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

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Masahiko Maekawa'
_publ_contact_author_email       MAEKAWA@RIST.KINDAI.AC.JP

_publ_section_title              
;
A unique chair-shaped hexanuclear Cu(I)
metallamacrocyclic C2H4 adduct encapsulating a BF4- anion
;
loop_
_publ_author_name
'Masahiko Maekawa'
'Susumu Kitagawa'
'T Kuroda-Sowa'
'Toshie Minemastu'
'M Munakata'
;
A.Nabei
;
'Takashi Okubo'
'Kunihisa Sugimoto'
'Toshi Tominaga'

# Attachment 'revised_cifs3-B812337C.cif'

#------------------------------------------------------------------------------
data_[Cu2(pprd)(C2H4)2(NO3)]NO3 #(complex-1) CCDC-695266
_database_code_depnum_ccdc_archive 'CCDC 695266'
#------------------------------------------------------------------------------

# CHEMICAL DATA

_chemical_formula_sum            'C13 H15 Cu2 N5 O6 '
_chemical_formula_moiety         'C13 H15 Cu2 N5 O6 '
_chemical_formula_weight         464.38
_chemical_melting_point          ?

#------------------------------------------------------------------------------

# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14

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

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

_cell_length_a                   13.7587(11)
_cell_length_b                   8.1512(6)
_cell_length_c                   15.7527(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.603(2)
_cell_angle_gamma                90.00
_cell_volume                     1724.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3689
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       platelet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.62
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22732
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         31.70
_reflns_number_total             5351
_reflns_number_gt                3065
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'CrystalStructure 3.8'
_computing_molecular_graphics    ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+5.3342P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5351
_refine_ls_number_parameters     282
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.1333
_refine_ls_wR_factor_gt          0.1075
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.064
_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 0.32057(4) 0.10280(7) 0.40258(4) 0.02648(15) Uani 1 1 d . . .
Cu2 Cu 0.58434(6) 0.29305(9) 0.16687(4) 0.0504(2) Uani 1 1 d . . .
O1 O 0.2913(2) 0.3889(4) 0.4161(2) 0.0394(9) Uani 1 1 d . . .
O2 O 0.1412(2) 0.3882(4) 0.3369(2) 0.0401(9) Uani 1 1 d . . .
O3 O 0.2147(3) 0.6179(4) 0.3798(2) 0.0417(9) Uani 1 1 d . . .
O4 O 0.705(2) 0.531(5) 0.1963(18) 0.067(7) Uani 0.42(5) 1 d PDU A 1
O5 O 0.654(2) 0.753(3) 0.1276(12) 0.057(6) Uani 0.42(5) 1 d PDU A 1
O6 O 0.552(2) 0.549(5) 0.125(4) 0.051(6) Uani 0.42(5) 1 d PDU A 1
N5 N 0.6356(19) 0.616(4) 0.152(3) 0.037(4) Uani 0.42(5) 1 d PDU A 1
O7 O 0.6956(12) 0.466(2) 0.1963(10) 0.043(3) Uani 0.58(5) 1 d PDU A 2
O8 O 0.699(2) 0.719(2) 0.160(3) 0.091(7) Uani 0.58(5) 1 d PDU A 2
O9 O 0.5580(18) 0.588(4) 0.136(3) 0.049(5) Uani 0.58(5) 1 d PDU A 2
N6 N 0.6522(17) 0.592(3) 0.160(3) 0.049(4) Uani 0.58(5) 1 d PDU A 2
N1 N 0.3968(3) 0.1388(4) 0.5252(2) 0.0250(8) Uani 1 1 d . . .
N2 N 0.4486(3) 0.1849(4) 0.3748(2) 0.0236(8) Uani 1 1 d . A .
N3 N 0.5515(3) 0.2809(5) 0.2836(2) 0.0309(9) Uani 1 1 d . A .
N4 N 0.2145(3) 0.4636(5) 0.3778(2) 0.0277(8) Uani 1 1 d . . .
C1 C 0.2183(3) -0.0043(6) 0.3094(3) 0.0307(11) Uani 1 1 d . . .
H1 H 0.1820 0.0679 0.2626 0.037 Uiso 1 1 calc R . .
H2 H 0.2363 -0.1122 0.2883 0.037 Uiso 1 1 calc R . .
C2 C 0.1865(3) -0.0040(6) 0.3857(3) 0.0304(10) Uani 1 1 d . . .
H3 H 0.1839 -0.1117 0.4143 0.036 Uiso 1 1 calc R . .
H4 H 0.1296 0.0685 0.3885 0.036 Uiso 1 1 calc R . .
C3 C 0.3637(3) 0.1135(6) 0.5976(3) 0.0285(10) Uani 1 1 d . . .
H5 H 0.3040 0.0528 0.5940 0.034 Uiso 1 1 calc R . .
C4 C 0.4130(4) 0.1723(6) 0.6773(3) 0.0341(11) Uani 1 1 d . . .
H6 H 0.3876 0.1527 0.7279 0.041 Uiso 1 1 calc R . .
C5 C 0.5003(4) 0.2604(6) 0.6825(3) 0.0347(12) Uani 1 1 d . . .
H7 H 0.5351 0.3032 0.7368 0.042 Uiso 1 1 calc R . .
C6 C 0.5363(3) 0.2858(6) 0.6077(3) 0.0288(10) Uani 1 1 d . . .
H8 H 0.5966 0.3441 0.6098 0.035 Uiso 1 1 calc R . .
C7 C 0.4815(3) 0.2234(5) 0.5298(3) 0.0232(9) Uani 1 1 d . . .
C8 C 0.5116(3) 0.2476(5) 0.4456(3) 0.0219(9) Uani 1 1 d . . .
C9 C 0.4717(3) 0.2028(5) 0.2978(3) 0.0259(10) Uani 1 1 d . . .
H9 H 0.4276 0.1561 0.2489 0.031 Uiso 1 1 calc R A .
C10 C 0.6144(3) 0.3427(6) 0.3546(3) 0.0317(11) Uani 1 1 d . . .
H10 H 0.6727 0.3982 0.3472 0.038 Uiso 1 1 calc R A .
C11 C 0.5971(3) 0.3282(6) 0.4369(3) 0.0289(10) Uani 1 1 d . A .
H11 H 0.6423 0.3720 0.4860 0.035 Uiso 1 1 calc R . .
C12 C 0.5914(5) 0.1974(7) 0.0514(4) 0.0514(15) Uani 1 1 d . A .
H12 H 0.5328 0.2133 0.0030 0.062 Uiso 0.46(3) 1 calc PR B 3
H13 H 0.6562 0.2042 0.0339 0.062 Uiso 0.46(3) 1 calc PR B 3
H16 H 0.5608 0.2624 -0.0007 0.062 Uiso 0.54(3) 1 calc PR B 4
H17 H 0.6550 0.1446 0.0473 0.062 Uiso 0.54(3) 1 calc PR B 4
C13 C 0.583(2) 0.085(2) 0.1122(14) 0.054(6) Uani 0.46(3) 1 d P A 3
H14 H 0.6422 0.0149 0.1331 0.065 Uiso 0.46(3) 1 calc PR B 3
H15 H 0.5196 0.0239 0.1023 0.065 Uiso 0.46(3) 1 calc PR B 3
C14 C 0.5265(17) 0.105(2) 0.0894(9) 0.045(5) Uani 0.54(3) 1 d P A 4
H18 H 0.5490 -0.0069 0.1097 0.054 Uiso 0.54(3) 1 calc PR B 4
H19 H 0.4548 0.1111 0.0617 0.054 Uiso 0.54(3) 1 calc PR B 4

