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

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Leone Spiccia'
'Ann Almesaker'
'Patrick Gamez'
'Jan Reedijk'
'Janet Scott'
'Simon J. Teat'

_publ_contact_author_name        'Leone Spiccia'
_publ_contact_author_email       LEONE.SPICCIA@SCI.MONASH.EDU.AU

_publ_section_title              
;
Stabilisation of a very short Cu-F bond within the
protected cavity of a copper(II) compound from a tris(2-aminoethyl)amine
derivative
;

# Attachment 'Cu-F_complex_cif'

data_CuF_complex
_database_code_depnum_ccdc_archive 'CCDC 720265'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H53 B Cu F5 N7 O7'
_chemical_formula_weight         1021.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
B B -0.0010 0.0008
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N -0.0031 0.0040
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O -0.0041 0.0074
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
F F -0.0053 0.0125
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cu Cu 0.1330 1.4803
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.2815(8)
_cell_length_b                   14.9581(14)
_cell_length_c                   17.4574(16)
_cell_angle_alpha                95.741(2)
_cell_angle_beta                 92.388(2)
_cell_angle_gamma                104.621(2)
_cell_volume                     2327.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6736
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      29.59

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1062
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_process_details   'SADABS v2.10 Bruker AXS, Madison, WI, US'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            34376
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         33.67
_reflns_number_total             13933
_reflns_number_gt                10521
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_structure_solution    'SIR97 through WinGX'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'

_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.
All non-hydrogen were refinement anisotropically. Geometrical and
displacement parameter restrains were used to model the BF4 group.
Displacement parameter restrains were in modelling end of one of the
ligand arms, even so the ratio of the displacemeter max:min is around 5:1.
Splitting the end of the arm was considered but as it reflected the movement
in the arm and no new chemical information would be gained, it was decided
not to do anything more to it. Hydrogens were placed geometrically where
possible and refined with a riding model. In the Case of the N-H these were
found in the diffence map and these were allowed to refine with a restraint
on the N-H distance.
;

_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^)+(0.0763P)^2^+0.5471P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13933
_refine_ls_number_parameters     670
_refine_ls_number_restraints     309
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0566
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.102
_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 0.25995(3) 0.842420(18) 0.156740(15) 0.02850(9) Uani 1 1 d . . .
F1 F 0.30459(19) 0.76123(11) 0.21917(9) 0.0468(4) Uani 1 1 d . . .
N1 N 0.21435(19) 0.92603(12) 0.08175(10) 0.0253(3) Uani 1 1 d . . .
C1 C 0.0626(3) 0.93944(17) 0.09476(12) 0.0324(4) Uani 1 1 d . . .
H1A H -0.0146 0.8849 0.0696 0.039 Uiso 1 1 calc R . .
H1B H 0.0507 0.9952 0.0717 0.039 Uiso 1 1 calc R . .
C2 C 0.0431(3) 0.95130(18) 0.18079(13) 0.0354(5) Uani 1 1 d . . .
H2A H 0.1169 1.0077 0.2057 0.043 Uiso 1 1 calc R . .
H2B H -0.0582 0.9586 0.1897 0.043 Uiso 1 1 calc R . .
N2 N 0.0647(2) 0.86854(14) 0.21418(11) 0.0312(4) Uani 1 1 d D . .
C3 C 0.0784(2) 0.87313(17) 0.29724(12) 0.0324(4) Uani 1 1 d . . .
C4 C 0.1261(3) 0.95737(19) 0.34368(15) 0.0444(6) Uani 1 1 d . . .
H4A H 0.1429 1.0141 0.3213 0.053 Uiso 1 1 calc R . .
C5 C 0.1491(4) 0.9585(2) 0.42308(16) 0.0530(7) Uani 1 1 d . . .
H5A H 0.1806 1.0163 0.4548 0.064 Uiso 1 1 calc R . .
C6 C 0.1266(3) 0.8769(2) 0.45611(14) 0.0456(6) Uani 1 1 d . . .
H6A H 0.1450 0.8781 0.5102 0.055 Uiso 1 1 calc R . .
C7 C 0.0771(3) 0.79333(19) 0.41013(14) 0.0400(5) Uani 1 1 d . . .
H7A H 0.0610 0.7371 0.4332 0.048 Uiso 1 1 calc R . .
C8 C 0.0500(3) 0.78929(17) 0.33034(13) 0.0369(5) Uani 1 1 d . . .
