -0.018(4) -0.008(3)
C21C 0.047(4) 0.054(4) 0.091(5) -0.004(4) -0.019(4) -0.008(4)
N2C 0.043(5) 0.046(4) 0.087(5) -0.006(4) -0.021(4) -0.012(4)
O23C 0.118(8) 0.064(6) 0.078(7) 0.000(5) -0.043(6) -0.040(6)
C3C 0.051(4) 0.058(4) 0.108(5) 0.007(4) -0.014(4) -0.008(4)
C4C 0.058(4) 0.058(4) 0.115(5) 0.010(4) -0.014(4) -0.006(4)
C41C 0.066(5) 0.063(5) 0.123(6) 0.006(5) -0.010(5) -0.005(5)
C42C 0.121(12) 0.079(10) 0.138(12) -0.028(9) -0.021(10) -0.021(9)
C43C 0.152(14) 0.066(9) 0.155(12) 0.007(9) -0.013(11) -0.034(10)
C44C 0.095(9) 0.063(9) 0.164(14) -0.003(10) -0.019(9) 0.006(8)
C5C 0.060(4) 0.063(4) 0.112(5) 0.018(4) -0.015(4) -0.008(4)
C6C 0.063(4) 0.066(4) 0.109(4) 0.019(4) -0.016(4) -0.009(4)
C61C 0.080(4) 0.080(5) 0.109(5) 0.022(4) -0.020(4) -0.010(4)
N3C 0.091(5) 0.095(5) 0.111(5) 0.021(4) -0.026(5) -0.012(4)
C31C 0.077(9) 0.107(11) 0.126(12) 0.001(9) -0.032(9) -0.012(8)
C63C 0.108(5) 0.108(5) 0.115(5) 0.018(5) -0.024(5) -0.012(5)
C64C 0.118(5) 0.114(5) 0.117(6) 0.015(5) -0.024(5) -0.011(5)
C65C 0.126(6) 0.119(6) 0.113(6) 0.010(5) -0.022(5) -0.009(5)
B1 0.095(12) 0.059(9) 0.051(9) 0.021(8) -0.018(9) -0.031(9)
F11 0.186(11) 0.104(8) 0.172(10) 0.059(7) -0.091(8) -0.068(7)
F12 0.191(11) 0.120(8) 0.122(9) 0.001(7) -0.002(8) -0.064(8)
F13 0.090(7) 0.146(8) 0.113(7) -0.013(6) -0.059(6) -0.021(6)
F14 0.153(9) 0.104(7) 0.112(7) 0.043(6) -0.061(6) -0.073(7)
B2 0.027(3) 0.026(3) 0.026(4) 0.009(3) -0.006(3) -0.001(3)
F21 0.047(7) 0.143(11) 0.132(10) -0.063(8) -0.049(6) 0.033(7)
F24 0.129(12) 0.087(11) 0.229(18) 0.009(11) -0.059(12) -0.037(9)
F23 0.096(7) 0.122(7) 0.114(7) -0.012(4) -0.042(4) -0.009(4)
F22 0.153(14) 0.181(13) 0.076(8) -0.028(10) -0.033(10) -0.045(11)
B2A 0.027(3) 0.026(3) 0.026(4) 0.009(3) -0.006(3) -0.001(3)
F21A 0.075(17) 0.069(15) 0.109(18) -0.031(13) -0.037(13) 0.019(12)
F22A 0.15(3) 0.17(3) 0.15(3) 0.021(18) -0.037(18) -0.010(18)
F23A 0.14(2) 0.13(2) 0.15(2) 0.001(17) -0.032(17) -0.030(17)
F24A 0.13(2) 0.072(18) 0.080(18) -0.012(15) -0.020(15) 0.014(15)
B3 0.102(14) 0.110(14) 0.112(15) 0.044(13) -0.009(12) 0.014(11)
F32 0.155(10) 0.154(10) 0.158(10) 0.054(9) 0.018(8) 0.000(8)
F31 0.204(13) 0.180(12) 0.164(12) 0.051(10) 0.008(10) -0.007(10)
F34 0.335(19) 0.227(17) 0.262(17) 0.047(14) -0.084(15) -0.062(15)
F33 0.33(2) 0.31(2) 0.35(2) 0.117(17) -0.050(16) 0.008(16)
B4 0.124(5) 0.125(5) 0.112(5) -0.022(5) -0.026(5) -0.016(5)
F41 0.125(6) 0.126(6) 0.112(6) -0.023(6) -0.026(6) -0.016(6)
F42 0.110(12) 0.093(11) 0.092(11) -0.038(9) -0.042(9) 0.027(9)
F43 0.096(19) 0.051(15) 0.044(15) -0.002(12) 0.008(13) -0.016(14)
F44 0.113(16) 0.098(12) 0.082(11) -0.019(9) -0.049(11) 0.007(11)
B4A 0.124(5) 0.125(5) 0.112(5) -0.022(5) -0.026(5) -0.016(5)
F44A 0.113(16) 0.098(12) 0.082(11) -0.019(9) -0.049(11) 0.007(11)
F41A 0.16(2) 0.11(2) 0.13(2) -0.006(17) -0.033(17) 0.007(17)
F42A 0.110(12) 0.093(11) 0.092(11) -0.038(9) -0.042(9) 0.027(9)
F43A 0.078(19) 0.09(2) 0.087(19) -0.016(15) -0.024(15) 0.012(15)
B5 0.198(11) 0.181(11) 0.177(10) -0.022(9) -0.051(8) -0.035(8)
F51 0.28(2) 0.22(2) 0.25(2) -0.031(17) -0.054(17) -0.117(18)
F52 0.197(11) 0.179(11) 0.173(11) -0.024(9) -0.053(9) -0.037(9)
F53 0.199(11) 0.184(11) 0.184(11) -0.019(9) -0.048(9) -0.035(9)
F54 0.200(11) 0.182(11) 0.175(11) -0.024(9) -0.054(9) -0.033(9)
N100 0.25(2) 0.23(2) 0.25(2) -0.085(16) -0.063(16) -0.073(16)
C100 0.173(18) 0.192(19) 0.186(19) -0.063(16) -0.007(15) -0.027(14)
C101 0.159(15) 0.130(14) 0.135(14) -0.027(12) -0.009(12) -0.017(11)
N200 0.208(17) 0.221(16) 0.154(14) 0.021(15) -0.041(14) -0.044(14)
C200 0.198(19) 0.172(17) 0.166(18) -0.003(15) -0.044(15) -0.005(14)
C201 0.21(2) 0.225(19) 0.20(2) 0.034(17) -0.050(16) -0.048(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu2 O1B 1.890(9) . ?
Cu2 O1A 1.919(8) . ?
Cu2 N2B 1.930(11) . ?
Cu2 N2A 1.961(11) . ?
Cu1 O1 1.877(9) . ?
Cu1 O1C 1.892(8) . ?
Cu1 N2 1.939(11) . ?
Cu1 N2C 1.960(11) . ?
O1 C1 1.339(14) . ?
C1 C6 1.371(18) . ?
C1 C2 1.430(18) . ?
C2 C21 1.408(18) . ?
C2 C3 1.465(18) . ?
C21 N2 1.314(16) . ?
N2 O23 1.378(12) . ?
C3 C4 1.312(19) . ?
C4 C5 1.398(18) . ?
C4 C41 1.596(15) . ?
C41 C42 1.507(14) . ?
C41 C44 1.526(14) . ?
C41 C43 1.527(15) . ?
C5 C6 1.414(17) . ?
C6 C61 1.508(18) . ?
C61 N3 1.526(16) . ?
N3 C31 1.495(15) . ?
N3 C63 1.528(17) . ?
C63 C64 1.412(15) . ?
C64 C65 1.509(15) . ?
C65 C65A 1.356(16) . ?
O1A C1A 1.302(15) . ?
C1A C2A 1.356(18) . ?
C1A C6A 1.444(19) . ?
C2A C3A 1.444(19) . ?
C2A C21A 1.469(18) . ?
C21A N2A 1.242(16) . ?
N2A O23A 1.385(11) . ?
C3A C4A 1.40(2) . ?
C4A C5A 1.37(2) . ?
C4A C41A 1.574(16) . ?
C41A C43A 1.474(16) . ?
C41A C42A 1.491(16) . ?
C41A C44A 1.525(16) . ?
C5A C6A 1.411(19) . ?
C6A C61A 1.453(19) . ?
C61A N3A 1.470(17) . ?
N3A C31A 1.474(15) . ?
N3A C63A 1.532(18) . ?
C63A C64A 1.465(15) . ?
C64A C65A 1.416(15) . ?
O1B C1B 1.356(16) . ?
C1B C2B 1.379(19) . ?
C1B C6B 1.409(18) . ?
C2B C3B 1.432(18) . ?
C2B C21B 1.436(17) . ?
C21B N2B 1.260(15) . ?
N2B O23B 1.415(11) . ?
C3B C4B 1.455(18) . ?
C4B C5B 1.318(18) . ?
C4B C41B 1.539(15) . ?
C41B C42B 1.532(15) . ?
C41B C43B 1.534(15) . ?
C41B C44B 1.539(14) . ?
C5B C6B 1.46(2) . ?
C6B C61B 1.36(2) . ?
C61B N3B 1.56(2) . ?
N3B C31B 1.497(16) . ?
N3B C63B 1.517(19) . ?
C63B C64B 1.468(15) . ?
C64B C65B 1.504(16) . ?
C65B C65C 1.430(15) . ?
O1C C1C 1.301(17) . ?
C1C C6C 1.41(2) . ?
C1C C2C 1.41(2) . ?
C2C C21C 1.429(19) . ?
C2C C3C 1.436(19) . ?
C21C N2C 1.288(16) . ?
N2C O23C 1.344(12) . ?
C3C C4C 1.41(2) . ?
C4C C5C 1.33(2) . ?
C4C C41C 1.583(16) . ?
C41C C42C 1.481(15) . ?
C41C C43C 1.526(15) . ?
C41C C44C 1.545(15) . ?
C5C C6C 1.33(2) . ?
C6C C61C 1.55(2) . ?
C61C N3C 1.51(2) . ?
N3C C31C 1.479(16) . ?
N3C C63C 1.49(2) . ?
C63C C64C 1.434(16) . ?
C64C C65C 1.449(16) . ?
B1 F12 1.332(14) . ?
B1 F13 1.345(13) . ?
B1 F11 1.344(13) . ?
B1 F14 1.388(14) . ?
B2 F23 1.350(14) . ?
B2 F22 1.347(14) . ?
B2 F24 1.350(14) . ?
B2 F21 1.361(14) . ?
B2A F24A 1.347(18) . ?
B2A F22A 1.356(18) . ?
B2A F21A 1.357(18) . ?
B2A F23A 1.358(18) . ?
B3 F34 1.326(17) . ?
B3 F33 1.349(16) . ?
B3 F32 1.354(15) . ?
B3 F31 1.361(16) . ?
B4 F44 1.358(19) . ?
B4 F41 1.355(19) . ?
B4 F43 1.356(19) . ?
B4 F42 1.360(19) . ?
F41 F41 1.57(6) 2_667 ?
B4A F42A 1.30(4) . ?
B4A F41A 1.33(5) . ?