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 0.0228(3) 0.0289(3) 0.0267(3) -0.0012(3) 0.0033(2) -0.0033(2)
Cu2 0.0670(5) 0.0532(5) 0.0393(4) -0.0142(3) 0.0297(3) -0.0261(4)
O1 0.0326(18) 0.0267(18) 0.050(2) -0.0027(16) -0.0113(16) 0.0080(16)
O2 0.0322(18) 0.0315(19) 0.047(2) -0.0035(17) -0.0113(16) -0.0058(16)
O3 0.046(2) 0.0163(18) 0.056(2) -0.0012(16) -0.0040(17) 0.0031(16)
O4 0.051(9) 0.080(16) 0.075(11) 0.018(11) 0.025(8) 0.038(11)
O5 0.051(11) 0.050(8) 0.075(10) 0.011(6) 0.022(8) -0.015(7)
O6 0.044(7) 0.044(14) 0.066(12) -0.009(12) 0.016(6) -0.009(7)
N5 0.027(7) 0.036(8) 0.054(10) -0.007(7) 0.021(7) 0.010(6)
O7 0.042(4) 0.053(7) 0.036(5) 0.001(5) 0.012(3) -0.006(5)
O8 0.067(11) 0.048(6) 0.178(18) -0.007(8) 0.071(13) -0.021(7)
O9 0.039(7) 0.044(11) 0.070(13) -0.001(10) 0.023(7) 0.005(5)
N6 0.043(8) 0.042(8) 0.076(11) -0.008(7) 0.040(8) -0.006(7)
N1 0.0207(18) 0.027(2) 0.0268(19) 0.0018(16) 0.0040(15) 0.0049(16)
N2 0.0212(18) 0.025(2) 0.0229(18) -0.0014(16) 0.0017(15) 0.0023(15)
N3 0.029(2) 0.037(2) 0.028(2) -0.0028(18) 0.0099(17) -0.0079(18)
N4 0.029(2) 0.027(2) 0.0248(19) 0.0009(17) 0.0017(16) -0.0001(17)
C1 0.024(2) 0.029(3) 0.035(3) -0.007(2) -0.005(2) -0.001(2)
C2 0.024(2) 0.023(2) 0.043(3) -0.004(2) 0.006(2) -0.0055(19)
C3 0.025(2) 0.030(3) 0.031(2) 0.008(2) 0.0078(19) 0.006(2)
C4 0.039(3) 0.041(3) 0.023(2) 0.007(2) 0.007(2) 0.011(2)
C5 0.034(3) 0.041(3) 0.026(2) -0.003(2) -0.002(2) 0.002(2)
C6 0.025(2) 0.030(3) 0.029(2) 0.004(2) -0.0007(19) 0.001(2)
C7 0.023(2) 0.020(2) 0.025(2) 0.0029(18) 0.0035(18) 0.0063(18)
C8 0.020(2) 0.017(2) 0.027(2) -0.0002(18) -0.0004(17) 0.0062(17)
C9 0.027(2) 0.026(2) 0.024(2) -0.0051(19) 0.0040(18) -0.001(2)
C10 0.023(2) 0.038(3) 0.036(3) -0.003(2) 0.010(2) -0.006(2)
C11 0.022(2) 0.033(3) 0.029(2) -0.004(2) 0.0002(19) -0.006(2)
C12 0.070(4) 0.054(4) 0.035(3) -0.013(3) 0.022(3) -0.009(3)
C13 0.069(14) 0.045(9) 0.050(10) -0.027(8) 0.018(10) -0.007(10)
C14 0.060(10) 0.045(8) 0.028(6) -0.017(6) 0.005(6) -0.036(8)

_geom_special_details            
;
The disordered nitrate was restrained as the ideal bond lengths and
angles using the DFIX and DANG commands on SHELXL-97.
The disordered nitrate lead to the short O8...C10 contact.
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 C1 1.999(4) . ?
Cu1 C2 2.004(4) . ?
Cu1 N1 2.009(4) . ?
Cu1 N2 2.020(4) . ?
Cu1 O1 2.384(3) . ?
Cu2 C13 1.899(17) . ?
Cu2 N3 1.990(4) . ?
Cu2 C12 2.001(5) . ?
Cu2 C14 2.014(11) . ?
Cu2 O7 2.059(16) . ?
Cu2 O6 2.21(5) . ?
O1 N4 1.254(4) . ?
O2 N4 1.235(4) . ?
O3 N4 1.258(5) . ?
O4 N5 1.256(16) . ?
O5 N5 1.223(16) . ?
O6 N5 1.256(17) . ?
O7 N6 1.257(13) . ?
O8 N6 1.222(14) . ?
O9 N6 1.270(15) . ?
N1 C3 1.332(5) . ?
N1 C7 1.343(5) . ?
N2 C9 1.328(5) . ?
N2 C8 1.354(5) . ?
N3 C9 1.329(5) . ?
N3 C10 1.354(6) . ?
C1 C2 1.366(6) . ?
C1 H1 0.9900 . ?
C1 H2 0.9900 . ?
C2 H3 0.9900 . ?
C2 H4 0.9900 . ?
C3 C4 1.377(6) . ?
C3 H5 0.9500 . ?
C4 C5 1.386(7) . ?
C4 H6 0.9500 . ?
C5 C6 1.390(6) . ?
C5 H7 0.9500 . ?
C6 C7 1.389(6) . ?
C6 H8 0.9500 . ?
C7 C8 1.486(6) . ?
C8 C11 1.381(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(6) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.346(19) . ?
C12 C14 1.401(14) . ?
C12 H12 0.9900 . ?
C12 H13 0.9900 . ?
C12 H16 0.9900 . ?
C12 H17 0.9900 . ?
C13 H14 0.9900 . ?
C13 H15 0.9900 . ?
C14 H18 0.9900 . ?
C14 H19 0.9900 . ?