C9 C -0.0119(4) 0.69837(19) 0.27983(15) 0.0529(8) Uani 1 1 d . . .
H9A H -0.1121 0.6974 0.2575 0.064 Uiso 1 1 calc R . .
H9B H 0.0531 0.6953 0.2366 0.064 Uiso 1 1 calc R . .
C10 C -0.0242(4) 0.6136(2) 0.32116(15) 0.0546(8) Uani 1 1 d . . .
C11 C -0.1550(4) 0.5753(2) 0.35560(18) 0.0616(9) Uani 1 1 d . . .
H11A H -0.2371 0.6023 0.3530 0.074 Uiso 1 1 calc R . .
C12 C -0.1637(5) 0.4964(2) 0.39408(18) 0.0693(11) Uani 1 1 d . . .
H12A H -0.2523 0.4686 0.4173 0.083 Uiso 1 1 calc R . .
C13 C -0.0414(5) 0.4598(2) 0.39776(16) 0.0617(9) Uani 1 1 d . . .
C14 C 0.0877(6) 0.4976(2) 0.3658(2) 0.0724(11) Uani 1 1 d . . .
H14A H 0.1712 0.4722 0.3705 0.087 Uiso 1 1 calc R . .
C15 C 0.0949(5) 0.5739(2) 0.32634(19) 0.0668(10) Uani 1 1 d . . .
H15A H 0.1834 0.5997 0.3022 0.080 Uiso 1 1 calc R . .
N5 N -0.0539(5) 0.3759(2) 0.43793(16) 0.0771(11) Uani 1 1 d . . .
O1 O 0.0609(5) 0.3500(2) 0.44870(18) 0.0999(11) Uani 1 1 d . . .
O2 O -0.1754(5) 0.3367(2) 0.45685(17) 0.0969(11) Uani 1 1 d . . .
C16 C 0.3281(3) 1.01773(15) 0.09426(13) 0.0342(5) Uani 1 1 d . . .
H16A H 0.2967 1.0592 0.1344 0.041 Uiso 1 1 calc R . .
H16B H 0.3350 1.0474 0.0459 0.041 Uiso 1 1 calc R . .
C17 C 0.4787(3) 1.00542(18) 0.11912(14) 0.0367(5) Uani 1 1 d . . .
H17A H 0.5200 0.9763 0.0747 0.044 Uiso 1 1 calc R . .
H17B H 0.5478 1.0671 0.1358 0.044 Uiso 1 1 calc R . .
N3 N 0.4691(2) 0.94653(14) 0.18340(11) 0.0325(4) Uani 1 1 d D . .
C18 C 0.4963(3) 0.99364(18) 0.26110(13) 0.0356(5) Uani 1 1 d . . .
C19 C 0.4652(3) 1.07965(18) 0.27749(16) 0.0470(6) Uani 1 1 d . . .
H19A H 0.4269 1.1073 0.2373 0.056 Uiso 1 1 calc R . .
C20 C 0.4897(4) 1.1255(2) 0.35195(17) 0.0594(9) Uani 1 1 d . . .
H20A H 0.4695 1.1845 0.3623 0.071 Uiso 1 1 calc R . .
C21 C 0.5432(4) 1.0851(2) 0.41075(17) 0.0590(8) Uani 1 1 d . . .
H21A H 0.5580 1.1154 0.4620 0.071 Uiso 1 1 calc R . .
C22 C 0.5750(3) 1.0004(2) 0.39460(16) 0.0506(7) Uani 1 1 d . . .
H22A H 0.6121 0.9731 0.4355 0.061 Uiso 1 1 calc R . .
C23 C 0.5545(3) 0.9531(2) 0.31997(14) 0.0408(5) Uani 1 1 d . . .
C24 C 0.6040(3) 0.8643(2) 0.30263(16) 0.0528(7) Uani 1 1 d U . .
H24A H 0.5374 0.8246 0.2598 0.063 Uiso 1 1 calc R . .
H24B H 0.7062 0.8806 0.2848 0.063 Uiso 1 1 calc R . .
C25 C 0.6033(3) 0.8090(2) 0.37037(16) 0.0515(7) Uani 1 1 d U . .
C26 C 0.7296(4) 0.8220(3) 0.42030(19) 0.0682(10) Uani 1 1 d U . .
H26A H 0.8192 0.8659 0.4113 0.082 Uiso 1 1 calc R . .