B4A F44A 1.33(2) . ?
B4A F43A 1.45(4) . ?
B5 F53 1.331(18) . ?
B5 F51 1.338(18) . ?
B5 F52 1.358(19) . ?
B5 F54 1.365(18) . ?
B5 F53 1.82(4) 2_656 ?
B5 B5 1.93(6) 2_656 ?
F52 F53 1.51(4) 2_656 ?
F53 F52 1.51(4) 2_656 ?
F53 F54 1.53(4) 2_656 ?
F53 B5 1.82(4) 2_656 ?
F54 F53 1.53(4) 2_656 ?
N100 C100 1.20(3) . ?
C100 C101 1.46(3) . ?
N200 C200 1.25(3) . ?
C200 C201 1.49(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Cu2 O1A 173.8(4) . . ?
O1B Cu2 N2B 91.8(4) . . ?
O1A Cu2 N2B 88.5(4) . . ?
O1B Cu2 N2A 89.4(4) . . ?
O1A Cu2 N2A 92.0(4) . . ?
N2B Cu2 N2A 163.7(4) . . ?
O1 Cu1 O1C 171.1(4) . . ?
O1 Cu1 N2 92.6(4) . . ?
O1C Cu1 N2 88.0(4) . . ?
O1 Cu1 N2C 90.7(4) . . ?
O1C Cu1 N2C 91.1(4) . . ?
N2 Cu1 N2C 164.7(4) . . ?
C1 O1 Cu1 128.0(8) . . ?
O1 C1 C6 119.1(11) . . ?
O1 C1 C2 121.8(12) . . ?
C6 C1 C2 118.9(12) . . ?
C21 C2 C1 126.8(12) . . ?
C21 C2 C3 117.3(12) . . ?
C1 C2 C3 115.8(12) . . ?
N2 C21 C2 120.6(13) . . ?
C21 N2 O23 110.3(11) . . ?
C21 N2 Cu1 129.1(9) . . ?
O23 N2 Cu1 120.4(8) . . ?
C4 C3 C2 125.1(13) . . ?
C3 C4 C5 117.6(12) . . ?
C3 C4 C41 121.0(12) . . ?
C5 C4 C41 120.8(13) . . ?
C42 C41 C44 111.4(11) . . ?
C42 C41 C43 109.8(11) . . ?
C44 C41 C43 107.1(11) . . ?
C42 C41 C4 106.3(11) . . ?
C44 C41 C4 112.3(11) . . ?
C43 C41 C4 109.9(11) . . ?
C4 C5 C6 120.9(13) . . ?
C1 C6 C5 121.6(13) . . ?
C1 C6 C61 118.9(11) . . ?
C5 C6 C61 119.5(12) . . ?
C6 C61 N3 110.8(10) . . ?
C31 N3 C61 112.4(10) . . ?
C31 N3 C63 114.1(12) . . ?
C61 N3 C63 110.5(10) . . ?
C64 C63 N3 118.4(12) . . ?
C63 C64 C65 112.1(13) . . ?
C65A C65 C64 113.5(12) . . ?
C1A O1A Cu2 126.9(8) . . ?
O1A C1A C2A 124.9(13) . . ?
O1A C1A C6A 117.7(12) . . ?
C2A C1A C6A 117.4(13) . . ?
C1A C2A C3A 122.4(14) . . ?
C1A C2A C21A 124.1(13) . . ?
C3A C2A C21A 113.4(12) . . ?
N2A C21A C2A 123.9(13) . . ?
C21A N2A O23A 115.9(11) . . ?
C21A N2A Cu2 127.2(9) . . ?
O23A N2A Cu2 116.7(8) . . ?
C4A C3A C2A 119.1(13) . . ?
C5A C4A C3A 119.6(13) . . ?
C5A C4A C41A 120.5(14) . . ?
C3A C4A C41A 119.7(13) . . ?
C43A C41A C42A 114.6(14) . . ?
C43A C41A C44A 111.0(13) . . ?
C42A C41A C44A 109.2(13) . . ?
C43A C41A C4A 103.9(13) . . ?
C42A C41A C4A 108.4(14) . . ?
C44A C41A C4A 109.4(13) . . ?
C4A C5A C6A 121.3(14) . . ?
C5A C6A C1A 120.2(14) . . ?
C5A C6A C61A 122.2(13) . . ?
C1A C6A C61A 117.5(13) . . ?
C6A C61A N3A 111.6(12) . . ?
C31A N3A C61A 110.8(12) . . ?
C31A N3A C63A 110.6(12) . . ?
C61A N3A C63A 112.0(11) . . ?
C64A C63A N3A 112.6(12) . . ?
C65A C64A C63A 117.3(13) . . ?
C65 C65A C64A 117.1(14) . . ?
C1B O1B Cu2 127.6(8) . . ?
O1B C1B C2B 122.6(11) . . ?
O1B C1B C6B 116.3(13) . . ?
C2B C1B C6B 120.9(13) . . ?
C1B C2B C3B 122.0(12) . . ?
C1B C2B C21B 123.3(12) . . ?
C3B C2B C21B 114.6(13) . . ?
N2B C21B C2B 125.1(13) . . ?
C21B N2B O23B 114.1(11) . . ?
C21B N2B Cu2 127.7(9) . . ?
O23B N2B Cu2 118.0(7) . . ?
C2B C3B C4B 117.6(13) . . ?
C5B C4B C3B 117.9(13) . . ?
C5B C4B C41B 122.7(13) . . ?
C3B C4B C41B 119.2(13) . . ?
C42B C41B C43B 109.8(11) . . ?
C42B C41B C44B 108.8(11) . . ?
C43B C41B C44B 106.5(10) . . ?
C42B C41B C4B 108.6(11) . . ?
C43B C41B C4B 114.0(12) . . ?
C44B C41B C4B 109.1(11) . . ?
C4B C5B C6B 126.3(13) . . ?
C61B C6B C1B 121.9(14) . . ?
C61B C6B C5B 123.1(13) . . ?
C1B C6B C5B 114.9(14) . . ?
C6B C61B N3B 111.3(13) . . ?
C31B N3B C63B 117.4(13) . . ?
C31B N3B C61B 110.6(13) . . ?
C63B N3B C61B 114.5(13) . . ?
C64B C63B N3B 114.4(13) . . ?
C63B C64B C65B 109.4(13) . . ?
C65C C65B C64B 109.2(13) . . ?
C1C O1C Cu1 131.1(10) . . ?
O1C C1C C6C 120.3(15) . . ?
O1C C1C C2C 121.8(13) . . ?
C6C C1C C2C 117.8(14) . . ?
C1C C2C C21C 123.8(13) . . ?
C1C C2C C3C 115.9(14) . . ?
C21C C2C C3C 119.7(14) . . ?
N2C C21C C2C 124.9(14) . . ?
C21C N2C O23C 113.5(11) . . ?
C21C N2C Cu1 126.8(11) . . ?
O23C N2C Cu1 119.8(8) . . ?
C4C C3C C2C 121.8(15) . . ?
C5C C4C C3C 119.8(14) . . ?
C5C C4C C41C 121.7(14) . . ?
C3C C4C C41C 118.3(15) . . ?
C42C C41C C43C 108.5(12) . . ?
C42C C41C C44C 111.6(12) . . ?
C43C C41C C44C 109.2(11) . . ?
C42C C41C C4C 111.9(12) . . ?
C43C C41C C4C 109.6(13) . . ?
C44C C41C C4C 106.0(11) . . ?
C4C C5C C6C 120.1(16) . . ?
C5C C6C C1C 124.4(17) . . ?
C5C C6C C61C 118.4(15) . . ?
C1C C6C C61C 116.5(14) . . ?
N3C C61C C6C 109.0(13) . . ?
C31C N3C C63C 111.3(14) . . ?
C31C N3C C61C 114.5(13) . . ?
C63C N3C C61C 109.5(14) . . ?
C64C C63C N3C 119.6(15) . . ?
C63C C64C C65C 114.9(14) . . ?
C65B C65C C64C 117.3(13) . . ?
F12 B1 F13 111.3(12) . . ?
F12 B1 F11 110.3(11) . . ?
F13 B1 F11 110.6(11) . . ?
F12 B1 F14 109.0(11) . . ?
F13 B1 F14 108.5(10) . . ?
F11 B1 F14 106.9(11) . . ?
F23 B2 F22 111.7(13) . . ?
F23 B2 F24 109.2(13) . . ?
F22 B2 F24 105.3(13) . . ?
F23 B2 F21 109.9(11) . . ?
F22 B2 F21 110.7(13) . . ?
F24 B2 F21 109.9(12) . . ?
F24A B2A F22A 111.1(18) . . ?
F24A B2A F21A 108.3(17) . . ?
F22A B2A F21A 108.1(17) . . ?
F24A B2A F23A 110.9(17) . . ?
F22A B2A F23A 107.6(17) . . ?
F21A B2A F23A 110.8(17) . . ?
F34 B3 F33 108.6(15) . . ?
F34 B3 F32 111.2(15) . . ?
F33 B3 F32 108.0(15) . . ?
F34 B3 F31 109.0(15) . . ?
F33 B3 F31 109.3(15) . . ?
F32 B3 F31 110.7(14) . . ?
F44 B4 F41 109.3(18) . . ?
F44 B4 F43 110.0(18) . . ?
F41 B4 F43 110.2(18) . . ?
F44 B4 F42 109.1(18) . . ?
F41 B4 F42 109.8(18) . . ?
F43 B4 F42 108.4(17) . . ?
B4 F41 F41 158(4) . 2_667 ?
F42A B4A F41A 114(3) . . ?
F42A B4A F44A 114(3) . . ?
F41A B4A F44A 111(3) . . ?
F42A B4A F43A 105(3) . . ?
F41A B4A F43A 105(3) . . ?
F44A B4A F43A 107(3) . . ?
F53 B5 F51 109.0(18) . . ?
F53 B5 F52 110.2(18) . . ?
F51 B5 F52 110.3(18) . . ?
F53 B5 F54 109.8(18) . . ?
F51 B5 F54 112.1(18) . . ?
F52 B5 F54 105.3(17) . . ?
F53 B5 F53 106(2) . 2_656 ?
F51 B5 F53 145(2) . 2_656 ?
F52 B5 F53 54.5(15) . 2_656 ?
F54 B5 F53 55.1(15) . 2_656 ?
F53 B5 B5 64.7(18) . 2_656 ?
F51 B5 B5 174(3) . 2_656 ?
F52 B5 B5 72.1(18) . 2_656 ?
F54 B5 B5 72.3(18) . 2_656 ?
F53 B5 B5 41.5(12) 2_656 2_656 ?
B5 F52 F53 78.5(19) . 2_656 ?
B5 F53 F52 89(2) . 2_656 ?
B5 F53 F54 88(2) . 2_656 ?
F52 F53 F54 91(2) 2_656 2_656 ?
B5 F53 B5 74(2) . 2_656 ?
F52 F53 B5 47.0(13) 2_656 2_656 ?
F54 F53 B5 47.2(13) 2_656 2_656 ?
B5 F54 F53 77.7(19) . 2_656 ?
N100 C100 C101 167(4) . . ?
N200 C200 C201 171(4) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.124