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
C1 Cu1 C2 39.91(18) . . ?
C1 Cu1 N1 155.00(18) . . ?
C2 Cu1 N1 117.60(17) . . ?
C1 Cu1 N2 119.54(17) . . ?
C2 Cu1 N2 159.43(17) . . ?
N1 Cu1 N2 82.12(14) . . ?
C1 Cu1 O1 112.79(16) . . ?
C2 Cu1 O1 105.57(16) . . ?
N1 Cu1 O1 80.46(13) . . ?
N2 Cu1 O1 82.38(13) . . ?
C13 Cu2 N3 113.2(6) . . ?
C13 Cu2 C12 40.3(6) . . ?
N3 Cu2 C12 152.5(2) . . ?
C13 Cu2 C14 23.3(6) . . ?
N3 Cu2 C14 112.5(4) . . ?
C12 Cu2 C14 40.8(4) . . ?
C13 Cu2 O7 130.2(11) . . ?
N3 Cu2 O7 97.7(5) . . ?
C12 Cu2 O7 106.9(5) . . ?
C14 Cu2 O7 146.6(7) . . ?
C13 Cu2 O6 136.7(17) . . ?
N3 Cu2 O6 104.6(16) . . ?
C12 Cu2 O6 98.3(16) . . ?
C14 Cu2 O6 121.0(14) . . ?
O7 Cu2 O6 60.5(10) . . ?
N4 O1 Cu1 125.0(3) . . ?
N5 O6 Cu2 102(3) . . ?
O5 N5 O6 121(3) . . ?
O5 N5 O4 120(2) . . ?
O6 N5 O4 118(3) . . ?
N6 O7 Cu2 101.5(11) . . ?
O8 N6 O7 119.7(15) . . ?
O8 N6 O9 121.4(17) . . ?
O7 N6 O9 118(2) . . ?
C3 N1 C7 119.3(4) . . ?
C3 N1 Cu1 126.6(3) . . ?
C7 N1 Cu1 113.0(3) . . ?
C9 N2 C8 118.3(4) . . ?
C9 N2 Cu1 128.9(3) . . ?
C8 N2 Cu1 112.2(3) . . ?
C9 N3 C10 116.3(4) . . ?
C9 N3 Cu2 122.8(3) . . ?
C10 N3 Cu2 120.8(3) . . ?
O2 N4 O1 121.0(4) . . ?
O2 N4 O3 120.5(4) . . ?
O1 N4 O3 118.5(4) . . ?
C2 C1 Cu1 70.3(3) . . ?
C2 C1 H1 116.6 . . ?
Cu1 C1 H1 116.6 . . ?
C2 C1 H2 116.6 . . ?
Cu1 C1 H2 116.6 . . ?
H1 C1 H2 113.6 . . ?
C1 C2 Cu1 69.8(3) . . ?
C1 C2 H3 116.7 . . ?
Cu1 C2 H3 116.7 . . ?
C1 C2 H4 116.7 . . ?
Cu1 C2 H4 116.7 . . ?
H3 C2 H4 113.7 . . ?
N1 C3 C4 122.3(4) . . ?
N1 C3 H5 118.9 . . ?
C4 C3 H5 118.9 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H6 120.6 . . ?
C5 C4 H6 120.6 . . ?
C4 C5 C6 119.4(4) . . ?
C4 C5 H7 120.3 . . ?
C6 C5 H7 120.3 . . ?
C7 C6 C5 118.0(4) . . ?
C7 C6 H8 121.0 . . ?
C5 C6 H8 121.0 . . ?
N1 C7 C6 122.2(4) . . ?
N1 C7 C8 115.3(4) . . ?
C6 C7 C8 122.5(4) . . ?
N2 C8 C11 120.3(4) . . ?
N2 C8 C7 115.6(4) . . ?
C11 C8 C7 124.1(4) . . ?
N2 C9 N3 125.2(4) . . ?
N2 C9 H9 117.4 . . ?
N3 C9 H9 117.4 . . ?
N3 C10 C11 122.5(4) . . ?
N3 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C8 117.5(4) . . ?
C10 C11 H11 121.3 . . ?
C8 C11 H11 121.3 . . ?
C13 C12 Cu2 65.8(7) . . ?
C14 C12 Cu2 70.1(5) . . ?
C13 C12 H12 117.1 . . ?
C14 C12 H12 85.0 . . ?
Cu2 C12 H12 117.1 . . ?
C13 C12 H13 117.1 . . ?
C14 C12 H13 147.8 . . ?
Cu2 C12 H13 117.1 . . ?
H12 C12 H13 114.2 . . ?
C13 C12 H16 150.0 . . ?
C14 C12 H16 116.6 . . ?
Cu2 C12 H16 116.6 . . ?
H13 C12 H16 89.2 . . ?
C13 C12 H17 87.9 . . ?
C14 C12 H17 116.6 . . ?
Cu2 C12 H17 116.6 . . ?
H12 C12 H17 126.1 . . ?
H16 C12 H17 113.6 . . ?
C12 C13 Cu2 73.9(8) . . ?
C12 C13 H14 116.1 . . ?
Cu2 C13 H14 116.1 . . ?
C12 C13 H15 116.1 . . ?
Cu2 C13 H15 116.1 . . ?
H14 C13 H15 113.1 . . ?
C12 C14 Cu2 69.1(5) . . ?
C12 C14 H18 116.8 . . ?
Cu2 C14 H18 116.8 . . ?
C12 C14 H19 116.8 . . ?
Cu2 C14 H19 116.8 . . ?
H18 C14 H19 113.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Cu1 O1 N4 8.5(4) . . . . ?
C2 Cu1 O1 N4 -33.2(4) . . . . ?
N1 Cu1 O1 N4 -149.3(4) . . . . ?
N2 Cu1 O1 N4 127.5(4) . . . . ?
C13 Cu2 O6 N5 -118(4) . . . . ?
N3 Cu2 O6 N5 92(4) . . . . ?
C12 Cu2 O6 N5 -104(4) . . . . ?
C14 Cu2 O6 N5 -140(4) . . . . ?
O7 Cu2 O6 N5 1(3) . . . . ?
Cu2 O6 N5 O5 166(4) . . . . ?
Cu2 O6 N5 O4 -4(6) . . . . ?
C13 Cu2 O7 N6 126(2) . . . . ?
N3 Cu2 O7 N6 -105(2) . . . . ?
C12 Cu2 O7 N6 88(2) . . . . ?
C14 Cu2 O7 N6 100(3) . . . . ?
O6 Cu2 O7 N6 -2(3) . . . . ?
Cu2 O7 N6 O8 -175(3) . . . . ?
Cu2 O7 N6 O9 14(4) . . . . ?
C1 Cu1 N1 C3 -29.0(6) . . . . ?
C2 Cu1 N1 C3 -7.0(4) . . . . ?
N2 Cu1 N1 C3 179.2(4) . . . . ?
O1 Cu1 N1 C3 95.6(4) . . . . ?
C1 Cu1 N1 C7 163.3(4) . . . . ?
C2 Cu1 N1 C7 -174.7(3) . . . . ?
N2 Cu1 N1 C7 11.5(3) . . . . ?
O1 Cu1 N1 C7 -72.0(3) . . . . ?
C1 Cu1 N2 C9 11.8(4) . . . . ?
C2 Cu1 N2 C9 14.3(7) . . . . ?
N1 Cu1 N2 C9 178.5(4) . . . . ?
O1 Cu1 N2 C9 -100.2(4) . . . . ?
C1 Cu1 N2 C8 -177.3(3) . . . . ?
C2 Cu1 N2 C8 -174.7(4) . . . . ?
N1 Cu1 N2 C8 -10.6(3) . . . . ?
O1 Cu1 N2 C8 70.8(3) . . . . ?
C13 Cu2 N3 C9 -50.7(12) . . . . ?
C12 Cu2 N3 C9 -37.5(7) . . . . ?
C14 Cu2 N3 C9 -25.3(9) . . . . ?
O7 Cu2 N3 C9 169.3(7) . . . . ?
O6 Cu2 N3 C9 107.8(8) . . . . ?
C13 Cu2 N3 C10 124.4(12) . . . . ?
C12 Cu2 N3 C10 137.6(5) . . . . ?
C14 Cu2 N3 C10 149.7(9) . . . . ?
O7 Cu2 N3 C10 -15.6(7) . . . . ?
O6 Cu2 N3 C10 -77.1(8) . . . . ?
Cu1 O1 N4 O2 8.8(6) . . . . ?
Cu1 O1 N4 O3 -169.2(3) . . . . ?
N1 Cu1 C1 C2 31.2(5) . . . . ?
N2 Cu1 C1 C2 178.6(3) . . . . ?
O1 Cu1 C1 C2 -87.2(3) . . . . ?
N1 Cu1 C2 C1 -165.7(3) . . . . ?
N2 Cu1 C2 C1 -3.5(6) . . . . ?
O1 Cu1 C2 C1 107.1(3) . . . . ?
C7 N1 C3 C4 0.5(6) . . . . ?
Cu1 N1 C3 C4 -166.5(3) . . . . ?
N1 C3 C4 C5 -0.2(7) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C4 C5 C6 C7 1.2(7) . . . . ?
C3 N1 C7 C6 0.0(6) . . . . ?
Cu1 N1 C7 C6 168.7(3) . . . . ?
C3 N1 C7 C8 -179.1(4) . . . . ?
Cu1 N1 C7 C8 -10.4(4) . . . . ?
C5 C6 C7 N1 -0.9(6) . . . . ?
C5 C6 C7 C8 178.1(4) . . . . ?
C9 N2 C8 C11 0.2(6) . . . . ?
Cu1 N2 C8 C11 -171.8(3) . . . . ?
C9 N2 C8 C7 -180.0(4) . . . . ?
Cu1 N2 C8 C7 8.0(4) . . . . ?
N1 C7 C8 N2 1.5(5) . . . . ?
C6 C7 C8 N2 -177.5(4) . . . . ?
N1 C7 C8 C11 -178.7(4) . . . . ?
C6 C7 C8 C11 2.3(6) . . . . ?
C8 N2 C9 N3 -1.4(6) . . . . ?
Cu1 N2 C9 N3 169.1(3) . . . . ?
C10 N3 C9 N2 1.6(7) . . . . ?
Cu2 N3 C9 N2 176.9(3) . . . . ?
C9 N3 C10 C11 -0.7(7) . . . . ?
Cu2 N3 C10 C11 -176.1(4) . . . . ?
N3 C10 C11 C8 -0.3(7) . . . . ?
N2 C8 C11 C10 0.6(6) . . . . ?
C7 C8 C11 C10 -179.2(4) . . . . ?
N3 Cu2 C12 C13 -19.0(17) . . . . ?
C14 Cu2 C12 C13 -36.2(9) . . . . ?
O7 Cu2 C12 C13 133.2(17) . . . . ?
O6 Cu2 C12 C13 -165.1(18) . . . . ?
C13 Cu2 C12 C14 36.2(9) . . . . ?
N3 Cu2 C12 C14 17.3(14) . . . . ?
O7 Cu2 C12 C14 169.5(13) . . . . ?
O6 Cu2 C12 C14 -128.9(14) . . . . ?
C14 C12 C13 Cu2 -90.0(17) . . . . ?
N3 Cu2 C13 C12 170.6(8) . . . . ?
C14 Cu2 C13 C12 77(2) . . . . ?
O7 Cu2 C13 C12 -65.9(18) . . . . ?
O6 Cu2 C13 C12 22(3) . . . . ?
C13 C12 C14 Cu2 75.9(17) . . . . ?
C13 Cu2 C14 C12 -74.7(19) . . . . ?
N3 Cu2 C14 C12 -171.5(7) . . . . ?
O7 Cu2 C14 C12 -19(2) . . . . ?
O6 Cu2 C14 C12 64.0(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.126

#------------------------------------------------------------------------------
#------------------------------------------------------------------------------

### END

#------------------------------------------------------------------------------
data_[Cu3(pprd)2(AN)2(C2H4)2](BF4)3 #(complex-2) CCDC-695267
_database_code_depnum_ccdc_archive 'CCDC 695267'
#------------------------------------------------------------------------------

# CHEMICAL DATA
_chemical_formula_sum            'C26 H28 B3 Cu3 F12 N8 '
_chemical_formula_moiety         'C26 H28 Cu3 N8 3+, 3(B F4 -)'
_chemical_formula_weight         903.61
_chemical_melting_point          ?
#------------------------------------------------------------------------------

# CRYSTAL DATA
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m '
_symmetry_space_group_name_Hall  '-P 2yb '
_symmetry_Int_Tables_number      11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.6904(8)
_cell_length_b                   23.414(2)
_cell_length_c                   8.8729(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.645(2)
_cell_angle_gamma                90.00
_cell_volume                     1678.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9989
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.6