C27 C 0.7260(4) 0.7719(3) 0.4826(2) 0.0746(10) Uani 1 1 d U . .
H27A H 0.8111 0.7829 0.5178 0.089 Uiso 1 1 calc R . .
C28 C 0.5972(4) 0.7057(3) 0.49310(19) 0.0674(9) Uani 1 1 d U . .
C29 C 0.4695(5) 0.6911(3) 0.4459(2) 0.0690(9) Uani 1 1 d U . .
H29A H 0.3814 0.6457 0.4545 0.083 Uiso 1 1 calc R . .
C30 C 0.4732(4) 0.7447(3) 0.38500(19) 0.0615(8) Uani 1 1 d U . .
H30A H 0.3850 0.7373 0.3527 0.074 Uiso 1 1 calc R . .
N6 N 0.5929(5) 0.6498(4) 0.5586(2) 0.0863(11) Uani 1 1 d U . .
O3 O 0.5039(6) 0.5774(3) 0.5578(2) 0.1260(15) Uani 1 1 d U . .
O4 O 0.6781(4) 0.6884(3) 0.6170(2) 0.1218(13) Uani 1 1 d U . .
C31 C 0.2199(3) 0.87938(15) 0.00238(12) 0.0294(4) Uani 1 1 d . . .
H31A H 0.3252 0.8849 -0.0090 0.035 Uiso 1 1 calc R . .
H31B H 0.1751 0.9108 -0.0359 0.035 Uiso 1 1 calc R . .
C32 C 0.1359(3) 0.77727(15) -0.00454(12) 0.0313(4) Uani 1 1 d . . .
H32A H 0.0275 0.7713 -0.0024 0.038 Uiso 1 1 calc R . .
H32B H 0.1527 0.7454 -0.0546 0.038 Uiso 1 1 calc R . .
N4 N 0.1902(2) 0.73395(12) 0.05995(10) 0.0274(3) Uani 1 1 d D . .
C33 C 0.0961(2) 0.64755(14) 0.07854(12) 0.0266(4) Uani 1 1 d . . .
C34 C -0.0570(2) 0.63556(16) 0.08110(13) 0.0306(4) Uani 1 1 d . . .
H34A H -0.1007 0.6832 0.0672 0.037 Uiso 1 1 calc R . .
C35 C -0.1468(2) 0.55462(17) 0.10374(13) 0.0338(5) Uani 1 1 d . . .
H35A H -0.2511 0.5473 0.1060 0.041 Uiso 1 1 calc R . .
C36 C -0.0836(3) 0.48510(17) 0.12283(15) 0.0372(5) Uani 1 1 d . . .
H36A H -0.1446 0.4292 0.1376 0.045 Uiso 1 1 calc R . .
C37 C 0.0690(3) 0.49675(16) 0.12048(15) 0.0349(5) Uani 1 1 d . . .
H37A H 0.1113 0.4484 0.1339 0.042 Uiso 1 1 calc R . .
C38 C 0.1618(2) 0.57737(15) 0.09895(13) 0.0298(4) Uani 1 1 d . . .
C39 C 0.3293(3) 0.59258(17) 0.09767(16) 0.0374(5) Uani 1 1 d . . .
H39A H 0.3568 0.5981 0.0438 0.045 Uiso 1 1 calc R . .
H39B H 0.3781 0.6525 0.1287 0.045 Uiso 1 1 calc R . .
C40 C 0.3912(2) 0.51783(16) 0.12768(14) 0.0333(5) Uani 1 1 d . . .
C41 C 0.4029(3) 0.44116(17) 0.07878(15) 0.0359(5) Uani 1 1 d . . .
H41A H 0.3671 0.4346 0.0262 0.043 Uiso 1 1 calc R . .
C42 C 0.4653(3) 0.37411(17) 0.10485(16) 0.0386(5) Uani 1 1 d . . .
H42A H 0.4740 0.3223 0.0709 0.046 Uiso 1 1 calc R . .
C43 C 0.5145(3) 0.38475(17) 0.18171(16) 0.0376(5) Uani 1 1 d . . .
C44 C 0.5020(3) 0.4587(2) 0.23301(16) 0.0450(6) Uani 1 1 d . . .
H44A H 0.5345 0.4635 0.2860 0.054 Uiso 1 1 calc R . .
C45 C 0.4410(3) 0.52529(18) 0.20506(16) 0.0420(6) Uani 1 1 d . . .
H45A H 0.4329 0.5771 0.2392 0.050 Uiso 1 1 calc R . .