# Attachment 'B902772F_PT_0530_fin.cif'

data_pt0530_pna21
_database_code_depnum_ccdc_archive 'CCDC 719945'
_oxford_structure_analysis_title 'pt0530 in Pna21'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H96 Cu2 N8 O8, 2.5(C2 H4 Cl2)'
_chemical_formula_sum            'C69 H106 Cl5 Cu2 N8 O8'
_chemical_formula_weight         1479.95

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n a 21 '
_symmetry_space_group_name_Hall  'P 2c -2n'

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'

_cell_length_a                   26.318(5)
_cell_length_b                   22.685(4)
_cell_length_c                   13.388(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7993(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    8551
_cell_measurement_theta_min      2
_cell_measurement_theta_max      23

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3132
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            67413
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         22.67
_reflns_number_total             10607
_reflns_number_gt                10358
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1993)'
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;

>>> The Following ALERTS were generated <<<
#------------------------------------------
Format: alert-number_ALERT_alert-type_alert-level text

023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6]..... 22.67 Deg.
341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14

The crystal did not diffract at higher than approx 45 deg in 2TH. For this
reason the data were only integrated to this resolution. This lack of high
resolution data has therefore affected the C-C bond precision.

220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.75 Ratio
222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 9.30 Ratio
230_ALERT_2_B Hirshfeld Test Diff for C412 -- C422 .. 10.72 su
230_ALERT_2_B Hirshfeld Test Diff for C412 -- C442 .. 7.31 su
242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C412
242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C413
230_ALERT_2_C Hirshfeld Test Diff for C412 -- C432 .. 6.67 su
230_ALERT_2_C Hirshfeld Test Diff for C413 -- C423 .. 5.53 su
230_ALERT_2_C Hirshfeld Test Diff for C413 -- C433 .. 6.69 su
230_ALERT_2_C Hirshfeld Test Diff for C413 -- C443 .. 5.45 su
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C411
360_ALERT_2_C Short C(sp3)-C(sp3) Bond C412 - C442 ... 1.43 Ang.
301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc.

The tBu groups present in the structure were badly behaved if left unrestrained
Similarity restraints were applied to ensure sensible bond lengths and angles.
The rotational nature of these tBu groups has however lead to large ADP's which
are often prolate.

221_ALERT_4_A Large Solvent/Anion Cl Ueq(max)/Ueq(min) ... 5.13 Ratio
245_ALERT_2_A U(iso) H30G Smaller than U(eq) Cl3B by ... 0.15 AngSq
231_ALERT_4_C Hirshfeld Test (Solvent) Cl31 -- C301 .. 8.89 su
231_ALERT_4_C Hirshfeld Test (Solvent) Cl32 -- C302 .. 8.60 su
231_ALERT_4_C Hirshfeld Test (Solvent) Cl3A -- C30A .. 5.94 su
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C301
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for Cl3B
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C30A
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C201
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl31
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C302
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl3A
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C30B
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C111
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C112
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C202
722_ALERT_1_C Angle Calc 108.00, Rep 109.10 Dev... 1.10 Deg.
C30B -C30A -H30A 1.555 1.555 1.555
302_ALERT_4_G Anion/Solvent Disorder ......................... 63.00 Perc.

The badly behaved and rather diffuse solvent within the cavity was modelled
as 2.5x 1,2-dichloroethanes per asymmetric unit

910_ALERT_3_B # Missing FCF Reflections Below Th(Min) ........ 12
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/l= 0.542 22

A data collection strategy aimed at collecting fully complete data to 54deg in
2TH was employed. Please refer to the completeness statistics below.

#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.997 4424 4411 13
22.67 0.542 0.994 5623 5589 34

061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.86

The crystal is a plate and this test often fails for plates as a high
range is expected anyway.

232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu2 -- N224 .. 5.03 su
333_ALERT_2_G Check Large Av C6-Ring C-C Dist. C11 -C61 1.40 Ang.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1005