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_process_details   '(Jacobson, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.62
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11828
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3847
_reflns_number_gt                2845
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSTALCLEAR
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_structure_solution    SHELXS97
_computing_structure_refinement  SHELXL97
_computing_publication_material  'teXsan Ver. 2.0'
_computing_molecular_graphics    ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+2.8758P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3847
_refine_ls_number_parameters     234
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0880
_refine_ls_wR_factor_ref         0.2434
_refine_ls_wR_factor_gt          0.2218
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_restrained_S_all      1.526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74787(11) 0.07443(4) 0.07942(10) 0.0278(3) Uani 1 1 d . . .
Cu2 Cu 1.05419(17) 0.2500 0.57696(16) 0.0302(4) Uani 1 2 d S . .
F1 F 0.5625(8) 0.0527(3) 0.2889(8) 0.0574(10) Uiso 0.834(6) 1 d PD A 1
F2 F 0.3528(7) 0.1139(3) 0.2530(8) 0.0574(10) Uiso 0.834(6) 1 d PD A 1
F3 F 0.6135(8) 0.1436(3) 0.3507(8) 0.0574(10) Uiso 0.834(6) 1 d PD A 1
F4 F 0.5212(9) 0.0911(3) 0.5050(7) 0.0574(10) Uiso 0.834(6) 1 d PD A 1
F5 F 0.465(3) 0.0416(6) 0.354(3) 0.0574(10) Uiso 0.166(6) 1 d PD A 2
F6 F 0.375(2) 0.1259(11) 0.249(3) 0.0574(10) Uiso 0.166(6) 1 d PD A 2
F7 F 0.639(2) 0.1012(12) 0.310(3) 0.0574(10) Uiso 0.166(6) 1 d PD A 2
F8 F 0.544(3) 0.1184(11) 0.5051(19) 0.0574(10) Uiso 0.166(6) 1 d PD A 2
F9 F 0.7521(9) 0.2546(8) 0.0736(8) 0.0397(12) Uiso 0.50 1 d PD . .
F10 F 1.0213(11) 0.2671(3) 0.1244(10) 0.0397(12) Uiso 0.50 1 d PD . .
F11 F 0.8217(13) 0.2968(4) -0.1142(12) 0.0397(12) Uiso 0.50 1 d PD B 3
F12 F 0.8807(13) 0.2976(4) -0.0621(12) 0.0397(12) Uiso 0.50 1 d PD B 4
N1 N 0.8815(8) 0.0034(3) 0.1362(7) 0.0263(13) Uani 1 1 d . . .
N2 N 0.9325(8) 0.1041(3) 0.2753(7) 0.0263(14) Uani 1 1 d . . .
N3 N 1.0711(8) 0.1726(3) 0.4768(7) 0.0266(14) Uani 1 1 d . . .
N4 N 0.8170(14) 0.2500 0.5561(12) 0.042(2) Uani 1 2 d S . .
N5 N 1.2162(12) 0.2500 0.8048(11) 0.034(2) Uani 1 2 d S . .
C1 C 0.5584(11) 0.1235(4) -0.0497(10) 0.038(2) Uani 1 1 d . . .
H1 H 0.4783 0.1336 0.0015 0.045 Uiso 1 1 calc R . .
H2 H 0.5837 0.1555 -0.1096 0.045 Uiso 1 1 calc R . .
C2 C 0.5409(10) 0.0713(3) -0.1198(9) 0.0304(18) Uani 1 1 d . . .
H3 H 0.5553 0.0691 -0.2252 0.036 Uiso 1 1 calc R . .
H4 H 0.4498 0.0471 -0.1139 0.036 Uiso 1 1 calc R . .
C3 C 0.8496(10) -0.0465(3) 0.0540(10) 0.0329(18) Uani 1 1 d . . .
H5 H 0.7541 -0.0493 -0.0426 0.039 Uiso 1 1 calc R . .
C4 C 0.9520(11) -0.0939(4) 0.1063(11) 0.037(2) Uani 1 1 d . . .
H6 H 0.9273 -0.1287 0.0472 0.044 Uiso 1 1 calc R . .
C5 C 1.0895(11) -0.0889(3) 0.2452(10) 0.0345(19) Uani 1 1 d . . .
H7 H 1.1608 -0.1208 0.2841 0.041 Uiso 1 1 calc R . .
C6 C 1.1250(10) -0.0382(3) 0.3288(10) 0.0300(17) Uani 1 1 d . . .
H8 H 1.2210 -0.0346 0.4246 0.036 Uiso 1 1 calc R . .
C7 C 1.0194(9) 0.0072(3) 0.2715(8) 0.0237(15) Uani 1 1 d . . .
C8 C 1.0457(9) 0.0640(3) 0.3507(9) 0.0240(15) Uani 1 1 d . . .
C9 C 1.1737(10) 0.0769(3) 0.4941(9) 0.0275(16) Uani 1 1 d . . .
H9 H 1.2528 0.0490 0.5517 0.033 Uiso 1 1 calc R . .
C10 C 1.1816(10) 0.1324(3) 0.5501(9) 0.0268(16) Uani 1 1 d . . .
H10 H 1.2712 0.1425 0.6466 0.032 Uiso 1 1 calc R . .
C11 C 0.9484(10) 0.1563(3) 0.3412(9) 0.0296(17) Uani 1 1 d . . .
H11 H 0.8662 0.1838 0.2874 0.036 Uiso 1 1 calc R . .
C12 C 1.2852(14) 0.2500 0.9370(14) 0.031(2) Uani 1 2 d S . .
C13 C 1.3746(15) 0.2500 1.1139(13) 0.034(3) Uani 1 2 d S . .
H12 H 1.4807 0.2302 1.1401 0.041 Uiso 0.50 1 calc PR . .
H13 H 1.3080 0.2303 1.1662 0.041 Uiso 0.50 1 calc PR . .
H14 H 1.3946 0.2895 1.1531 0.041 Uiso 0.50 1 calc PR . .
C14 C 0.6876(15) 0.2500 0.5562(14) 0.033(3) Uani 1 2 d S . .
C15 C 0.5180(15) 0.2500 0.5607(16) 0.040(3) Uani 1 2 d S . .
H15 H 0.4419 0.2697 0.4646 0.048 Uiso 0.50 1 calc PR . .
H16 H 0.5196 0.2698 0.6586 0.048 Uiso 0.50 1 calc PR . .
H17 H 0.4809 0.2105 0.5620 0.048 Uiso 0.50 1 calc PR . .
B1 B 0.5091(9) 0.0983(3) 0.3516(8) 0.034(2) Uani 1 1 d D . .
B2 B 0.8745(17) 0.2500 0.0003(15) 0.036(3) Uani 1 2 d SD . .

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 0.0201(6) 0.0319(6) 0.0289(5) -0.0006(4) 0.0062(4) 0.0010(4)
Cu2 0.0264(8) 0.0317(8) 0.0326(7) 0.000 0.0109(6) 0.000
N1 0.020(3) 0.030(3) 0.032(3) -0.001(3) 0.014(3) -0.002(3)
N2 0.020(3) 0.029(3) 0.030(3) -0.001(3) 0.010(3) 0.001(3)
N3 0.023(4) 0.028(3) 0.027(3) 0.001(2) 0.007(3) -0.002(3)
N4 0.037(7) 0.050(6) 0.040(6) 0.000 0.017(5) 0.000
N5 0.032(6) 0.043(6) 0.022(5) 0.000 0.004(4) 0.000
C1 0.033(5) 0.036(4) 0.038(4) 0.007(3) 0.007(4) 0.010(4)
C2 0.015(4) 0.044(5) 0.028(4) 0.002(3) 0.004(3) 0.000(3)
C3 0.024(4) 0.036(4) 0.042(4) -0.005(3) 0.016(4) 0.000(3)
C4 0.042(5) 0.033(4) 0.048(5) -0.007(4) 0.031(4) -0.003(4)
C5 0.035(5) 0.030(4) 0.050(5) 0.000(3) 0.029(4) 0.005(4)
C6 0.020(4) 0.034(4) 0.043(4) -0.001(3) 0.019(3) -0.002(3)
C7 0.018(4) 0.028(4) 0.031(4) 0.003(3) 0.016(3) -0.001(3)
C8 0.018(4) 0.029(4) 0.031(4) 0.001(3) 0.016(3) -0.001(3)
C9 0.016(4) 0.035(4) 0.031(4) 0.002(3) 0.009(3) 0.003(3)
C10 0.021(4) 0.035(4) 0.028(4) -0.002(3) 0.013(3) -0.002(3)
C11 0.026(4) 0.028(4) 0.034(4) -0.004(3) 0.011(3) -0.001(3)
C12 0.025(6) 0.024(5) 0.047(7) 0.000 0.015(5) 0.000
C13 0.030(7) 0.044(7) 0.027(5) 0.000 0.010(5) 0.000
C14 0.030(7) 0.037(6) 0.037(6) 0.000 0.017(5) 0.000
C15 0.023(6) 0.052(7) 0.053(7) 0.000 0.023(6) 0.000
B1 0.025(5) 0.050(6) 0.030(4) 0.003(4) 0.013(4) 0.000(4)
B2 0.039(8) 0.048(8) 0.027(6) 0.000 0.018(6) 0.000