N7 N 0.5868(3) 0.31602(17) 0.20939(17) 0.0528(6) Uani 1 1 d . . .
O5 O 0.6276(3) 0.32377(18) 0.27717(17) 0.0776(8) Uani 1 1 d . . .
O6 O 0.6043(3) 0.25402(18) 0.16140(18) 0.0789(8) Uani 1 1 d . . .
B1 B 0.6713(6) 0.8164(4) 0.0678(3) 0.0431(16) Uani 0.50 1 d PDU A 1
F11 F 0.7064(6) 0.7695(4) 0.1274(3) 0.0735(13) Uani 0.50 1 d PDU A 1
F12 F 0.7222(5) 0.9110(3) 0.0932(3) 0.0507(10) Uani 0.50 1 d PDU A 1
B1' B 0.6645(6) 0.7977(5) 0.0660(3) 0.0454(17) Uani 0.50 1 d PDU A 2
F11' F 0.6557(5) 0.7153(4) 0.0953(3) 0.0773(14) Uani 0.50 1 d PDU A 2
F12' F 0.7140(5) 0.8710(4) 0.1213(3) 0.0771(15) Uani 0.50 1 d PDU A 2
F13 F 0.51969(16) 0.79590(11) 0.04268(11) 0.0509(4) Uani 1 1 d DU . .
F14 F 0.75293(17) 0.80058(13) 0.00526(10) 0.0534(4) Uani 1 1 d DU . .
O1S O 1.0103(3) 0.85758(15) 0.83641(13) 0.0577(5) Uani 1 1 d . . .
C1S C 0.8885(4) 0.7778(2) 0.8146(2) 0.0611(8) Uani 1 1 d . . .
H1SA H 0.8030 0.7959 0.7907 0.073 Uiso 1 1 calc R . .
H1SB H 0.8556 0.7454 0.8600 0.073 Uiso 1 1 calc R . .
C2S C 0.9483(5) 0.7170(3) 0.7576(3) 0.0842(13) Uani 1 1 d . . .
H2SA H 0.9992 0.6767 0.7840 0.101 Uiso 1 1 calc R . .
H2SB H 0.8677 0.6776 0.7209 0.101 Uiso 1 1 calc R . .
C3S C 1.0559(5) 0.7858(3) 0.7177(2) 0.0784(11) Uani 1 1 d . . .
H3SA H 1.1328 0.7583 0.6947 0.094 Uiso 1 1 calc R . .
H3SB H 1.0042 0.8101 0.6770 0.094 Uiso 1 1 calc R . .
C4S C 1.1215(4) 0.8591(2) 0.7819(2) 0.0636(9) Uani 1 1 d . . .
H4SA H 1.2116 0.8468 0.8064 0.076 Uiso 1 1 calc R . .
H4SB H 1.1502 0.9207 0.7624 0.076 Uiso 1 1 calc R . .
H4N H 0.2784(16) 0.7282(19) 0.0484(15) 0.033(7) Uiso 1 1 d D . .
H3N H 0.533(3) 0.9128(18) 0.1806(18) 0.048(9) Uiso 1 1 d D . .
H2N H -0.009(2) 0.8215(15) 0.1962(18) 0.050(9) Uiso 1 1 d D . .