not abnormal given the quality of data

795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C111

no action
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+52.8937P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack, 10348 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.67(2)
_refine_ls_number_reflns         10607
_refine_ls_number_parameters     910
_refine_ls_number_restraints     1005
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0865
_refine_ls_wR_factor_ref         0.1977
_refine_ls_wR_factor_gt          0.1967
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_restrained_S_all      1.190
_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 0.39277(4) 0.78612(4) 0.17256(8) 0.0189(2) Uani 1 1 d . . .
Cu2 Cu 0.00678(4) 0.77344(4) 0.11588(7) 0.0167(2) Uani 1 1 d . . .
O11 O 0.3743(2) 0.8381(3) 0.2767(5) 0.0289(15) Uani 1 1 d U . .
C11 C 0.3623(3) 0.8936(4) 0.2753(7) 0.0244(16) Uani 1 1 d U . .
C12 C 0.4002(3) 0.6786(4) 0.0583(6) 0.0210(15) Uani 1 1 d U . .
O12 O 0.4153(2) 0.7324(2) 0.0731(4) 0.0212(14) Uani 1 1 d U . .
O13 O -0.0123(2) 0.7147(2) 0.2108(4) 0.0217(14) Uani 1 1 d U . .
C13 C 0.0019(3) 0.6599(4) 0.2120(6) 0.0206(15) Uani 1 1 d U . .
O14 O 0.0199(2) 0.8310(3) 0.0194(4) 0.0195(14) Uani 1 1 d U . .
C14 C 0.0350(3) 0.8870(4) 0.0292(6) 0.0168(14) Uani 1 1 d U . .
O21 O 0.4074(2) 0.8423(3) -0.0238(4) 0.0249(14) Uani 1 1 d U . .
H21 H 0.4145 0.8075 -0.0323 0.030 Uiso 1 1 calc R . .
C21 C 0.3643(3) 0.9277(4) 0.1882(7) 0.0252(14) Uani 1 1 d U . .
C22 C 0.3801(3) 0.6423(4) 0.1358(6) 0.0241(14) Uani 1 1 d U . .
O22 O 0.3569(3) 0.7314(3) 0.3577(5) 0.0361(17) Uani 1 1 d U . .
H22 H 0.3586 0.7670 0.3677 0.043 Uiso 1 1 calc R . .
O23 O 0.0436(2) 0.7291(3) -0.0778(4) 0.0269(15) Uani 1 1 d U . .
H23 H 0.0413 0.7650 -0.0841 0.032 Uiso 1 1 calc R . .
C23 C 0.0188(3) 0.6277(3) 0.1282(6) 0.0191(13) Uani 1 1 d U . .
C24 C 0.0371(3) 0.9156(3) 0.1237(7) 0.0192(13) Uani 1 1 d U . .
O24 O -0.0022(2) 0.8172(3) 0.3225(4) 0.0295(15) Uani 1 1 d U . .
H24 H -0.0105 0.7824 0.3247 0.035 Uiso 1 1 calc R . .
C31 C 0.3517(4) 0.9886(4) 0.1903(8) 0.0348(17) Uani 1 1 d U . .
H52A H 0.3546 1.0104 0.1318 0.042 Uiso 1 1 calc R . .
C32 C 0.3705(3) 0.5813(4) 0.1184(8) 0.0265(15) Uani 1 1 d U . .
H27A H 0.3597 0.5579 0.1715 0.032 Uiso 1 1 calc R . .
C33 C 0.0280(3) 0.5675(4) 0.1331(6) 0.0218(15) Uani 1 1 d U . .
H62A H 0.0395 0.5484 0.0760 0.026 Uiso 1 1 calc R . .
C34 C 0.0552(3) 0.9738(3) 0.1284(7) 0.0219(14) Uani 1 1 d U . .
H48A H 0.0574 0.9919 0.1906 0.026 Uiso 1 1 calc R . .
C41 C 0.3354(4) 1.0161(5) 0.2741(8) 0.0388(16) Uani 1 1 d U . .
C42 C 0.3764(3) 0.5564(4) 0.0283(7) 0.0248(14) Uani 1 1 d U . .
C43 C 0.0208(4) 0.5351(4) 0.2174(7) 0.0274(15) Uani 1 1 d U . .
C44 C 0.0698(3) 1.0053(4) 0.0454(6) 0.0202(14) Uani 1 1 d U A .
C51 C 0.3327(4) 0.9804(4) 0.3624(7) 0.0330(17) Uani 1 1 d U . .
H50A H 0.3210 0.9975 0.4212 0.040 Uiso 1 1 calc R . .
C52 C 0.3918(3) 0.5932(4) -0.0499(7) 0.0232(15) Uani 1 1 d U . .
H14A H 0.3944 0.5773 -0.1138 0.028 Uiso 1 1 calc R . .
C53 C 0.0075(3) 0.5674(4) 0.3052(7) 0.0246(15) Uani 1 1 d U . .
H47A H 0.0049 0.5477 0.3660 0.030 Uiso 1 1 calc R . .
C54 C 0.0658(3) 0.9772(3) -0.0451(6) 0.0174(14) Uani 1 1 d U . .
H39A H 0.0754 0.9975 -0.1024 0.021 Uiso 1 1 calc R . .
C61 C 0.3466(3) 0.9217(4) 0.3636(7) 0.0276(15) Uani 1 1 d U . .
C62 C 0.4033(3) 0.6517(4) -0.0364(6) 0.0174(13) Uani 1 1 d U . .
C63 C -0.0019(3) 0.6283(4) 0.3012(6) 0.0222(14) Uani 1 1 d U . .
C64 C 0.0477(3) 0.9192(3) -0.0551(6) 0.0159(13) Uani 1 1 d U . .
C211 C 0.3809(3) 0.9052(4) 0.0908(6) 0.0214(18) Uani 1 1 d U . .
H40A H 0.3832 0.9315 0.0377 0.026 Uiso 1 1 calc R . .
C212 C 0.3708(3) 0.6661(4) 0.2344(6) 0.0235(18) Uani 1 1 d U . .
H37A H 0.3632 0.6389 0.2843 0.028 Uiso 1 1 calc R . .
C213 C 0.0307(3) 0.6569(4) 0.0331(7) 0.0233(17) Uani 1 1 d U . .
H20A H 0.0405 0.6333 -0.0202 0.028 Uiso 1 1 calc R . .
C214 C 0.0227(3) 0.8869(4) 0.2172(7) 0.0205(17) Uani 1 1 d U . .
H44A H 0.0233 0.9096 0.2750 0.025 Uiso 1 1 calc R . .
N221 N 0.3924(3) 0.8510(3) 0.0754(5) 0.0192(17) Uani 1 1 d U . .
N222 N 0.3718(3) 0.7192(3) 0.2598(5) 0.0276(18) Uani 1 1 d U . .
N223 N 0.0284(3) 0.7130(3) 0.0184(5) 0.0172(16) Uani 1 1 d U . .
N224 N 0.0090(3) 0.8323(3) 0.2258(6) 0.0214(17) Uani 1 1 d U . .
C411 C 0.3200(4) 1.0814(5) 0.2801(8) 0.045(2) Uani 1 1 d U . .
C412 C 0.3694(4) 0.4895(4) 0.0105(7) 0.0280(18) Uani 1 1 d U . .
C413 C 0.0269(4) 0.4683(5) 0.2205(8) 0.038(2) Uani 1 1 d U . .
C414 C 0.0899(3) 1.0684(4) 0.0576(7) 0.0252(17) Uani 1 1 d U . .
C421 C 0.2643(5) 1.0864(6) 0.3157(10) 0.060(3) Uani 1 1 d U . .
H75A H 0.2548 1.1272 0.3195 0.090 Uiso 1 1 calc R . .
H75B H 0.2610 1.0686 0.3805 0.090 Uiso 1 1 calc R . .
H75C H 0.2425 1.0664 0.2693 0.090 Uiso 1 1 calc R . .
C422 C 0.4207(8) 0.4618(9) 0.0006(16) 0.124(7) Uani 1 1 d U . .
H20B H 0.4170 0.4202 -0.0102 0.186 Uiso 1 1 calc R . .
H20C H 0.4398 0.4684 0.0607 0.186 Uiso 1 1 calc R . .
H20D H 0.4383 0.4791 -0.0549 0.186 Uiso 1 1 calc R . .
C423 C 0.0169(6) 0.4424(6) 0.3204(10) 0.069(4) Uani 1 1 d U . .
H82A H 0.0421 0.4561 0.3668 0.103 Uiso 1 1 calc R . .
H82B H 0.0183 0.4002 0.3161 0.103 Uiso 1 1 calc R . .
H82C H -0.0162 0.4542 0.3429 0.103 Uiso 1 1 calc R . .
C424 C 0.1013(5) 1.0965(6) -0.0389(10) 0.034(4) Uani 0.761(14) 1 d PU A 1
H79A H 0.1270 1.0742 -0.0730 0.051 Uiso 0.761(14) 1 calc PR A 1
H79B H 0.1133 1.1359 -0.0277 0.051 Uiso 0.761(14) 1 calc PR A 1
H79C H 0.0711 1.0977 -0.0789 0.051 Uiso 0.761(14) 1 calc PR A 1
C431 C 0.3237(6) 1.1109(6) 0.1774(12) 0.076(4) Uani 1 1 d U . .
H10G H 0.3137 1.1515 0.1829 0.115 Uiso 1 1 calc R . .
H10U H 0.3016 1.0910 0.1314 0.115 Uiso 1 1 calc R . .
H10I H 0.3580 1.1086 0.1537 0.115 Uiso 1 1 calc R . .
C432 C 0.3376(6) 0.4782(6) -0.0799(11) 0.072(4) Uani 1 1 d U . .
H88A H 0.3341 0.4365 -0.0897 0.108 Uiso 1 1 calc R . .
H88B H 0.3537 0.4954 -0.1373 0.108 Uiso 1 1 calc R . .
H88C H 0.3047 0.4955 -0.0708 0.108 Uiso 1 1 calc R . .
C433 C 0.0720(6) 0.4496(7) 0.1684(14) 0.090(5) Uani 1 1 d U . .
H10D H 0.1015 0.4625 0.2046 0.135 Uiso 1 1 calc R . .
H10E H 0.0724 0.4665 0.1027 0.135 Uiso 1 1 calc R . .
H10F H 0.0723 0.4074 0.1633 0.135 Uiso 1 1 calc R . .
C434 C 0.1354(5) 1.0700(6) 0.1285(10) 0.038(4) Uani 0.761(14) 1 d PU A 1
H94A H 0.1627 1.0472 0.1008 0.057 Uiso 0.761(14) 1 calc PR A 1
H94B H 0.1258 1.0539 0.1920 0.057 Uiso 0.761(14) 1 calc PR A 1
H94C H 0.1464 1.1101 0.1371 0.057 Uiso 0.761(14) 1 calc PR A 1
C441 C 0.3547(5) 1.1134(6) 0.3494(11) 0.069(4) Uani 1 1 d U . .
H81A H 0.3447 1.1540 0.3532 0.103 Uiso 1 1 calc R . .
H81B H 0.3889 1.1108 0.3250 0.103 Uiso 1 1 calc R . .
H81C H 0.3528 1.0959 0.4146 0.103 Uiso 1 1 calc R . .
C442 C 0.3459(6) 0.4599(7) 0.0928(12) 0.089(5) Uani 1 1 d U . .
H10S H 0.3430 0.4186 0.0781 0.133 Uiso 1 1 calc R . .
H10T H 0.3127 0.4762 0.1039 0.133 Uiso 1 1 calc R . .
H10L H 0.3663 0.4651 0.1517 0.133 Uiso 1 1 calc R . .
C443 C -0.0160(6) 0.4417(7) 0.1491(12) 0.088(5) Uani 1 1 d U . .
H84A H -0.0489 0.4510 0.1755 0.132 Uiso 1 1 calc R . .
H84B H -0.0121 0.3997 0.1452 0.132 Uiso 1 1 calc R . .
H84C H -0.0126 0.4584 0.0835 0.132 Uiso 1 1 calc R . .
C444 C 0.0473(4) 1.1075(5) 0.1080(10) 0.029(3) Uani 0.761(14) 1 d PU A 1
H10A H 0.0597 1.1470 0.1164 0.043 Uiso 0.761(14) 1 calc PR A 1
H10B H 0.0387 1.0913 0.1720 0.043 Uiso 0.761(14) 1 calc PR A 1
H10C H 0.0177 1.1080 0.0662 0.043 Uiso 0.761(14) 1 calc PR A 1
C454 C 0.0932(14) 1.0936(16) 0.147(3) 0.027(11) Uani 0.239(14) 1 d PU A 2