_geom_special_details            
;
All BF4 anions are restrained using ideal bond lengthes and angles by DFIX
and DANG command on SHELXL-97.
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 C1 1.987(8) . ?
Cu1 N1 1.985(6) . ?
Cu1 C2 2.005(7) . ?
Cu1 N2 2.005(6) . ?
Cu2 N5 1.992(9) . ?
Cu2 N4 2.000(11) . ?
Cu2 N3 2.048(6) . ?
Cu2 N3 2.048(6) 4_565 ?
F1 B1 1.362(8) . ?
F2 B1 1.366(8) . ?
F3 B1 1.397(8) . ?
F4 B1 1.336(8) . ?
F5 B1 1.385(10) . ?
F6 B1 1.348(10) . ?
F7 B1 1.318(10) . ?
F8 B1 1.365(10) . ?
F9 F9 0.22(4) 4_565 ?
F9 B2 1.441(14) . ?
F10 F10 0.802(15) 4_565 ?
F10 B2 1.401(15) . ?
F11 B2 1.449(12) . ?
F12 B2 1.255(11) . ?
N1 C3 1.350(10) . ?
N1 C7 1.350(9) . ?
N2 C11 1.341(9) . ?
N2 C8 1.345(9) . ?
N3 C10 1.330(10) . ?
N3 C11 1.335(9) . ?
N4 C14 1.125(16) . ?
N5 C12 1.104(14) . ?
C1 C2 1.354(11) . ?
C1 H1 0.9900 . ?
C1 H2 0.9900 . ?
C2 H3 0.9900 . ?
C2 H4 0.9900 . ?
C3 C4 1.390(11) . ?
C3 H5 0.9500 . ?
C4 C5 1.369(12) . ?
C4 H6 0.9500 . ?
C5 C6 1.373(11) . ?
C5 H7 0.9500 . ?
C6 C7 1.374(10) . ?
C6 H8 0.9500 . ?
C7 C8 1.483(10) . ?
C8 C9 1.380(10) . ?
C9 C10 1.385(10) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.472(15) . ?
C13 H12 0.9800 . ?
C13 H13 0.9800 . ?
C13 H14 0.9800 . ?
C14 C15 1.490(16) . ?
C15 H15 0.9800 . ?
C15 H16 0.9800 . ?
C15 H17 0.9800 . ?
B2 F12 1.255(11) 4_565 ?
B2 F10 1.401(15) 4_565 ?
B2 F11 1.449(12) 4_565 ?
B2 F9 1.441(14) 4_565 ?

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
C1 Cu1 N1 156.0(3) . . ?
C1 Cu1 C2 39.7(3) . . ?
N1 Cu1 C2 116.3(3) . . ?
C1 Cu1 N2 121.8(3) . . ?
N1 Cu1 N2 82.2(3) . . ?
C2 Cu1 N2 161.4(3) . . ?
N5 Cu2 N4 114.3(4) . . ?
N5 Cu2 N3 107.7(2) . . ?
N4 Cu2 N3 101.3(2) . . ?
N5 Cu2 N3 107.7(2) . 4_565 ?
N4 Cu2 N3 101.3(2) . 4_565 ?
N3 Cu2 N3 124.5(3) . 4_565 ?
F9 F9 B2 85.7(7) 4_565 . ?
F10 F10 B2 73.4(4) 4_565 . ?
C3 N1 C7 118.4(7) . . ?
C3 N1 Cu1 127.1(5) . . ?
C7 N1 Cu1 114.5(5) . . ?
C11 N2 C8 118.7(6) . . ?
C11 N2 Cu1 128.0(5) . . ?
C8 N2 Cu1 113.2(5) . . ?
C10 N3 C11 115.6(6) . . ?
C10 N3 Cu2 124.6(5) . . ?
C11 N3 Cu2 118.9(5) . . ?
C14 N4 Cu2 175.0(10) . . ?
C12 N5 Cu2 169.3(10) . . ?
C2 C1 Cu1 70.9(5) . . ?
C2 C1 H1 116.5 . . ?
Cu1 C1 H1 116.5 . . ?
C2 C1 H2 116.5 . . ?
Cu1 C1 H2 116.5 . . ?
H1 C1 H2 113.5 . . ?
C1 C2 Cu1 69.5(5) . . ?
C1 C2 H3 116.7 . . ?
Cu1 C2 H3 116.7 . . ?
C1 C2 H4 116.7 . . ?
Cu1 C2 H4 116.7 . . ?
H3 C2 H4 113.7 . . ?
N1 C3 C4 122.0(8) . . ?
N1 C3 H5 119.0 . . ?
C4 C3 H5 119.0 . . ?
C5 C4 C3 118.2(8) . . ?
C5 C4 H6 120.9 . . ?
C3 C4 H6 120.9 . . ?
C6 C5 C4 120.5(8) . . ?
C6 C5 H7 119.8 . . ?
C4 C5 H7 119.8 . . ?
C5 C6 C7 118.9(8) . . ?
C5 C6 H8 120.6 . . ?
C7 C6 H8 120.6 . . ?
N1 C7 C6 122.0(7) . . ?
N1 C7 C8 114.3(6) . . ?
C6 C7 C8 123.7(7) . . ?
N2 C8 C9 120.0(7) . . ?
N2 C8 C7 115.7(6) . . ?
C9 C8 C7 124.3(7) . . ?
C8 C9 C10 116.9(7) . . ?
C8 C9 H9 121.5 . . ?
C10 C9 H9 121.5 . . ?
N3 C10 C9 123.8(7) . . ?
N3 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
N3 C11 N2 125.0(7) . . ?
N3 C11 H11 117.5 . . ?
N2 C11 H11 117.5 . . ?
N5 C12 C13 179.1(12) . . ?
C12 C13 H12 109.5 . . ?
C12 C13 H13 109.5 . . ?
H12 C13 H13 109.5 . . ?
C12 C13 H14 109.5 . . ?
H12 C13 H14 109.5 . . ?
H13 C13 H14 109.5 . . ?
N4 C14 C15 178.6(13) . . ?
C14 C15 H15 109.5 . . ?
C14 C15 H16 109.5 . . ?
H15 C15 H16 109.5 . . ?
C14 C15 H17 109.5 . . ?
H15 C15 H17 109.5 . . ?
H16 C15 H17 109.5 . . ?
F7 B1 F4 122.7(13) . . ?
F7 B1 F6 113.6(10) . . ?
F4 B1 F6 118.3(14) . . ?
F4 B1 F1 114.0(6) . . ?
F7 B1 F8 111.4(10) . . ?
F6 B1 F8 109.3(10) . . ?
F4 B1 F2 111.9(7) . . ?
F1 B1 F2 110.8(6) . . ?
F7 B1 F5 109.1(10) . . ?
F6 B1 F5 107.1(10) . . ?
F8 B1 F5 105.9(10) . . ?
F4 B1 F3 107.1(6) . . ?
F1 B1 F3 105.8(6) . . ?
F2 B1 F3 106.7(6) . . ?
F12 B2 F12 125.3(14) 4_565 . ?
F12 B2 F10 115.2(10) 4_565 . ?
F12 B2 F10 85.3(8) . . ?
F12 B2 F10 85.3(8) 4_565 4_565 ?
F12 B2 F10 115.2(10) . 4_565 ?
F12 B2 F11 114.6(10) . 4_565 ?
F10 B2 F11 136.7(10) . 4_565 ?
F10 B2 F11 107.2(7) 4_565 4_565 ?
F12 B2 F11 114.6(10) 4_565 . ?
F10 B2 F11 107.2(7) . . ?
F10 B2 F11 136.7(10) 4_565 . ?
F11 B2 F11 98.2(11) 4_565 . ?
F12 B2 F9 115.1(11) 4_565 . ?
F12 B2 F9 107.0(10) . . ?
F10 B2 F9 103.5(9) . . ?
F10 B2 F9 106.1(9) 4_565 . ?
F11 B2 F9 106.1(10) 4_565 . ?
F11 B2 F9 99.5(10) . . ?
F12 B2 F9 107.0(10) 4_565 4_565 ?
F12 B2 F9 115.1(11) . 4_565 ?
F10 B2 F9 106.1(9) . 4_565 ?
F10 B2 F9 103.5(9) 4_565 4_565 ?
F11 B2 F9 99.5(10) 4_565 4_565 ?
F11 B2 F9 106.1(10) . 4_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Cu1 N1 C3 2.2(11) . . . . ?
C2 Cu1 N1 C3 1.1(7) . . . . ?
N2 Cu1 N1 C3 -177.2(6) . . . . ?
C1 Cu1 N1 C7 -178.6(7) . . . . ?
C2 Cu1 N1 C7 -179.7(5) . . . . ?
N2 Cu1 N1 C7 2.0(5) . . . . ?
C1 Cu1 N2 C11 1.7(8) . . . . ?
N1 Cu1 N2 C11 -178.6(7) . . . . ?
C2 Cu1 N2 C11 6.1(13) . . . . ?
C1 Cu1 N2 C8 177.3(5) . . . . ?
N1 Cu1 N2 C8 -3.0(5) . . . . ?
C2 Cu1 N2 C8 -178.3(8) . . . . ?
N5 Cu2 N3 C10 -5.1(7) . . . . ?
N4 Cu2 N3 C10 -125.4(6) . . . . ?
N3 Cu2 N3 C10 122.2(5) 4_565 . . . ?
N5 Cu2 N3 C11 163.0(6) . . . . ?
N4 Cu2 N3 C11 42.7(6) . . . . ?
N3 Cu2 N3 C11 -69.7(7) 4_565 . . . ?
N4 Cu2 N5 C12 0.000(18) . . . . ?
N3 Cu2 N5 C12 -111.7(2) . . . . ?
N3 Cu2 N5 C12 111.7(2) 4_565 . . . ?
N1 Cu1 C1 C2 -1.5(11) . . . . ?
N2 Cu1 C1 C2 177.8(5) . . . . ?
N1 Cu1 C2 C1 179.3(5) . . . . ?
N2 Cu1 C2 C1 -6.0(12) . . . . ?
C7 N1 C3 C4 1.3(11) . . . . ?
Cu1 N1 C3 C4 -179.5(6) . . . . ?
N1 C3 C4 C5 -0.4(12) . . . . ?
C3 C4 C5 C6 -0.7(12) . . . . ?
C4 C5 C6 C7 0.7(12) . . . . ?
C3 N1 C7 C6 -1.4(10) . . . . ?
Cu1 N1 C7 C6 179.4(5) . . . . ?
C3 N1 C7 C8 178.5(6) . . . . ?
Cu1 N1 C7 C8 -0.7(7) . . . . ?
C5 C6 C7 N1 0.4(11) . . . . ?
C5 C6 C7 C8 -179.5(7) . . . . ?
C11 N2 C8 C9 0.8(10) . . . . ?
Cu1 N2 C8 C9 -175.3(5) . . . . ?
C11 N2 C8 C7 179.5(6) . . . . ?
Cu1 N2 C8 C7 3.5(8) . . . . ?
N1 C7 C8 N2 -1.9(9) . . . . ?
C6 C7 C8 N2 178.0(6) . . . . ?
N1 C7 C8 C9 176.8(7) . . . . ?
C6 C7 C8 C9 -3.3(11) . . . . ?
N2 C8 C9 C10 -2.3(10) . . . . ?
C7 C8 C9 C10 179.0(7) . . . . ?
C11 N3 C10 C9 -0.4(11) . . . . ?
Cu2 N3 C10 C9 168.0(6) . . . . ?
C8 C9 C10 N3 2.2(11) . . . . ?
C10 N3 C11 N2 -1.4(11) . . . . ?
Cu2 N3 C11 N2 -170.5(6) . . . . ?
C8 N2 C11 N3 1.2(12) . . . . ?
Cu1 N2 C11 N3 176.6(6) . . . . ?
F10 F10 B2 F12 -27.8(8) 4_565 . . 4_565 ?
F10 F10 B2 F12 -154.9(8) 4_565 . . . ?
F10 F10 B2 F11 -33.5(11) 4_565 . . 4_565 ?
F10 F10 B2 F11 -156.7(9) 4_565 . . . ?
F10 F10 B2 F9 98.8(8) 4_565 . . . ?
F10 F10 B2 F9 90.3(8) 4_565 . . 4_565 ?
F9 F9 B2 F12 18.4(9) 4_565 . . 4_565 ?
F9 F9 B2 F12 162.6(9) 4_565 . . . ?
F9 F9 B2 F10 -108.3(4) 4_565 . . . ?
F9 F9 B2 F10 -73.9(4) 4_565 . . 4_565 ?
F9 F9 B2 F11 39.9(7) 4_565 . . 4_565 ?
F9 F9 B2 F11 141.4(7) 4_565 . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.957
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.184