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 0.03334(15) 0.02900(14) 0.02551(14) 0.00918(10) -0.00317(10) 0.01088(10)
F1 0.0649(10) 0.0400(8) 0.0389(8) 0.0151(6) -0.0128(7) 0.0186(7)
N1 0.0288(8) 0.0274(8) 0.0218(8) 0.0067(6) 0.0010(6) 0.0100(7)
C1 0.0348(11) 0.0423(12) 0.0270(10) 0.0089(9) 0.0014(8) 0.0209(9)
C2 0.0391(12) 0.0470(13) 0.0278(10) 0.0084(9) 0.0054(9) 0.0228(10)
N2 0.0341(10) 0.0344(10) 0.0248(9) 0.0071(7) 0.0022(7) 0.0068(8)
C3 0.0301(10) 0.0424(12) 0.0236(10) 0.0045(8) 0.0023(8) 0.0071(9)
C4 0.0581(16) 0.0409(13) 0.0304(12) 0.0054(10) 0.0017(11) 0.0054(12)
C5 0.072(2) 0.0470(15) 0.0313(13) -0.0010(11) -0.0066(12) 0.0029(14)
C6 0.0503(15) 0.0542(16) 0.0249(11) 0.0050(10) -0.0032(10) 0.0006(12)
C7 0.0427(13) 0.0467(14) 0.0284(11) 0.0113(10) 0.0014(9) 0.0048(11)
C8 0.0418(13) 0.0401(12) 0.0250(10) 0.0059(9) 0.0028(9) 0.0027(10)
C9 0.081(2) 0.0400(14) 0.0273(12) 0.0087(10) 0.0026(12) -0.0053(13)
C10 0.092(2) 0.0384(14) 0.0241(11) 0.0060(10) 0.0026(13) -0.0011(14)
C11 0.082(2) 0.0495(17) 0.0427(16) 0.0155(13) -0.0017(15) -0.0056(15)
C12 0.101(3) 0.0527(18) 0.0370(15) 0.0150(13) -0.0015(16) -0.0147(18)
C13 0.113(3) 0.0405(15) 0.0292(13) 0.0060(11) 0.0036(15) 0.0135(17)
C14 0.123(3) 0.0524(18) 0.0432(17) 0.0022(14) 0.0151(19) 0.025(2)
C15 0.105(3) 0.0531(18) 0.0410(16) 0.0051(13) 0.0221(17) 0.0162(19)
N5 0.147(4) 0.0489(16) 0.0327(13) 0.0071(11) 0.0085(17) 0.020(2)
O1 0.175(4) 0.077(2) 0.0641(18) 0.0211(15) 0.011(2) 0.059(2)
O2 0.158(3) 0.0623(16) 0.0638(17) 0.0305(14) 0.0143(19) 0.0061(18)
C16 0.0437(12) 0.0272(10) 0.0309(11) 0.0092(8) 0.0050(9) 0.0051(9)
C17 0.0353(12) 0.0411(12) 0.0295(11) 0.0057(9) 0.0050(9) 0.0013(10)
N3 0.0305(9) 0.0420(11) 0.0250(9) 0.0044(8) 0.0008(7) 0.0092(8)
C18 0.0305(11) 0.0428(12) 0.0279(11) 0.0023(9) 0.0005(8) 0.0000(9)
C19 0.0635(17) 0.0364(13) 0.0343(13) 0.0040(10) 0.0021(12) 0.0006(12)
C20 0.092(2) 0.0386(14) 0.0380(14) -0.0013(11) 0.0043(15) 0.0020(15)
C21 0.078(2) 0.0549(17) 0.0314(13) -0.0049(12) -0.0044(14) -0.0004(16)
C22 0.0508(16) 0.0654(18) 0.0300(12) 0.0006(12) -0.0079(11) 0.0082(13)
C23 0.0320(12) 0.0574(15) 0.0308(11) 0.0040(11) -0.0039(9) 0.0087(11)
C24 0.0524(16) 0.086(2) 0.0308(12) 0.0060(13) -0.0045(11) 0.0389(16)
C25 0.0519(15) 0.082(2) 0.0325(12) 0.0066(13) -0.0018(11) 0.0400(15)
C26 0.0473(16) 0.121(3) 0.0485(17) 0.0272(18) -0.0017(13) 0.0382(18)
C27 0.0576(18) 0.130(3) 0.0531(17) 0.0328(18) 0.0001(14) 0.0468(19)
C28 0.075(2) 0.106(3) 0.0460(16) 0.0262(17) 0.0132(15) 0.061(2)
C29 0.071(2) 0.083(2) 0.0573(19) 0.0110(17) -0.0009(16) 0.0278(19)
C30 0.0624(19) 0.077(2) 0.0507(17) 0.0060(15) -0.0113(14) 0.0302(17)
N6 0.090(2) 0.141(3) 0.0597(19) 0.042(2) 0.0191(17) 0.073(2)