H79D H 0.1137 1.0696 0.1903 0.040 Uiso 0.239(14) 1 calc PR A 2
H79E H 0.0598 1.0977 0.1751 0.040 Uiso 0.239(14) 1 calc PR A 2
H79F H 0.1085 1.1318 0.1405 0.040 Uiso 0.239(14) 1 calc PR A 2
C464 C 0.1462(16) 1.0702(19) -0.001(3) 0.036(11) Uani 0.239(14) 1 d PU A 2
H94D H 0.1429 1.0524 -0.0660 0.053 Uiso 0.239(14) 1 calc PR A 2
H94E H 0.1709 1.0488 0.0372 0.053 Uiso 0.239(14) 1 calc PR A 2
H94F H 0.1570 1.1104 -0.0085 0.053 Uiso 0.239(14) 1 calc PR A 2
C474 C 0.0593(13) 1.1062(15) -0.018(3) 0.019(9) Uani 0.239(14) 1 d PU A 2
H10J H 0.0581 1.0863 -0.0812 0.028 Uiso 0.239(14) 1 calc PR A 2
H10K H 0.0755 1.1438 -0.0259 0.028 Uiso 0.239(14) 1 calc PR A 2
H10H H 0.0254 1.1118 0.0066 0.028 Uiso 0.239(14) 1 calc PR A 2
C611 C 0.3487(4) 0.8896(4) 0.4614(7) 0.0334(19) Uani 1 1 d U . .
H56A H 0.3842 0.8836 0.4783 0.040 Uiso 1 1 calc R . .
H56B H 0.3343 0.9151 0.5122 0.040 Uiso 1 1 calc R . .
C612 C 0.4227(3) 0.6889(4) -0.1230(6) 0.0165(16) Uani 1 1 d U . .
H51A H 0.4578 0.6996 -0.1100 0.020 Uiso 1 1 calc R . .
H51B H 0.4221 0.6652 -0.1833 0.020 Uiso 1 1 calc R . .
C613 C -0.0192(3) 0.6598(4) 0.3966(6) 0.0203(17) Uani 1 1 d U . .
H18A H -0.0539 0.6732 0.3877 0.024 Uiso 1 1 calc R . .
H18B H -0.0189 0.6320 0.4515 0.024 Uiso 1 1 calc R . .
C614 C 0.0405(3) 0.8927(4) -0.1576(6) 0.0165(16) Uani 1 1 d U . .
H34A H 0.0048 0.8835 -0.1666 0.020 Uiso 1 1 calc R . .
H34B H 0.0496 0.9219 -0.2074 0.020 Uiso 1 1 calc R . .
N621 N 0.3230(3) 0.8327(4) 0.4669(6) 0.038(2) Uani 1 1 d U . .
N622 N 0.3935(3) 0.7427(3) -0.1403(5) 0.0180(16) Uani 1 1 d U . .
N623 N 0.0125(3) 0.7102(3) 0.4228(6) 0.033(2) Uani 1 1 d U . .
N624 N 0.0705(3) 0.8387(3) -0.1758(5) 0.0217(16) Uani 1 1 d U . .
C631 C 0.3387(5) 0.8045(6) 0.5613(9) 0.061(3) Uani 1 1 d U . .
H76A H 0.3225 0.7668 0.5672 0.092 Uiso 1 1 calc R . .
H76B H 0.3289 0.8290 0.6166 0.092 Uiso 1 1 calc R . .
H76C H 0.3749 0.7994 0.5616 0.092 Uiso 1 1 calc R . .
C632 C 0.4189(4) 0.7756(4) -0.2206(7) 0.029(2) Uani 1 1 d U . .
H31A H 0.4534 0.7834 -0.2019 0.043 Uiso 1 1 calc R . .
H31B H 0.4014 0.8121 -0.2316 0.043 Uiso 1 1 calc R . .
H31C H 0.4184 0.7526 -0.2809 0.043 Uiso 1 1 calc R . .
C633 C -0.0096(4) 0.7382(5) 0.5109(8) 0.042(3) Uani 1 1 d U . .
H59A H 0.0103 0.7719 0.5292 0.063 Uiso 1 1 calc R . .
H59B H -0.0101 0.7105 0.5652 0.063 Uiso 1 1 calc R . .
H59C H -0.0437 0.7504 0.4961 0.063 Uiso 1 1 calc R . .
C634 C 0.0546(4) 0.8125(4) -0.2705(7) 0.028(2) Uani 1 1 d U . .
H67A H 0.0190 0.8034 -0.2678 0.042 Uiso 1 1 calc R . .
H67B H 0.0736 0.7770 -0.2822 0.042 Uiso 1 1 calc R . .
H67C H 0.0609 0.8398 -0.3239 0.042 Uiso 1 1 calc R . .
C641 C 0.2693(5) 0.8420(5) 0.4615(10) 0.054(2) Uani 1 1 d U . .
H68A H 0.2618 0.8668 0.4044 0.064 Uiso 1 1 calc R . .
H68B H 0.2583 0.8627 0.5210 0.064 Uiso 1 1 calc R . .
C642 C 0.3408(3) 0.7308(4) -0.1674(7) 0.0203(17) Uani 1 1 d U . .
H57A H 0.3276 0.7004 -0.1235 0.024 Uiso 1 1 calc R . .
H57B H 0.3399 0.7156 -0.2350 0.024 Uiso 1 1 calc R . .
C643 C 0.0643(4) 0.6944(5) 0.4364(9) 0.044(2) Uani 1 1 d U . .
H71A H 0.0758 0.6716 0.3794 0.053 Uiso 1 1 calc R . .
H71B H 0.0675 0.6699 0.4954 0.053 Uiso 1 1 calc R . .
C644 C 0.1236(3) 0.8530(4) -0.1771(7) 0.0292(18) Uani 1 1 d U . .
H49A H 0.1316 0.8748 -0.1168 0.035 Uiso 1 1 calc R . .
H49B H 0.1299 0.8791 -0.2333 0.035 Uiso 1 1 calc R . .
C651 C 0.2395(5) 0.7855(5) 0.4523(10) 0.059(2) Uani 1 1 d U . .
H60A H 0.2478 0.7668 0.3892 0.070 Uiso 1 1 calc R . .
H60B H 0.2496 0.7590 0.5055 0.070 Uiso 1 1 calc R . .
C652 C 0.3068(3) 0.7841(4) -0.1611(7) 0.0241(15) Uani 1 1 d U . .
H36A H 0.3176 0.8132 -0.2097 0.029 Uiso 1 1 calc R . .
H36B H 0.3096 0.8015 -0.0952 0.029 Uiso 1 1 calc R . .
C653 C 0.0986(4) 0.7499(5) 0.4481(10) 0.053(2) Uani 1 1 d U . .
H89A H 0.0911 0.7773 0.3945 0.064 Uiso 1 1 calc R . .
H89B H 0.0906 0.7692 0.5107 0.064 Uiso 1 1 calc R . .
C654 C 0.1597(3) 0.8014(4) -0.1845(7) 0.0288(16) Uani 1 1 d U . .
H42A H 0.1512 0.7732 -0.1326 0.035 Uiso 1 1 calc R . .
H42B H 0.1545 0.7821 -0.2484 0.035 Uiso 1 1 calc R . .
C661 C 0.1847(5) 0.7952(5) 0.4574(10) 0.058(2) Uani 1 1 d U . .
H73A H 0.1748 0.8223 0.4049 0.070 Uiso 1 1 calc R . .
H73B H 0.1764 0.8134 0.5209 0.070 Uiso 1 1 calc R . .
C662 C 0.2507(3) 0.7668(4) -0.1814(7) 0.0282(16) Uani 1 1 d U . .
H80A H 0.2483 0.7496 -0.2475 0.034 Uiso 1 1 calc R . .
H80B H 0.2405 0.7370 -0.1335 0.034 Uiso 1 1 calc R . .
C663 C 0.1526(5) 0.7361(5) 0.4462(10) 0.057(2) Uani 1 1 d U . .
H66A H 0.1612 0.7169 0.3837 0.069 Uiso 1 1 calc R . .
H66B H 0.1608 0.7094 0.5004 0.069 Uiso 1 1 calc R . .
C664 C 0.21475(13) 0.81746(19) -0.1749(4) 0.0302(16) Uani 1 1 d U . .
H61A H 0.2232 0.8455 -0.2271 0.036 Uiso 1 1 calc R . .
H61B H 0.2198 0.8371 -0.1113 0.036 Uiso 1 1 calc R . .
Cl11 Cl 0.22364(13) 0.93693(19) 0.1655(4) 0.133(2) Uani 0.88 1 d PRD . .
Cl12 Cl 0.13143(13) 0.78261(19) 0.1305(4) 0.180(4) Uani 0.88 1 d PRD . .
C111 C 0.17978(13) 0.88888(19) 0.1151(4) 0.091(4) Uani 0.88 1 d PRDU . .
H66C H 0.1510 0.9114 0.0907 0.110 Uiso 0.88 1 calc PR . .
H66D H 0.1951 0.8691 0.0583 0.110 Uiso 0.88 1 calc PR . .
C112 C 0.1619(7) 0.8457(7) 0.1833(14) 0.096(4) Uani 0.88 1 d PDU . .
H66E H 0.1382 0.8645 0.2286 0.115 Uiso 0.88 1 calc PR . .
H66F H 0.1905 0.8322 0.2228 0.115 Uiso 0.88 1 calc PR . .
C201 C 0.2421(8) 0.6913(7) 0.1553(17) 0.121(6) Uani 0.88 1 d PDU . .
H77A H 0.2613 0.6768 0.2120 0.146 Uiso 0.88 1 calc PR . .
H77B H 0.2082 0.7013 0.1782 0.146 Uiso 0.88 1 calc PR . .
C202 C 0.2392(9) 0.6480(7) 0.0829(17) 0.123(6) Uani 0.88 1 d PDU . .
H77C H 0.2733 0.6383 0.0609 0.147 Uiso 0.88 1 calc PR . .
H77D H 0.2208 0.6635 0.0258 0.147 Uiso 0.88 1 calc PR . .
Cl22 Cl 0.2081(4) 0.5813(3) 0.1250(6) 0.174(4) Uani 0.88 1 d PD . .
Cl21 Cl 0.27290(13) 0.75666(19) 0.1044(3) 0.0731(11) Uani 0.88 1 d PD . .
Cl31 Cl 0.1402(3) 0.5459(4) 0.4133(6) 0.076(2) Uani 0.50 1 d PD B 1
Cl32 Cl 0.2932(3) 0.4847(3) 0.3679(7) 0.078(2) Uani 0.50 1 d PD B 1
C301 C 0.2084(9) 0.5461(18) 0.402(7) 0.201(16) Uani 0.50 1 d PDU B 1
H30E H 0.2184 0.5747 0.3521 0.241 Uiso 0.50 1 calc PR B 1
H30F H 0.2231 0.5582 0.4655 0.241 Uiso 0.50 1 calc PR B 1
C302 C 0.2272(9) 0.4916(18) 0.377(5) 0.201(16) Uani 0.50 1 d PDU B 1
H30G H 0.2127 0.4807 0.3127 0.241 Uiso 0.50 1 calc PR B 1
H30H H 0.2152 0.4633 0.4255 0.241 Uiso 0.50 1 calc PR B 1
Cl3A Cl 0.2526(7) 0.6202(7) 0.4056(15) 0.096(5) Uani 0.25 1 d PD C 2
Cl3B Cl 0.1926(17) 0.455(3) 0.375(4) 0.39(5) Uani 0.25 1 d PD C 2
C30A C 0.2014(19) 0.570(2) 0.411(12) 0.201(16) Uani 0.25 1 d PDU C 2
H30A H 0.1752 0.5856 0.4546 0.241 Uiso 0.25 1 calc PR C 2
H30B H 0.1869 0.5654 0.3450 0.241 Uiso 0.25 1 calc PR C 2
C30B C 0.216(4) 0.514(2) 0.447(6) 0.201(16) Uani 0.25 1 d PDU C 2
H30C H 0.2043 0.5099 0.5149 0.241 Uiso 0.25 1 calc PR C 2
H30D H 0.2530 0.5124 0.4476 0.241 Uiso 0.25 1 calc PR C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0323(6) 0.0103(4) 0.0140(5) -0.0008(5) 0.0021(5) 0.0030(4)
Cu2 0.0297(6) 0.0095(4) 0.0111(4) -0.0007(4) 0.0006(5) -0.0011(4)
O11 0.035(3) 0.026(3) 0.026(3) -0.004(3) 0.001(3) 0.006(3)
C11 0.025(3) 0.022(3) 0.026(3) -0.005(2) 0.005(2) 0.000(3)
C12 0.024(3) 0.022(3) 0.017(3) 0.003(2) -0.001(2) -0.002(2)
O12 0.030(3) 0.017(3) 0.016(3) -0.001(2) -0.003(2) -0.006(2)
O13 0.034(3) 0.017(3) 0.014(3) 0.002(2) 0.005(2) 0.004(2)
C13 0.018(3) 0.022(3) 0.023(3) 0.003(2) -0.001(2) 0.002(2)
O14 0.028(3) 0.017(3) 0.014(3) 0.000(2) -0.005(2) -0.007(2)
C14 0.022(3) 0.015(3) 0.014(3) 0.001(2) -0.003(2) -0.002(2)
O21 0.034(3) 0.018(3) 0.022(3) 0.003(2) 0.006(2) 0.003(2)