#------------------------------------------------------------------------------
#------------------------------------------------------------------------------

### END

#------------------------------------------------------------------------------
data_{[Cu6(pprd)6(C2H4)6](BF4)6}2.6H2O #(complex-3) CCDC-695268
_database_code_depnum_ccdc_archive 'CCDC 695268'
#------------------------------------------------------------------------------

# CHEMICAL DATA
_chemical_formula_sum            'C66 H72 B6 Cu6 F24 N18 O3 '
_chemical_formula_moiety         'C66 H72 B6 Cu6 F24 N18 O3 '
_chemical_formula_weight         2067.52
_chemical_melting_point          ?
#------------------------------------------------------------------------------

# CRYSTAL DATA
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 '
_symmetry_space_group_name_Hall  '-R 3 '
_symmetry_Int_Tables_number      148

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   27.6972(15)
_cell_length_b                   27.6972(15)
_cell_length_c                   19.8549(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13190.8(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    7840
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6228
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6570
_exptl_absorpt_correction_T_max  0.8260
_exptl_absorpt_process_details   '(Jacobson, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.62
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33514
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6725
_reflns_number_gt                4036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CRYSTALCLEAR
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_reduction        CRYSTALCLEAR
_computing_structure_solution    SHELXS97
_computing_structure_refinement  SHELXL97
_computing_publication_material  'Crystal Structure 3.8'
_computing_molecular_graphics    ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6725
_refine_ls_number_parameters     427
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.1063
_refine_ls_wR_factor_ref         0.3483
_refine_ls_wR_factor_gt          0.3126
_refine_ls_goodness_of_fit_ref   1.895
_refine_ls_restrained_S_all      1.917
_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 0.36961(3) 0.52944(4) 0.56094(4) 0.0533(4) Uani 1 1 d . . .
Cu2 Cu 0.19540(3) 0.49723(3) 0.27137(4) 0.0514(3) Uani 1 1 d . . .
F1 F 0.3758(6) 0.6717(8) 0.6268(9) 0.138(5) Uani 0.50 1 d PDU . .
F2 F 0.342(2) 0.6319(19) 0.629(2) 0.116(9) Uani 0.17 1 d PDU . .
F3 F 0.2847(4) 0.6524(6) 0.2056(9) 0.131(5) Uani 0.50 1 d PDU . .
F4 F 0.327(2) 0.7001(18) 0.213(2) 0.143(10) Uani 0.17 1 d PDU . .
F5 F 0.5339(6) 0.6877(4) 0.4754(4) 0.167(4) Uani 0.83 1 d PU . .
F6 F 0.4951(3) 0.7036(3) 0.5594(4) 0.122(2) Uani 0.83 1 d PU . .
F7 F 0.5852(3) 0.7557(3) 0.5448(5) 0.135(3) Uani 0.83 1 d PU . .
F8 F 0.5514(3) 0.6711(3) 0.5779(3) 0.0927(18) Uani 0.83 1 d PU . .
F9 F 0.5836(6) 0.4794(4) 0.7145(5) 0.230(6) Uani 0.83 1 d PU . .
F10 F 0.6213(3) 0.5484(3) 0.6490(3) 0.099(2) Uani 0.83 1 d PU . .
F11 F 0.6226(3) 0.5583(3) 0.7580(3) 0.115(2) Uani 0.83 1 d PU . .
F12 F 0.6750(6) 0.5359(7) 0.7132(6) 0.239(6) Uani 0.83 1 d PU . .
O1 O 0.7556(8) 0.6095(9) 0.5541(12) 0.046(2) Uani 0.206(9) 1 d PU . .
O2 O 0.7593(8) 0.5934(9) 0.5966(13) 0.046(2) Uani 0.194(8) 1 d PU . .
O3 O 0.7790(5) 0.6158(5) 0.6354(8) 0.046(2) Uani 0.297(8) 1 d PU . .
O4 O 0.5892(9) 0.7207(9) 0.4974(14) 0.046(2) Uani 0.177(8) 1 d P . .
O5 O 0.7482(13) 0.6299(14) 0.5477(19) 0.046(2) Uani 0.127(9) 1 d PU . .
N1 N 0.49070(19) 0.63593(19) 0.7149(3) 0.0412(11) Uani 1 1 d . . .
N2 N 0.43583(19) 0.5687(2) 0.6314(2) 0.0391(11) Uani 1 1 d . . .
N3 N 0.4087(2) 0.4827(2) 0.5507(3) 0.0486(13) Uani 1 1 d . . .
N4 N 0.1305(2) 0.5685(2) 0.1238(3) 0.0465(13) Uani 1 1 d . . .
N5 N 0.1455(2) 0.5148(2) 0.2053(3) 0.0443(12) Uani 1 1 d . . .
N6 N 0.1152(2) 0.4336(2) 0.2948(3) 0.0518(13) Uani 1 1 d . . .
C1 C 0.4482(2) 0.6130(2) 0.6699(3) 0.0412(13) Uani 1 1 d . . .
H1 H 0.4256 0.6296 0.6654 0.049 Uiso 1 1 calc R . .
C2 C 0.4678(2) 0.5448(2) 0.6365(3) 0.0384(13) Uani 1 1 d . . .
C3 C 0.5120(2) 0.5653(3) 0.6816(3) 0.0487(15) Uani 1 1 d . . .
H2 H 0.5345 0.5486 0.6861 0.058 Uiso 1 1 calc R . .
C4 C 0.5219(3) 0.6114(3) 0.7199(4) 0.0522(16) Uani 1 1 d . . .
H3 H 0.5520 0.6262 0.7509 0.063 Uiso 1 1 calc R . .
C5 C 0.4526(2) 0.4965(2) 0.5929(3) 0.0432(14) Uani 1 1 d . . .
C6 C 0.4810(3) 0.4679(3) 0.5927(3) 0.0493(15) Uani 1 1 d . . .
H4 H 0.5120 0.4784 0.6218 0.059 Uiso 1 1 calc R . .
C7 C 0.4633(3) 0.4230(3) 0.5487(4) 0.0624(19) Uani 1 1 d . . .
H5 H 0.4819 0.4020 0.5482 0.075 Uiso 1 1 calc R . .
C8 C 0.4199(3) 0.4090(3) 0.5067(4) 0.064(2) Uani 1 1 d . . .
H6 H 0.4080 0.3786 0.4764 0.077 Uiso 1 1 calc R . .
C9 C 0.3942(3) 0.4387(3) 0.5087(3) 0.0532(17) Uani 1 1 d . . .
H7 H 0.3638 0.4286 0.4788 0.064 Uiso 1 1 calc R . .