O3 0.198(5) 0.109(3) 0.094(3) 0.048(2) 0.021(3) 0.067(3)
O4 0.099(2) 0.208(4) 0.077(2) 0.070(2) 0.0075(17) 0.054(2)
C31 0.0363(11) 0.0335(10) 0.0221(9) 0.0089(8) 0.0030(8) 0.0136(9)
C32 0.0392(12) 0.0320(10) 0.0245(10) 0.0047(8) -0.0042(8) 0.0130(9)
N4 0.0295(9) 0.0279(8) 0.0287(9) 0.0087(7) 0.0009(7) 0.0128(7)
C33 0.0293(10) 0.0268(9) 0.0254(9) 0.0034(7) 0.0008(7) 0.0104(8)
C34 0.0307(10) 0.0353(11) 0.0292(10) 0.0049(8) 0.0006(8) 0.0145(9)
C35 0.0269(10) 0.0394(12) 0.0347(11) 0.0043(9) -0.0004(8) 0.0083(9)
C36 0.0318(11) 0.0342(11) 0.0448(13) 0.0083(10) 0.0041(9) 0.0054(9)
C37 0.0356(11) 0.0291(10) 0.0437(13) 0.0100(9) 0.0052(9) 0.0126(9)
C38 0.0297(10) 0.0293(10) 0.0339(11) 0.0066(8) 0.0031(8) 0.0126(8)
C39 0.0299(11) 0.0354(12) 0.0538(15) 0.0169(10) 0.0067(10) 0.0157(9)
C40 0.0281(10) 0.0322(11) 0.0441(13) 0.0119(9) 0.0032(9) 0.0131(8)
C41 0.0333(11) 0.0382(12) 0.0394(12) 0.0090(10) -0.0010(9) 0.0141(9)
C42 0.0381(12) 0.0308(11) 0.0501(14) 0.0068(10) 0.0025(10) 0.0137(9)
C43 0.0304(11) 0.0336(11) 0.0538(15) 0.0188(10) -0.0001(10) 0.0125(9)
C44 0.0489(15) 0.0487(15) 0.0405(14) 0.0124(11) -0.0033(11) 0.0163(12)
C45 0.0475(14) 0.0381(12) 0.0441(14) 0.0044(10) 0.0015(11) 0.0183(11)
N7 0.0452(13) 0.0427(13) 0.0777(18) 0.0291(13) 0.0009(12) 0.0161(10)
O5 0.0836(18) 0.0715(16) 0.0874(19) 0.0364(14) -0.0214(14) 0.0319(14)
O6 0.101(2) 0.0630(15) 0.098(2) 0.0320(15) 0.0155(16) 0.0572(15)
B1 0.041(3) 0.052(3) 0.046(3) 0.012(3) 0.008(3) 0.026(3)
F11 0.096(4) 0.089(3) 0.059(3) 0.034(2) 0.016(2) 0.055(3)
F12 0.0362(18) 0.052(2) 0.065(3) -0.0046(18) -0.0070(18) 0.0181(16)
B1' 0.034(3) 0.060(3) 0.051(3) 0.009(3) 0.009(3) 0.026(3)
F11' 0.050(2) 0.093(3) 0.111(4) 0.059(3) 0.020(2) 0.039(2)
F12' 0.041(2) 0.114(4) 0.068(3) -0.031(3) 0.003(2) 0.020(3)
F13 0.0288(7) 0.0462(9) 0.0796(12) 0.0073(8) 0.0084(7) 0.0123(6)
F14 0.0354(8) 0.0765(12) 0.0472(9) -0.0012(8) 0.0079(7) 0.0150(8)
O1S 0.0655(14) 0.0496(12) 0.0527(12) -0.0035(10) -0.0024(10) 0.0099(10)
C1S 0.0603(19) 0.0537(18) 0.066(2) 0.0060(15) -0.0058(16) 0.0106(15)
C2S 0.097(3) 0.060(2) 0.091(3) -0.007(2) -0.018(3) 0.021(2)
C3S 0.088(3) 0.097(3) 0.055(2) -0.005(2) -0.0024(19) 0.039(2)
C4S 0.0592(19) 0.0553(19) 0.080(2) -0.0002(17) 0.0076(17) 0.0235(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 F1 1.8208(14) . ?
Cu1 N1 2.0014(17) . ?
Cu1 N2 2.207(2) . ?
Cu1 N3 2.160(2) . ?
Cu1 N4 2.1764(19) . ?
N1 C1 1.495(3) . ?
N1 C16 1.494(3) . ?
N1 C31 1.497(3) . ?
C1 C2 1.519(3) . ?
C2 N2 1.474(3) . ?
N2 C3 1.443(3) . ?
C3 C4 1.387(3) . ?
C3 C8 1.403(3) . ?
C4 C5 1.391(4) . ?
C5 C6 1.374(4) . ?
C6 C7 1.377(4) . ?
C7 C8 1.398(3) . ?
C8 C9 1.510(4) . ?
C9 C10 1.503(4) . ?
C10 C11 1.393(5) . ?
C10 C15 1.385(5) . ?
C11 C12 1.402(4) . ?