C21 0.028(3) 0.023(2) 0.024(3) -0.003(2) 0.000(2) 0.000(2)
C22 0.031(3) 0.024(3) 0.017(2) 0.001(2) -0.004(2) -0.002(2)
O22 0.056(4) 0.031(3) 0.021(3) -0.003(3) 0.013(3) 0.005(3)
O23 0.046(3) 0.021(3) 0.014(3) 0.003(2) 0.009(2) 0.000(3)
C23 0.023(2) 0.017(2) 0.018(2) 0.002(2) 0.001(2) 0.003(2)
C24 0.022(2) 0.016(2) 0.019(2) -0.002(2) 0.000(2) -0.003(2)
O24 0.049(3) 0.021(3) 0.018(3) 0.003(2) 0.006(3) -0.007(3)
C31 0.038(3) 0.031(3) 0.036(3) -0.005(3) 0.002(3) -0.001(3)
C32 0.029(3) 0.025(3) 0.025(3) 0.004(3) 0.000(3) 0.000(2)
C33 0.026(3) 0.019(3) 0.020(3) -0.003(2) 0.004(2) 0.005(2)
C34 0.0224(16) 0.0218(16) 0.0214(17) 0.0002(9) -0.0003(9) -0.0001(9)
C41 0.042(3) 0.034(3) 0.041(3) -0.006(2) 0.001(3) -0.001(2)
C42 0.028(3) 0.022(3) 0.024(2) 0.005(2) -0.005(2) 0.001(2)
C43 0.032(3) 0.022(3) 0.028(2) 0.002(2) 0.007(2) 0.003(2)
C44 0.025(2) 0.017(2) 0.018(2) 0.003(2) -0.004(2) 0.000(2)
C51 0.034(3) 0.032(3) 0.033(3) -0.007(3) 0.003(3) -0.004(3)
C52 0.028(3) 0.021(3) 0.021(3) 0.002(2) -0.005(2) 0.000(2)
C53 0.028(3) 0.022(3) 0.024(3) 0.003(2) 0.006(2) 0.001(2)
C54 0.023(3) 0.015(3) 0.015(3) 0.009(2) -0.004(2) 0.001(2)
C61 0.026(3) 0.028(3) 0.029(3) -0.005(2) 0.002(2) -0.001(2)
C62 0.023(2) 0.016(2) 0.013(2) 0.003(2) 0.000(2) 0.000(2)
C63 0.025(3) 0.021(2) 0.020(2) 0.003(2) -0.002(2) 0.000(2)
C64 0.020(2) 0.015(2) 0.013(2) 0.005(2) -0.002(2) 0.000(2)
C211 0.027(3) 0.017(3) 0.021(3) 0.000(3) -0.003(3) -0.001(3)
C212 0.034(3) 0.021(3) 0.016(3) 0.002(3) 0.003(3) -0.003(3)
C213 0.030(3) 0.018(3) 0.023(3) -0.001(3) 0.001(3) 0.000(3)
C214 0.025(3) 0.019(3) 0.018(3) 0.002(3) 0.003(3) -0.001(3)
N221 0.016(3) 0.024(3) 0.017(3) -0.001(3) -0.001(3) -0.002(3)
N222 0.038(4) 0.024(3) 0.020(3) 0.004(3) 0.012(3) 0.000(3)
N223 0.023(3) 0.016(3) 0.012(3) 0.005(3) 0.002(3) 0.000(3)
N224 0.025(3) 0.018(3) 0.021(3) 0.005(3) 0.001(3) 0.003(3)
C411 0.048(4) 0.039(3) 0.048(4) -0.005(3) 0.002(3) 0.002(3)
C412 0.033(3) 0.024(3) 0.027(3) 0.004(3) -0.006(3) 0.001(3)
C413 0.043(3) 0.035(3) 0.036(3) 0.003(3) 0.012(3) 0.006(3)
C414 0.031(3) 0.018(3) 0.026(3) 0.002(3) -0.006(3) -0.003(3)
C421 0.061(5) 0.052(5) 0.068(5) -0.011(4) 0.000(4) 0.008(4)
C422 0.125(8) 0.115(8) 0.132(8) -0.003(5) -0.003(5) 0.000(5)
C423 0.080(5) 0.059(5) 0.067(5) 0.002(4) 0.009(4) 0.008(4)
C424 0.034(5) 0.033(5) 0.034(5) -0.005(4) 0.002(4) -0.007(4)
C431 0.085(6) 0.066(5) 0.078(5) 0.000(4) 0.007(4) 0.012(4)
C432 0.082(6) 0.062(5) 0.072(5) 0.006(4) -0.011(4) -0.006(4)
C433 0.093(6) 0.085(6) 0.092(6) 0.000(5) 0.015(5) 0.013(4)
C434 0.044(5) 0.034(5) 0.036(5) 0.001(4) -0.006(4) -0.008(4)
C441 0.072(5) 0.060(5) 0.074(6) -0.007(4) 0.002(4) 0.001(4)
C442 0.103(6) 0.076(6) 0.087(6) 0.000(4) 0.009(5) -0.009(4)
C443 0.096(6) 0.079(6) 0.088(6) -0.003(4) 0.004(4) -0.004(4)
C444 0.033(5) 0.021(4) 0.032(5) -0.003(4) 0.001(4) -0.001(4)
C454 0.028(11) 0.027(11) 0.026(11) -0.004(5) 0.000(5) -0.001(5)
C464 0.037(12) 0.034(12) 0.036(12) 0.000(5) -0.001(5) -0.002(5)
C474 0.017(10) 0.020(10) 0.020(10) 0.005(5) -0.001(5) -0.001(5)
C611 0.032(3) 0.037(3) 0.031(3) -0.006(3) 0.000(3) 0.003(3)
C612 0.021(3) 0.016(3) 0.012(3) 0.003(3) -0.004(3) 0.001(3)
C613 0.026(3) 0.018(3) 0.016(3) 0.004(3) -0.005(3) -0.002(3)
C614 0.019(3) 0.018(3) 0.013(3) 0.005(3) 0.000(3) -0.001(3)
N621 0.049(4) 0.038(4) 0.028(4) 0.002(3) -0.002(3) 0.006(3)
N622 0.024(3) 0.016(3) 0.014(3) 0.006(3) 0.004(3) 0.005(3)
N623 0.046(4) 0.026(3) 0.028(4) -0.007(3) 0.006(3) -0.005(3)
N624 0.027(3) 0.022(3) 0.015(3) -0.004(3) 0.003(3) -0.001(3)
C631 0.068(5) 0.066(5) 0.050(5) 0.004(4) -0.004(4) 0.004(4)
C632 0.035(4) 0.027(4) 0.025(4) 0.005(3) 0.002(3) 0.001(3)
C633 0.055(5) 0.038(4) 0.034(4) -0.004(4) 0.001(4) -0.003(4)
C634 0.030(4) 0.033(4) 0.022(4) -0.001(3) 0.004(3) -0.005(3)
C641 0.058(4) 0.049(4) 0.054(4) -0.005(3) 0.004(3) -0.002(3)
C642 0.025(3) 0.017(3) 0.019(3) -0.002(3) -0.001(3) -0.001(3)
C643 0.050(4) 0.041(4) 0.042(4) -0.001(3) -0.002(3) -0.010(3)
C644 0.032(3) 0.027(3) 0.029(3) 0.000(3) 0.001(3) 0.003(3)
C651 0.059(3) 0.056(3) 0.061(3) -0.005(3) 0.004(3) 0.000(3)
C652 0.028(3) 0.021(3) 0.023(3) 0.001(2) 0.001(2) 0.004(2)
C653 0.054(3) 0.051(3) 0.055(3) -0.004(3) -0.002(3) -0.007(3)
C654 0.032(3) 0.025(3) 0.029(3) 0.001(3) 0.003(3) 0.002(3)
C661 0.059(3) 0.055(3) 0.061(3) -0.004(3) 0.004(3) -0.003(3)
C662 0.029(3) 0.027(3) 0.029(3) -0.001(3) 0.000(3) 0.001(3)
C663 0.058(3) 0.055(3) 0.059(3) -0.004(3) 0.001(3) -0.004(3)
C664 0.030(3) 0.030(3) 0.031(3) 0.000(3) 0.003(3) 0.002(3)
Cl11 0.110(4) 0.140(5) 0.149(5) -0.027(5) -0.041(4) 0.018(4)
Cl12 0.063(3) 0.246(9) 0.233(9) -0.151(8) -0.047(4) 0.042(4)
C111 0.087(5) 0.095(5) 0.092(5) -0.002(4) -0.003(4) 0.008(4)
C112 0.092(5) 0.097(5) 0.098(5) 0.000(4) -0.005(4) 0.007(4)
C201 0.121(7) 0.121(7) 0.122(7) -0.002(4) -0.003(4) 0.003(4)
C202 0.123(7) 0.123(7) 0.122(7) -0.001(4) -0.004(4) 0.003(4)
Cl22 0.313(11) 0.107(4) 0.103(5) 0.021(4) -0.012(6) -0.019(6)
Cl21 0.046(2) 0.099(3) 0.073(3) 0.025(3) 0.002(2) 0.0093(19)
Cl31 0.053(4) 0.090(5) 0.084(5) 0.024(4) 0.002(4) 0.024(4)
Cl32 0.063(4) 0.062(4) 0.109(6) -0.012(4) 0.026(4) 0.013(3)
C301 0.201(16) 0.201(16) 0.200(16) 0.000(3) -0.001(3) 0.000(3)
C302 0.201(16) 0.201(16) 0.200(16) 0.000(3) -0.001(3) 0.000(3)
Cl3A 0.101(12) 0.058(9) 0.129(15) -0.002(9) 0.010(11) -0.001(9)
Cl3B 0.20(4) 0.76(14) 0.21(4) 0.04(6) 0.12(3) -0.17(6)
C30A 0.201(16) 0.201(16) 0.200(16) 0.000(4) -0.001(3) 0.000(3)
C30B 0.201(16) 0.201(16) 0.200(16) 0.000(3) -0.001(3) 0.000(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O11 1.889(6) . ?
Cu1 O12 1.901(6) . ?
Cu1 N221 1.965(7) . ?
Cu1 N222 1.994(7) . ?
Cu2 O14 1.869(6) . ?
Cu2 O13 1.909(6) . ?
Cu2 N223 1.976(7) . ?
Cu2 N224 1.989(8) . ?
O11 C11 1.299(11) . ?
C11 C21 1.400(13) . ?
C11 C61 1.405(13) . ?
C12 O12 1.299(10) . ?
C12 C62 1.409(12) . ?
C12 C22 1.427(12) . ?
O13 C13 1.297(10) . ?
C13 C63 1.397(12) . ?
C13 C23 1.411(12) . ?
O14 C14 1.337(10) . ?
C14 C64 1.386(12) . ?
C14 C24 1.424(12) . ?
O21 N221 1.399(9) . ?
O21 H21 0.8200 . ?
C21 C31 1.422(13) . ?
C21 C211 1.467(12) . ?
C22 C32 1.426(12) . ?
C22 C212 1.447(12) . ?
O22 N222 1.396(9) . ?
O22 H22 0.8200 . ?
O23 N223 1.397(9) . ?
O23 H23 0.8200 . ?
C23 C33 1.388(11) . ?
C23 C213 1.469(12) . ?
C24 C34 1.403(11) . ?
C24 C214 1.461(12) . ?
O24 N224 1.371(10) . ?
O24 H24 0.8200 . ?
C31 C41 1.353(14) . ?
C31 H52A 0.9300 . ?
C32 C42 1.342(13) . ?
C32 H27A 0.9300 . ?
C33 C43 1.360(12) . ?
C33 H62A 0.9300 . ?
C34 C44 1.375(12) . ?
C34 H48A 0.9300 . ?
C41 C51 1.434(14) . ?
C41 C411 1.537(15) . ?
C42 C52 1.399(13) . ?
C42 C412 1.547(13) . ?
C43 C53 1.428(13) . ?
C43 C413 1.524(14) . ?
C44 C54 1.373(12) . ?
C44 C414 1.535(12) . ?
C51 C61 1.381(13) . ?
C51 H50A 0.9300 . ?
C52 C62 1.374(12) . ?
C52 H14A 0.9300 . ?
C53 C63 1.405(12) . ?
C53 H47A 0.9300 . ?
C54 C64 1.406(11) . ?
C54 H39A 0.9300 . ?
C61 C611 1.499(14) . ?
C62 C612 1.521(11) . ?
C63 C613 1.533(12) . ?
C64 C614 1.511(11) . ?
C211 N221 1.283(11) . ?
C211 H40A 0.9300 . ?
C212 N222 1.253(11) . ?
C212 H37A 0.9300 . ?
C213 N223 1.289(11) . ?
C213 H20A 0.9300 . ?
C214 N224 1.294(12) . ?
C214 H44A 0.9300 . ?
C411 C441 1.490(17) . ?
C411 C431 1.532(18) . ?
C411 C421 1.546(16) . ?
C412 C442 1.430(17) . ?
C412 C432 1.494(16) . ?
C412 C422 1.50(2) . ?
C413 C433 1.442(17) . ?
C413 C423 1.484(17) . ?
C413 C443 1.597(18) . ?
C414 C454 1.33(3) . ?
C414 C424 1.472(16) . ?
C414 C434 1.529(16) . ?
C414 C474 1.55(3) . ?
C414 C444 1.580(15) . ?
C414 C464 1.68(4) . ?
C421 H75A 0.9600 . ?