C10 C 0.3879(5) 0.5782(5) 0.4783(6) 0.127(4) Uani 1 1 d DU . .
H8 H 0.4175 0.6176 0.4835 0.152 Uiso 1 1 calc R . .
H9 H 0.3898 0.5615 0.4351 0.152 Uiso 1 1 calc R . .
C11 C 0.3385(5) 0.5656(6) 0.4991(6) 0.128(5) Uani 1 1 d DU . .
H10 H 0.3069 0.5402 0.4700 0.154 Uiso 1 1 calc R . .
H11 H 0.3346 0.5964 0.5184 0.154 Uiso 1 1 calc R . .
C12 C 0.1625(3) 0.5567(2) 0.1626(3) 0.0444(14) Uani 1 1 d . . .
H12 H 0.2016 0.5810 0.1592 0.053 Uiso 1 1 calc R . .
C13 C 0.0902(2) 0.4797(2) 0.2102(3) 0.0459(15) Uani 1 1 d . . .
C14 C 0.0532(3) 0.4882(3) 0.1716(4) 0.0589(18) Uani 1 1 d . . .
H13 H 0.0142 0.4631 0.1739 0.071 Uiso 1 1 calc R . .
C15 C 0.0744(3) 0.5332(3) 0.1306(4) 0.064(2) Uani 1 1 d . . .
H14 H 0.0495 0.5405 0.1057 0.077 Uiso 1 1 calc R . .
C16 C 0.0742(2) 0.4340(2) 0.2599(3) 0.0477(15) Uani 1 1 d . . .
C17 C 0.0176(3) 0.3938(3) 0.2690(4) 0.063(2) Uani 1 1 d . . .
H15 H -0.0110 0.3948 0.2437 0.076 Uiso 1 1 calc R . .
C18 C 0.0056(3) 0.3527(3) 0.3166(4) 0.069(2) Uani 1 1 d . . .
H16 H -0.0319 0.3251 0.3253 0.083 Uiso 1 1 calc R . .
C19 C 0.0479(3) 0.3522(3) 0.3509(4) 0.069(2) Uani 1 1 d . . .
H17 H 0.0401 0.3238 0.3831 0.082 Uiso 1 1 calc R . .
C20 C 0.1020(3) 0.3929(3) 0.3387(4) 0.0635(19) Uani 1 1 d . . .
H18 H 0.1311 0.3918 0.3626 0.076 Uiso 1 1 calc R . .
C21 C 0.2169(4) 0.5520(4) 0.3486(4) 0.097(3) Uani 1 1 d DU . .
H19 H 0.2155 0.5864 0.3396 0.117 Uiso 1 1 calc R . .
H20 H 0.2028 0.5360 0.3938 0.117 Uiso 1 1 calc R . .
C22 C 0.2620(4) 0.5515(5) 0.3275(6) 0.115(4) Uani 1 1 d DU . .
H21 H 0.2778 0.5350 0.3584 0.138 Uiso 1 1 calc R . .
H22 H 0.2905 0.5855 0.3043 0.138 Uiso 1 1 calc R . .
B1 B 0.3333 0.6667 0.6667 0.117(7) Uani 1 6 d SDU . .
B2 B 0.3333 0.6667 0.1667 0.131(8) Uani 1 6 d SDU . .
B3 B 0.5403(4) 0.7027(4) 0.5415(5) 0.053(2) Uani 0.83 1 d PU . .
B4 B 0.6232(7) 0.5265(6) 0.7089(8) 0.091(3) Uani 0.83 1 d PU . .

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 0.0483(5) 0.0725(6) 0.0459(6) 0.0090(4) 0.0003(3) 0.0352(4)
Cu2 0.0414(5) 0.0535(5) 0.0561(6) -0.0038(4) 0.0013(3) 0.0213(4)
F1 0.076(9) 0.115(10) 0.227(16) 0.010(12) 0.004(9) 0.052(8)
F2 0.074(18) 0.096(15) 0.20(3) -0.009(17) -0.017(19) 0.059(9)
F3 0.071(7) 0.094(7) 0.244(16) -0.040(10) -0.025(7) 0.054(6)
F4 0.086(17) 0.075(12) 0.29(3) -0.008(16) -0.01(2) 0.057(9)
F5 0.331(13) 0.163(7) 0.086(4) -0.008(5) 0.007(6) 0.183(8)
F6 0.112(5) 0.144(6) 0.145(6) -0.020(5) -0.009(5) 0.090(5)
F7 0.100(5) 0.097(4) 0.209(9) 0.008(5) -0.014(5) 0.050(4)
F8 0.089(4) 0.109(5) 0.087(4) 0.026(4) 0.027(3) 0.055(4)
F9 0.326(12) 0.087(5) 0.132(7) 0.019(5) 0.015(9) -0.005(7)
F10 0.093(4) 0.117(5) 0.104(4) 0.004(4) -0.023(4) 0.065(4)
F11 0.128(6) 0.093(5) 0.105(5) 0.005(4) 0.001(4) 0.040(4)
F12 0.219(8) 0.439(18) 0.196(10) -0.031(12) -0.064(9) 0.268(11)
O1 0.035(4) 0.038(5) 0.076(7) -0.018(4) -0.034(4) 0.026(4)
O2 0.035(4) 0.038(5) 0.076(7) -0.018(4) -0.034(4) 0.026(4)
O3 0.035(4) 0.038(5) 0.076(7) -0.018(4) -0.034(4) 0.026(4)
O4 0.035(4) 0.038(5) 0.076(7) -0.018(4) -0.034(4) 0.026(4)
O5 0.035(4) 0.038(5) 0.076(7) -0.018(4) -0.034(4) 0.026(4)
N1 0.034(2) 0.035(2) 0.052(3) -0.002(2) 0.004(2) 0.015(2)
N2 0.032(2) 0.042(3) 0.044(3) 0.005(2) 0.004(2) 0.019(2)
N3 0.035(3) 0.060(3) 0.045(3) -0.004(2) 0.003(2) 0.019(2)
N4 0.037(3) 0.042(3) 0.062(3) -0.004(2) -0.008(2) 0.021(2)
N5 0.037(3) 0.035(3) 0.061(3) -0.004(2) 0.000(2) 0.018(2)
N6 0.046(3) 0.041(3) 0.060(3) 0.009(3) 0.011(3) 0.015(2)
C1 0.037(3) 0.042(3) 0.048(3) 0.007(3) 0.004(3) 0.022(3)
C2 0.029(3) 0.040(3) 0.043(3) 0.000(2) 0.004(2) 0.015(2)
C3 0.040(3) 0.054(4) 0.059(4) -0.009(3) -0.005(3) 0.028(3)
C4 0.037(3) 0.047(4) 0.065(4) -0.012(3) -0.009(3) 0.015(3)
C5 0.033(3) 0.044(3) 0.048(3) -0.002(3) 0.004(3) 0.016(3)
C6 0.044(3) 0.047(4) 0.057(4) -0.007(3) 0.001(3) 0.023(3)
C7 0.055(4) 0.049(4) 0.080(5) -0.006(4) 0.016(4) 0.024(3)
C8 0.044(4) 0.064(4) 0.072(5) -0.021(4) 0.008(4) 0.017(3)
C9 0.039(3) 0.057(4) 0.053(4) -0.016(3) 0.005(3) 0.016(3)
C10 0.134(9) 0.143(10) 0.109(8) 0.076(8) 0.024(7) 0.075(9)
C11 0.104(7) 0.181(11) 0.133(9) 0.107(9) 0.019(7) 0.096(8)
C12 0.041(3) 0.041(3) 0.055(4) -0.009(3) 0.001(3) 0.023(3)
C13 0.036(3) 0.036(3) 0.065(4) -0.007(3) 0.002(3) 0.017(3)
C14 0.034(3) 0.049(4) 0.082(5) 0.010(4) 0.000(3) 0.013(3)
C15 0.042(4) 0.057(4) 0.089(6) 0.008(4) -0.014(4) 0.021(3)
C16 0.038(3) 0.036(3) 0.065(4) 0.000(3) 0.014(3) 0.016(3)
C17 0.044(4) 0.044(4) 0.093(6) -0.002(4) 0.011(4) 0.015(3)
C18 0.055(4) 0.052(4) 0.090(6) 0.002(4) 0.011(4) 0.019(4)
C19 0.064(5) 0.056(4) 0.079(5) 0.025(4) 0.023(4) 0.024(4)
C20 0.056(4) 0.057(4) 0.069(5) 0.023(4) 0.011(4) 0.022(4)
C21 0.108(7) 0.100(7) 0.060(5) -0.036(5) -0.010(5) 0.034(6)
C22 0.079(6) 0.134(9) 0.098(7) -0.057(7) -0.037(6) 0.027(6)
B1 0.053(7) 0.053(7) 0.25(3) 0.000 0.000 0.026(4)
B2 0.064(8) 0.064(8) 0.27(3) 0.000 0.000 0.032(4)
B3 0.068(5) 0.055(5) 0.056(5) -0.011(4) -0.007(5) 0.045(4)
B4 0.092(7) 0.083(7) 0.088(8) 0.016(6) 0.041(7) 0.036(6)