C12 C13 1.381(6) . ?
C13 C14 1.359(5) . ?
C13 N5 1.479(4) . ?
C14 C15 1.379(5) . ?
N5 O1 1.236(5) . ?
N5 O2 1.209(5) . ?
C16 C17 1.508(4) . ?
C17 N3 1.486(3) . ?
N3 C18 1.446(3) . ?
C18 C19 1.393(4) . ?
C18 C23 1.400(4) . ?
C19 C20 1.389(4) . ?
C20 C21 1.378(5) . ?
C21 C22 1.377(5) . ?
C22 C23 1.400(4) . ?
C23 C24 1.518(4) . ?
C24 C25 1.509(4) . ?
C25 C26 1.392(4) . ?
C25 C30 1.392(5) . ?
C26 C27 1.377(5) . ?
C27 C28 1.379(6) . ?
C28 C29 1.372(5) . ?
C28 N6 1.478(5) . ?
C29 C30 1.390(5) . ?
N6 O3 1.183(6) . ?
N6 O4 1.258(6) . ?
C31 C32 1.520(3) . ?
C32 N4 1.485(3) . ?
N4 C33 1.441(3) . ?
C33 C34 1.390(3) . ?
C33 C38 1.408(3) . ?
C34 C35 1.389(3) . ?
C35 C36 1.378(3) . ?
C36 C37 1.385(3) . ?
C37 C38 1.390(3) . ?
C38 C39 1.514(3) . ?
C39 C40 1.507(3) . ?
C40 C41 1.389(3) . ?
C40 C45 1.394(4) . ?
C41 C42 1.383(3) . ?
C42 C43 1.380(4) . ?
C43 C44 1.383(4) . ?
C43 N7 1.470(3) . ?
C44 C45 1.382(4) . ?
N7 O5 1.213(4) . ?
N7 O6 1.233(4) . ?
B1 F11 1.384(6) . ?
B1 F12 1.393(6) . ?
B1 F13 1.403(6) . ?
B1 F14 1.389(6) . ?
B1' F11' 1.367(6) . ?
B1' F12' 1.358(6) . ?
B1' F13 1.380(6) . ?
B1' F14 1.365(6) . ?
O1S C1S 1.428(4) . ?
O1S C4S 1.431(4) . ?
C1S C2S 1.499(6) . ?
C2S C3S 1.491(6) . ?
C3S C4S 1.479(5) . ?

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
F1 Cu1 N1 175.92(7) . . ?
F1 Cu1 N2 98.36(8) . . ?
F1 Cu1 N3 95.20(8) . . ?
F1 Cu1 N4 91.99(7) . . ?
N1 Cu1 N2 84.79(7) . . ?
N1 Cu1 N3 85.62(7) . . ?
N1 Cu1 N4 84.45(7) . . ?
N2 Cu1 N3 116.71(7) . . ?
N2 Cu1 N4 110.80(7) . . ?
N3 Cu1 N4 130.16(7) . . ?
Cu1 N1 C1 108.32(12) . . ?
Cu1 N1 C16 109.74(13) . . ?
Cu1 N1 C31 107.26(12) . . ?
C1 N1 C16 109.89(17) . . ?
C1 N1 C31 111.39(16) . . ?
C16 N1 C31 110.18(16) . . ?
N1 C1 C2 109.58(17) . . ?
C1 C2 N2 108.79(19) . . ?
Cu1 N2 C2 102.65(13) . . ?
Cu1 N2 C3 114.26(14) . . ?
C2 N2 C3 117.49(19) . . ?
N2 C3 C4 121.7(2) . . ?
N2 C3 C8 118.1(2) . . ?
C4 C3 C8 120.1(2) . . ?
C3 C4 C5 119.9(3) . . ?
C4 C5 C6 120.7(3) . . ?
C5 C6 C7 119.4(2) . . ?
C6 C7 C8 121.6(2) . . ?
C3 C8 C7 118.2(2) . . ?
C3 C8 C9 119.6(2) . . ?
C7 C8 C9 122.1(2) . . ?
C8 C9 C10 114.2(2) . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 C15 120.3(3) . . ?
C11 C10 C15 119.6(3) . . ?
C10 C11 C12 119.1(4) . . ?
C11 C12 C13 119.0(3) . . ?
C12 C13 C14 122.4(3) . . ?
C12 C13 N5 118.0(4) . . ?
C14 C13 N5 119.6(4) . . ?