C421 H75B 0.9600 . ?
C421 H75C 0.9600 . ?
C422 H20B 0.9600 . ?
C422 H20C 0.9600 . ?
C422 H20D 0.9600 . ?
C423 H82A 0.9600 . ?
C423 H82B 0.9600 . ?
C423 H82C 0.9600 . ?
C424 H79A 0.9600 . ?
C424 H79B 0.9600 . ?
C424 H79C 0.9600 . ?
C431 H10G 0.9600 . ?
C431 H10U 0.9600 . ?
C431 H10I 0.9600 . ?
C432 H88A 0.9600 . ?
C432 H88B 0.9600 . ?
C432 H88C 0.9600 . ?
C433 H10D 0.9600 . ?
C433 H10E 0.9600 . ?
C433 H10F 0.9600 . ?
C434 H94A 0.9600 . ?
C434 H94B 0.9600 . ?
C434 H94C 0.9600 . ?
C441 H81A 0.9600 . ?
C441 H81B 0.9600 . ?
C441 H81C 0.9600 . ?
C442 H10S 0.9600 . ?
C442 H10T 0.9600 . ?
C442 H10L 0.9600 . ?
C443 H84A 0.9600 . ?
C443 H84B 0.9600 . ?
C443 H84C 0.9600 . ?
C444 H10A 0.9600 . ?
C444 H10B 0.9600 . ?
C444 H10C 0.9600 . ?
C454 H79D 0.9600 . ?
C454 H79E 0.9600 . ?
C454 H79F 0.9600 . ?
C464 H94D 0.9600 . ?
C464 H94E 0.9600 . ?
C464 H94F 0.9600 . ?
C474 H10J 0.9600 . ?
C474 H10K 0.9600 . ?
C474 H10H 0.9600 . ?
C611 N621 1.460(13) . ?
C611 H56A 0.9700 . ?
C611 H56B 0.9700 . ?
C612 N622 1.461(10) . ?
C612 H51A 0.9700 . ?
C612 H51B 0.9700 . ?
C613 N623 1.458(11) . ?
C613 H18A 0.9700 . ?
C613 H18B 0.9700 . ?
C614 N624 1.478(11) . ?
C614 H34A 0.9700 . ?
C614 H34B 0.9700 . ?
N621 C641 1.430(15) . ?
N621 C631 1.476(14) . ?
N622 C642 1.458(11) . ?
N622 C632 1.469(11) . ?
N623 C643 1.421(14) . ?
N623 C633 1.462(13) . ?
N624 C644 1.436(11) . ?
N624 C634 1.462(11) . ?
C631 H76A 0.9600 . ?
C631 H76B 0.9600 . ?
C631 H76C 0.9600 . ?
C632 H31A 0.9600 . ?
C632 H31B 0.9600 . ?
C632 H31C 0.9600 . ?
C633 H59A 0.9600 . ?
C633 H59B 0.9600 . ?
C633 H59C 0.9600 . ?
C634 H67A 0.9600 . ?
C634 H67B 0.9600 . ?
C634 H67C 0.9600 . ?
C641 C651 1.506(16) . ?
C641 H68A 0.9700 . ?
C641 H68B 0.9700 . ?
C642 C652 1.506(12) . ?
C642 H57A 0.9700 . ?
C642 H57B 0.9700 . ?
C643 C653 1.556(15) . ?
C643 H71A 0.9700 . ?
C643 H71B 0.9700 . ?
C644 C654 1.510(13) . ?
C644 H49A 0.9700 . ?
C644 H49B 0.9700 . ?
C651 C661 1.462(17) . ?
C651 H60A 0.9700 . ?
C651 H60B 0.9700 . ?
C652 C662 1.551(13) . ?
C652 H36A 0.9700 . ?
C652 H36B 0.9700 . ?
C653 C663 1.455(16) . ?
C653 H89A 0.9700 . ?
C653 H89B 0.9700 . ?
C654 C664 1.500(10) . ?
C654 H42A 0.9700 . ?
C654 H42B 0.9700 . ?
C661 C663 1.590(16) . ?
C661 H73A 0.9700 . ?
C661 H73B 0.9700 . ?
C662 C664 1.490(10) . ?
C662 H80A 0.9700 . ?
C662 H80B 0.9700 . ?
C663 H66A 0.9700 . ?
C663 H66B 0.9700 . ?
C664 H61A 0.9700 . ?
C664 H61B 0.9700 . ?
Cl11 C111 1.7250 . ?
Cl12 C112 1.786(14) . ?
C111 C112 1.419(16) . ?
C111 H66C 0.9700 . ?
C111 H66D 0.9700 . ?
C112 H66E 0.9700 . ?
C112 H66F 0.9700 . ?
C201 C202 1.38(2) . ?
C201 Cl21 1.821(16) . ?
C201 H77A 0.9700 . ?
C201 H77B 0.9700 . ?
C202 Cl22 1.811(15) . ?
C202 H77C 0.9700 . ?
C202 H77D 0.9700 . ?
Cl31 C301 1.80(2) . ?
Cl32 C302 1.75(2) . ?
C301 C302 1.37(3) . ?
C301 H30E 0.9700 . ?
C301 H30F 0.9700 . ?
C302 H30G 0.9700 . ?
C302 H30H 0.9700 . ?
Cl3A C30A 1.77(2) . ?
Cl3B C30B 1.76(2) . ?
C30A C30B 1.40(3) . ?
C30A H30A 0.9700 . ?
C30A H30B 0.9700 . ?
C30B H30C 0.9700 . ?
C30B H30D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Cu1 O12 176.1(3) . . ?
O11 Cu1 N221 91.2(3) . . ?
O12 Cu1 N221 91.0(3) . . ?
O11 Cu1 N222 88.3(3) . . ?
O12 Cu1 N222 90.5(3) . . ?
N221 Cu1 N222 163.2(3) . . ?
O14 Cu2 O13 175.3(3) . . ?
O14 Cu2 N223 88.5(3) . . ?
O13 Cu2 N223 91.8(2) . . ?
O14 Cu2 N224 92.1(2) . . ?
O13 Cu2 N224 89.1(3) . . ?
N223 Cu2 N224 161.1(3) . . ?
C11 O11 Cu1 131.1(6) . . ?
O11 C11 C21 122.6(8) . . ?
O11 C11 C61 120.0(8) . . ?
C21 C11 C61 117.5(8) . . ?
O12 C12 C62 121.7(8) . . ?
O12 C12 C22 123.0(8) . . ?
C62 C12 C22 115.3(8) . . ?
C12 O12 Cu1 127.9(5) . . ?
C13 O13 Cu2 127.0(5) . . ?
O13 C13 C63 118.9(8) . . ?
O13 C13 C23 125.2(8) . . ?
C63 C13 C23 115.8(8) . . ?
C14 O14 Cu2 130.6(5) . . ?
O14 C14 C64 119.5(7) . . ?
O14 C14 C24 122.2(7) . . ?
C64 C14 C24 118.3(7) . . ?
N221 O21 H21 109.5 . . ?
C11 C21 C31 120.7(8) . . ?
C11 C21 C211 124.1(8) . . ?
C31 C21 C211 115.2(8) . . ?
C32 C22 C12 120.5(8) . . ?
C32 C22 C212 118.7(8) . . ?
C12 C22 C212 120.8(8) . . ?
N222 O22 H22 109.5 . . ?
N223 O23 H23 109.5 . . ?
C33 C23 C13 121.8(8) . . ?
C33 C23 C213 116.6(7) . . ?
C13 C23 C213 121.5(7) . . ?
C34 C24 C14 118.8(8) . . ?
C34 C24 C214 118.0(8) . . ?
C14 C24 C214 123.1(7) . . ?
N224 O24 H24 109.5 . . ?
C41 C31 C21 122.6(10) . . ?
C41 C31 H52A 118.7 . . ?
C21 C31 H52A 118.7 . . ?
C42 C32 C22 122.3(9) . . ?
C42 C32 H27A 118.8 . . ?
C22 C32 H27A 118.8 . . ?
C43 C33 C23 123.1(8) . . ?
C43 C33 H62A 118.4 . . ?
C23 C33 H62A 118.4 . . ?
C44 C34 C24 123.2(8) . . ?
C44 C34 H48A 118.4 . . ?
C24 C34 H48A 118.4 . . ?
C31 C41 C51 116.0(9) . . ?
C31 C41 C411 124.8(10) . . ?
C51 C41 C411 119.2(9) . . ?
C32 C42 C52 117.1(8) . . ?
C32 C42 C412 122.5(8) . . ?
C52 C42 C412 120.3(8) . . ?
C33 C43 C53 116.1(8) . . ?
C33 C43 C413 123.0(8) . . ?
C53 C43 C413 120.9(8) . . ?
C54 C44 C34 116.8(8) . . ?
C54 C44 C414 123.5(8) . . ?
C34 C44 C414 119.7(8) . . ?
C61 C51 C41 122.7(9) . . ?
C61 C51 H50A 118.6 . . ?
C41 C51 H50A 118.6 . . ?
C62 C52 C42 122.8(8) . . ?
C62 C52 H14A 118.6 . . ?
C42 C52 H14A 118.6 . . ?
C63 C53 C43 121.1(8) . . ?
C63 C53 H47A 119.5 . . ?
C43 C53 H47A 119.5 . . ?
C44 C54 C64 122.9(8) . . ?
C44 C54 H39A 118.5 . . ?
C64 C54 H39A 118.5 . . ?
C51 C61 C11 120.4(9) . . ?
C51 C61 C611 119.3(9) . . ?
C11 C61 C611 120.2(8) . . ?
C52 C62 C12 121.5(8) . . ?
C52 C62 C612 120.7(7) . . ?
C12 C62 C612 117.7(7) . . ?
C13 C63 C53 121.7(8) . . ?
C13 C63 C613 119.5(8) . . ?
C53 C63 C613 118.7(8) . . ?
C14 C64 C54 119.9(7) . . ?
C14 C64 C614 119.9(7) . . ?
C54 C64 C614 120.2(7) . . ?
N221 C211 C21 123.1(8) . . ?
N221 C211 H40A 118.4 . . ?
C21 C211 H40A 118.4 . . ?
N222 C212 C22 127.1(8) . . ?
N222 C212 H37A 116.5 . . ?
C22 C212 H37A 116.5 . . ?
N223 C213 C23 124.6(8) . . ?
N223 C213 H20A 117.7 . . ?
C23 C213 H20A 117.7 . . ?
N224 C214 C24 125.2(8) . . ?
N224 C214 H44A 117.4 . . ?
C24 C214 H44A 117.4 . . ?
C211 N221 O21 110.8(7) . . ?
C211 N221 Cu1 127.8(6) . . ?
O21 N221 Cu1 121.4(5) . . ?
C212 N222 O22 116.1(7) . . ?
C212 N222 Cu1 125.4(6) . . ?
O22 N222 Cu1 118.5(5) . . ?
C213 N223 O23 112.7(7) . . ?
C213 N223 Cu2 126.6(6) . . ?
O23 N223 Cu2 120.7(5) . . ?
C214 N224 O24 112.6(7) . . ?
C214 N224 Cu2 125.7(6) . . ?
O24 N224 Cu2 121.6(5) . . ?
C441 C411 C431 107.9(11) . . ?
C441 C411 C41 109.9(10) . . ?
C431 C411 C41 110.9(9) . . ?
C441 C411 C421 110.7(10) . . ?
C431 C411 C421 107.7(10) . . ?
C41 C411 C421 109.7(9) . . ?
C442 C412 C432 107.6(11) . . ?
C442 C412 C422 105.2(12) . . ?
C432 C412 C422 111.2(12) . . ?
C442 C412 C42 113.2(10) . . ?
C432 C412 C42 111.0(9) . . ?
C422 C412 C42 108.5(10) . . ?
C433 C413 C423 117.7(11) . . ?
C433 C413 C43 111.5(10) . . ?
C423 C413 C43 113.5(9) . . ?
C433 C413 C443 100.4(11) . . ?
C423 C413 C443 105.4(10) . . ?
C43 C413 C443 106.6(9) . . ?
C454 C414 C424 126.2(17) . . ?
C454 C414 C434 51.7(17) . . ?
C424 C414 C434 111.9(9) . . ?
C454 C414 C44 121.3(17) . . ?
C424 C414 C44 112.4(8) . . ?
C434 C414 C44 111.1(8) . . ?
C454 C414 C474 113(2) . . ?
C424 C414 C474 45.1(14) . . ?
C434 C414 C474 142.9(15) . . ?
C44 C414 C474 105.5(14) . . ?
C454 C414 C444 54.6(17) . . ?
C424 C414 C444 106.0(9) . . ?
C434 C414 C444 106.1(9) . . ?
C44 C414 C444 108.9(8) . . ?
C474 C414 C444 66.4(14) . . ?
C454 C414 C464 111(2) . . ?
C424 C414 C464 52.9(16) . . ?
C434 C414 C464 66.3(16) . . ?
C44 C414 C464 106.1(16) . . ?
C474 C414 C464 98(2) . . ?
C444 C414 C464 144.3(16) . . ?
C411 C421 H75A 109.5 . . ?
C411 C421 H75B 109.5 . . ?
H75A C421 H75B 109.5 . . ?