C13 C14 C15 118.5(4) . . ?
C10 C15 C14 121.4(4) . . ?
C13 N5 O1 117.4(4) . . ?
C13 N5 O2 118.1(4) . . ?
O1 N5 O2 124.5(4) . . ?
N1 C16 C17 110.67(18) . . ?
C16 C17 N3 111.63(18) . . ?
Cu1 N3 C17 104.04(14) . . ?
Cu1 N3 C18 116.95(14) . . ?
C17 N3 C18 117.3(2) . . ?
N3 C18 C19 120.1(2) . . ?
N3 C18 C23 120.1(2) . . ?
C19 C18 C23 119.8(2) . . ?
C18 C19 C20 120.8(3) . . ?
C19 C20 C21 119.9(3) . . ?
C20 C21 C22 119.5(3) . . ?
C21 C22 C23 122.2(3) . . ?
C18 C23 C22 117.8(3) . . ?
C18 C23 C24 121.1(2) . . ?
C22 C23 C24 120.9(2) . . ?
C23 C24 C25 114.3(2) . . ?
C24 C25 C26 121.5(3) . . ?
C24 C25 C30 119.9(3) . . ?
C26 C25 C30 118.6(3) . . ?
C25 C26 C27 120.6(4) . . ?
C26 C27 C28 119.1(3) . . ?
C27 C28 C29 122.2(3) . . ?
C27 C28 N6 119.7(3) . . ?
C29 C28 N6 118.1(4) . . ?
C28 C29 C30 118.0(4) . . ?
C25 C30 C29 121.4(3) . . ?
C28 N6 O3 120.9(4) . . ?
C28 N6 O4 115.8(5) . . ?
O3 N6 O4 122.9(4) . . ?
N1 C31 C32 110.87(17) . . ?
C31 C32 N4 108.89(17) . . ?
Cu1 N4 C32 106.86(13) . . ?
Cu1 N4 C33 115.02(13) . . ?
C32 N4 C33 117.38(17) . . ?
N4 C33 C34 120.54(18) . . ?
N4 C33 C38 119.24(18) . . ?
C34 C33 C38 120.1(2) . . ?
C33 C34 C35 120.6(2) . . ?
C34 C35 C36 119.6(2) . . ?
C35 C36 C37 120.0(2) . . ?
C36 C37 C38 121.7(2) . . ?
C33 C38 C37 118.0(2) . . ?
C33 C38 C39 119.38(19) . . ?
C37 C38 C39 122.66(19) . . ?
C38 C39 C40 115.56(19) . . ?
C39 C40 C41 121.0(2) . . ?
C39 C40 C45 120.5(2) . . ?
C41 C40 C45 118.5(2) . . ?
C40 C41 C42 121.5(2) . . ?
C41 C42 C43 118.0(2) . . ?
C42 C43 C44 122.6(2) . . ?
C42 C43 N7 118.5(2) . . ?
C44 C43 N7 118.9(2) . . ?
C43 C44 C45 118.1(2) . . ?
C40 C45 C44 121.2(2) . . ?
C43 N7 O5 118.9(3) . . ?
C43 N7 O6 117.5(3) . . ?
O5 N7 O6 123.6(3) . . ?
F11 B1 F12 106.6(5) . . ?
F11 B1 F13 116.1(5) . . ?
F11 B1 F14 109.4(4) . . ?
F12 B1 F13 109.2(4) . . ?
F12 B1 F14 105.9(4) . . ?
F13 B1 F14 109.0(4) . . ?
F11' B1' F12' 111.3(6) . . ?
F11' B1' F13 105.5(4) . . ?
F11' B1' F14 107.4(5) . . ?
F12' B1' F13 107.3(5) . . ?
F12' B1' F14 113.3(5) . . ?
F13 B1' F14 111.8(4) . . ?
B1 F13 B1' 11.0(4) . . ?
B1 F14 B1' 11.1(4) . . ?
C1S O1S C4S 108.7(2) . . ?
O1S C1S C2S 105.0(3) . . ?
C1S C2S C3S 102.7(3) . . ?
C2S C3S C4S 101.9(3) . . ?
O1S C4S C3S 107.1(3) . . ?

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
N4 H4N F13 0.874(10) 2.224(17) 3.000(2) 148(2) .
N3 H3N F12' 0.872(10) 2.196(19) 2.979(5) 149(3) .
N3 H3N F12 0.872(10) 2.38(3) 3.008(5) 130(3) .

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.071