C411 C421 H75C 109.5 . . ?
H75A C421 H75C 109.5 . . ?
H75B C421 H75C 109.5 . . ?
C412 C422 H20B 109.5 . . ?
C412 C422 H20C 109.5 . . ?
H20B C422 H20C 109.5 . . ?
C412 C422 H20D 109.5 . . ?
H20B C422 H20D 109.5 . . ?
H20C C422 H20D 109.5 . . ?
C413 C423 H82A 109.5 . . ?
C413 C423 H82B 109.5 . . ?
H82A C423 H82B 109.5 . . ?
C413 C423 H82C 109.5 . . ?
H82A C423 H82C 109.5 . . ?
H82B C423 H82C 109.5 . . ?
C414 C424 H79A 109.5 . . ?
C414 C424 H79B 109.5 . . ?
H79A C424 H79B 109.5 . . ?
C414 C424 H79C 109.5 . . ?
H79A C424 H79C 109.5 . . ?
H79B C424 H79C 109.5 . . ?
C411 C431 H10G 109.5 . . ?
C411 C431 H10U 109.5 . . ?
H10G C431 H10U 109.5 . . ?
C411 C431 H10I 109.5 . . ?
H10G C431 H10I 109.5 . . ?
H10U C431 H10I 109.5 . . ?
C412 C432 H88A 109.5 . . ?
C412 C432 H88B 109.5 . . ?
H88A C432 H88B 109.5 . . ?
C412 C432 H88C 109.5 . . ?
H88A C432 H88C 109.5 . . ?
H88B C432 H88C 109.5 . . ?
C413 C433 H10D 109.5 . . ?
C413 C433 H10E 109.5 . . ?
H10D C433 H10E 109.5 . . ?
C413 C433 H10F 109.5 . . ?
H10D C433 H10F 109.5 . . ?
H10E C433 H10F 109.5 . . ?
C414 C434 H94A 109.5 . . ?
C414 C434 H94B 109.5 . . ?
H94A C434 H94B 109.5 . . ?
C414 C434 H94C 109.5 . . ?
H94A C434 H94C 109.5 . . ?
H94B C434 H94C 109.5 . . ?
C411 C441 H81A 109.5 . . ?
C411 C441 H81B 109.5 . . ?
H81A C441 H81B 109.5 . . ?
C411 C441 H81C 109.5 . . ?
H81A C441 H81C 109.5 . . ?
H81B C441 H81C 109.5 . . ?
C412 C442 H10S 109.5 . . ?
C412 C442 H10T 109.5 . . ?
H10S C442 H10T 109.5 . . ?
C412 C442 H10L 109.5 . . ?
H10S C442 H10L 109.5 . . ?
H10T C442 H10L 109.5 . . ?
C413 C443 H84A 109.5 . . ?
C413 C443 H84B 109.5 . . ?
H84A C443 H84B 109.5 . . ?
C413 C443 H84C 109.5 . . ?
H84A C443 H84C 109.5 . . ?
H84B C443 H84C 109.5 . . ?
C414 C444 H10A 109.5 . . ?
C414 C444 H10B 109.5 . . ?
H10A C444 H10B 109.5 . . ?
C414 C444 H10C 109.5 . . ?
H10A C444 H10C 109.5 . . ?
H10B C444 H10C 109.5 . . ?
C414 C454 H79D 109.5 . . ?
C414 C454 H79E 109.5 . . ?
H79D C454 H79E 109.5 . . ?
C414 C454 H79F 109.5 . . ?
H79D C454 H79F 109.5 . . ?
H79E C454 H79F 109.5 . . ?
C414 C464 H94D 109.5 . . ?
C414 C464 H94E 109.5 . . ?
H94D C464 H94E 109.5 . . ?
C414 C464 H94F 109.5 . . ?
H94D C464 H94F 109.5 . . ?
H94E C464 H94F 109.5 . . ?
C414 C474 H10J 109.5 . . ?
C414 C474 H10K 109.5 . . ?
H10J C474 H10K 109.5 . . ?
C414 C474 H10H 109.5 . . ?
H10J C474 H10H 109.5 . . ?
H10K C474 H10H 109.5 . . ?
N621 C611 C61 117.2(8) . . ?
N621 C611 H56A 108.0 . . ?
C61 C611 H56A 108.0 . . ?
N621 C611 H56B 108.0 . . ?
C61 C611 H56B 108.0 . . ?
H56A C611 H56B 107.2 . . ?
N622 C612 C62 114.1(7) . . ?
N622 C612 H51A 108.7 . . ?
C62 C612 H51A 108.7 . . ?
N622 C612 H51B 108.7 . . ?
C62 C612 H51B 108.7 . . ?
H51A C612 H51B 107.6 . . ?
N623 C613 C63 113.3(7) . . ?
N623 C613 H18A 108.9 . . ?
C63 C613 H18A 108.9 . . ?
N623 C613 H18B 108.9 . . ?
C63 C613 H18B 108.9 . . ?
H18A C613 H18B 107.7 . . ?
N624 C614 C64 114.4(6) . . ?
N624 C614 H34A 108.7 . . ?
C64 C614 H34A 108.7 . . ?
N624 C614 H34B 108.7 . . ?
C64 C614 H34B 108.7 . . ?
H34A C614 H34B 107.6 . . ?
C641 N621 C611 109.1(8) . . ?
C641 N621 C631 112.6(9) . . ?
C611 N621 C631 107.3(9) . . ?
C642 N622 C612 112.7(6) . . ?
C642 N622 C632 110.1(7) . . ?
C612 N622 C632 107.6(6) . . ?
C643 N623 C613 112.5(8) . . ?
C643 N623 C633 112.9(8) . . ?
C613 N623 C633 107.8(8) . . ?
C644 N624 C634 111.1(7) . . ?
C644 N624 C614 109.6(7) . . ?
C634 N624 C614 109.1(7) . . ?
N621 C631 H76A 109.5 . . ?
N621 C631 H76B 109.5 . . ?
H76A C631 H76B 109.5 . . ?
N621 C631 H76C 109.5 . . ?
H76A C631 H76C 109.5 . . ?
H76B C631 H76C 109.5 . . ?
N622 C632 H31A 109.5 . . ?
N622 C632 H31B 109.5 . . ?
H31A C632 H31B 109.5 . . ?
N622 C632 H31C 109.5 . . ?
H31A C632 H31C 109.5 . . ?
H31B C632 H31C 109.5 . . ?
N623 C633 H59A 109.5 . . ?
N623 C633 H59B 109.5 . . ?
H59A C633 H59B 109.5 . . ?
N623 C633 H59C 109.5 . . ?
H59A C633 H59C 109.5 . . ?
H59B C633 H59C 109.5 . . ?
N624 C634 H67A 109.5 . . ?
N624 C634 H67B 109.5 . . ?
H67A C634 H67B 109.5 . . ?
N624 C634 H67C 109.5 . . ?
H67A C634 H67C 109.5 . . ?
H67B C634 H67C 109.5 . . ?
N621 C641 C651 113.2(10) . . ?
N621 C641 H68A 108.9 . . ?
C651 C641 H68A 108.9 . . ?
N621 C641 H68B 108.9 . . ?
C651 C641 H68B 108.9 . . ?
H68A C641 H68B 107.8 . . ?
N622 C642 C652 113.8(7) . . ?
N622 C642 H57A 108.8 . . ?
C652 C642 H57A 108.8 . . ?
N622 C642 H57B 108.8 . . ?
C652 C642 H57B 108.8 . . ?
H57A C642 H57B 107.7 . . ?
N623 C643 C653 111.5(9) . . ?
N623 C643 H71A 109.3 . . ?
C653 C643 H71A 109.3 . . ?
N623 C643 H71B 109.3 . . ?
C653 C643 H71B 109.3 . . ?
H71A C643 H71B 108.0 . . ?
N624 C644 C654 115.9(8) . . ?
N624 C644 H49A 108.3 . . ?
C654 C644 H49A 108.3 . . ?
N624 C644 H49B 108.3 . . ?
C654 C644 H49B 108.3 . . ?
H49A C644 H49B 107.4 . . ?
C661 C651 C641 112.5(11) . . ?
C661 C651 H60A 109.1 . . ?
C641 C651 H60A 109.1 . . ?
C661 C651 H60B 109.1 . . ?
C641 C651 H60B 109.1 . . ?
H60A C651 H60B 107.8 . . ?
C642 C652 C662 110.8(7) . . ?
C642 C652 H36A 109.5 . . ?
C662 C652 H36A 109.5 . . ?
C642 C652 H36B 109.5 . . ?
C662 C652 H36B 109.5 . . ?
H36A C652 H36B 108.1 . . ?
C663 C653 C643 113.0(10) . . ?
C663 C653 H89A 109.0 . . ?
C643 C653 H89A 109.0 . . ?
C663 C653 H89B 109.0 . . ?
C643 C653 H89B 109.0 . . ?
H89A C653 H89B 107.8 . . ?
C664 C654 C644 114.4(7) . . ?
C664 C654 H42A 108.7 . . ?
C644 C654 H42A 108.7 . . ?
C664 C654 H42B 108.7 . . ?
C644 C654 H42B 108.7 . . ?
H42A C654 H42B 107.6 . . ?
C651 C661 C663 113.2(10) . . ?
C651 C661 H73A 108.9 . . ?
C663 C661 H73A 108.9 . . ?
C651 C661 H73B 108.9 . . ?
C663 C661 H73B 108.9 . . ?
H73A C661 H73B 107.8 . . ?
C664 C662 C652 113.6(7) . . ?
C664 C662 H80A 108.8 . . ?
C652 C662 H80A 108.8 . . ?
C664 C662 H80B 108.8 . . ?
C652 C662 H80B 108.8 . . ?
H80A C662 H80B 107.7 . . ?
C653 C663 C661 109.5(10) . . ?
C653 C663 H66A 109.8 . . ?
C661 C663 H66A 109.8 . . ?
C653 C663 H66B 109.8 . . ?
C661 C663 H66B 109.8 . . ?
H66A C663 H66B 108.2 . . ?
C662 C664 C654 114.9(6) . . ?
C662 C664 H61A 108.5 . . ?
C654 C664 H61A 108.5 . . ?
C662 C664 H61B 108.5 . . ?
C654 C664 H61B 108.5 . . ?
H61A C664 H61B 107.5 . . ?
C112 C111 Cl11 114.0(7) . . ?
C112 C111 H66C 108.8 . . ?
Cl11 C111 H66C 108.8 . . ?
C112 C111 H66D 108.8 . . ?
Cl11 C111 H66D 108.8 . . ?
H66C C111 H66D 107.7 . . ?
C111 C112 Cl12 116.6(12) . . ?
C111 C112 H66E 108.1 . . ?
Cl12 C112 H66E 108.1 . . ?
C111 C112 H66F 108.1 . . ?
Cl12 C112 H66F 108.1 . . ?
H66E C112 H66F 107.3 . . ?
C202 C201 Cl21 109.9(14) . . ?
C202 C201 H77A 109.7 . . ?
Cl21 C201 H77A 109.7 . . ?
C202 C201 H77B 109.7 . . ?
Cl21 C201 H77B 109.7 . . ?
H77A C201 H77B 108.2 . . ?
C201 C202 Cl22 113.6(15) . . ?
C201 C202 H77C 108.8 . . ?
Cl22 C202 H77C 108.8 . . ?
C201 C202 H77D 108.8 . . ?
Cl22 C202 H77D 108.8 . . ?
H77C C202 H77D 107.7 . . ?
C302 C301 Cl31 112(2) . . ?
C302 C301 H30E 109.2 . . ?
Cl31 C301 H30E 109.2 . . ?
C302 C301 H30F 109.2 . . ?
Cl31 C301 H30F 109.2 . . ?
H30E C301 H30F 107.9 . . ?
C301 C302 Cl32 117(2) . . ?
C301 C302 H30G 108.0 . . ?
Cl32 C302 H30G 108.0 . . ?
C301 C302 H30H 108.0 . . ?
Cl32 C302 H30H 108.0 . . ?
H30G C302 H30H 107.3 . . ?
C30B C30A Cl3A 113(2) . . ?
C30B C30A H30A 109.1 . . ?
Cl3A C30A H30A 109.1 . . ?
C30B C30A H30B 109.1 . . ?
Cl3A C30A H30B 109.1 . . ?
H30A C30A H30B 107.8 . . ?
C30A C30B Cl3B 113(3) . . ?
C30A C30B H30C 108.9 . . ?
Cl3B C30B H30C 108.9 . . ?
C30A C30B H30D 108.9 . . ?
Cl3B C30B H30D 108.9 . . ?
H30C C30B H30D 107.7 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        22.67
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.109