_geom_special_details            
;
The large Ueq(max)/Ueq(min) ratio of C10, C11 and C22 is due to
the ethylene molecule being slightly disordered as a result
of the flexibility of the Cu-ethylene bond.
The hydrogen atoms are not located to disordered water molecules.
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 C10 2.022(9) . ?
Cu1 C11 2.029(7) . ?
Cu1 N1 2.029(5) 14_456 ?
Cu1 N3 2.073(5) . ?
Cu1 N2 2.123(5) . ?
Cu2 N4 2.017(5) 15 ?
Cu2 C21 2.027(8) . ?
Cu2 C22 2.032(8) . ?
Cu2 N6 2.084(5) . ?
Cu2 N5 2.130(5) . ?
F1 F2 1.03(4) . ?
F1 F2 1.19(3) 2_665 ?
F1 B1 1.365(11) . ?
F1 F2 1.53(4) 15_556 ?
F2 F1 1.19(3) 3_565 ?
F2 B1 1.331(19) . ?
F2 F1 1.53(4) 14_456 ?
F3 F4 0.99(4) 2_665 ?
F3 F4 1.27(4) . ?
F3 B2 1.426(11) . ?
F3 F4 1.70(4) 15 ?
F4 F3 0.99(4) 3_565 ?
F4 B2 1.368(19) . ?
F4 F3 1.70(4) 14_455 ?
F4 F4 1.76(6) 2_665 ?
F4 F4 1.76(6) 3_565 ?
F5 B3 1.361(12) . ?
F5 O4 1.40(2) . ?
F6 B3 1.312(11) . ?
F7 B3 1.372(13) . ?
F7 O4 1.40(3) . ?
F8 B3 1.287(11) . ?
F9 B4 1.220(16) . ?
F10 B4 1.348(16) . ?
F11 B4 1.319(15) . ?
F12 B4 1.328(18) . ?
O1 O5 0.70(3) . ?
O1 O2 0.98(3) . ?
O1 O3 1.72(3) . ?
O2 O3 0.97(2) . ?
O2 O5 1.54(4) . ?
O4 B3 1.48(3) . ?
N1 C4 1.344(8) . ?
N1 C1 1.357(8) . ?
N1 Cu1 2.029(5) 15_556 ?
N2 C1 1.336(8) . ?
N2 C2 1.347(7) . ?
N3 C9 1.361(8) . ?
N3 C5 1.363(7) . ?
N4 C12 1.333(8) . ?
N4 C15 1.366(8) . ?
N4 Cu2 2.017(5) 14_455 ?
N5 C12 1.319(8) . ?
N5 C13 1.346(7) . ?
N6 C20 1.323(8) . ?
N6 C16 1.334(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.389(8) . ?
C2 C5 1.467(8) . ?
C3 C4 1.389(9) . ?
C3 H2 0.9500 . ?
C4 H3 0.9500 . ?
C5 C6 1.370(8) . ?
C6 C7 1.394(9) . ?
C6 H4 0.9500 . ?
C7 C8 1.351(10) . ?
C7 H5 0.9500 . ?
C8 C9 1.330(10) . ?
C8 H6 0.9500 . ?
C9 H7 0.9500 . ?
C10 C11 1.297(12) . ?
C10 H8 0.9900 . ?
C10 H9 0.9900 . ?
C11 H10 0.9900 . ?
C11 H11 0.9900 . ?
C12 H12 0.9500 . ?
C13 C14 1.391(9) . ?
C13 C16 1.487(9) . ?
C14 C15 1.352(10) . ?
C14 H13 0.9500 . ?
C15 H14 0.9500 . ?
C16 C17 1.408(8) . ?
C17 C18 1.386(10) . ?
C17 H15 0.9500 . ?
C18 C19 1.362(11) . ?
C18 H16 0.9500 . ?
C19 C20 1.372(10) . ?
C19 H17 0.9500 . ?
C20 H18 0.9500 . ?
C21 C22 1.323(12) . ?
C21 H19 0.9900 . ?
C21 H20 0.9900 . ?
C22 H21 0.9900 . ?
C22 H22 0.9900 . ?
B1 F2 1.331(19) 15_556 ?
B1 F2 1.331(19) 3_565 ?
B1 F2 1.331(19) 2_665 ?
B1 F2 1.331(19) 14_456 ?
B1 F2 1.331(19) 13_566 ?
B1 F1 1.365(11) 14_456 ?
B1 F1 1.365(11) 2_665 ?
B1 F1 1.365(11) 3_565 ?
B1 F1 1.365(12) 15_556 ?
B1 F1 1.365(11) 13_566 ?
B2 F4 1.368(19) 13_565 ?
B2 F4 1.368(19) 14_455 ?
B2 F4 1.368(19) 2_665 ?
B2 F4 1.368(19) 3_565 ?
B2 F4 1.368(19) 15 ?
B2 F3 1.426(11) 13_565 ?
B2 F3 1.426(11) 15 ?
B2 F3 1.426(11) 3_565 ?
B2 F3 1.426(11) 2_665 ?
B2 F3 1.426(11) 14_455 ?

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
C10 Cu1 C11 37.4(3) . . ?
C10 Cu1 N1 139.2(4) . 14_456 ?
C11 Cu1 N1 102.5(3) . 14_456 ?
C10 Cu1 N3 107.7(4) . . ?
C11 Cu1 N3 137.1(4) . . ?
N1 Cu1 N3 101.73(19) 14_456 . ?
C10 Cu1 N2 109.2(4) . . ?
C11 Cu1 N2 128.1(4) . . ?
N1 Cu1 N2 103.96(19) 14_456 . ?
N3 Cu1 N2 78.29(19) . . ?
N4 Cu2 C21 140.7(3) 15 . ?
N4 Cu2 C22 102.7(4) 15 . ?
C21 Cu2 C22 38.1(3) . . ?
N4 Cu2 N6 106.6(2) 15 . ?
C21 Cu2 N6 104.8(3) . . ?
C22 Cu2 N6 133.8(4) . . ?
N4 Cu2 N5 103.2(2) 15 . ?
C21 Cu2 N5 106.0(4) . . ?
C22 Cu2 N5 128.4(4) . . ?
N6 Cu2 N5 78.0(2) . . ?
F2 F1 F2 119(3) . 2_665 ?
F2 F1 B1 65.8(15) . . ?
F2 F1 B1 62.3(14) 2_665 . ?
F2 F1 F2 90(3) . 15_556 ?
F2 F1 F2 84(2) 2_665 15_556 ?
B1 F1 F2 54.3(11) . 15_556 ?
F1 F2 F1 120(4) . 3_565 ?
F1 F2 B1 69.3(16) . . ?
F1 F2 B1 65.3(13) 3_565 . ?
F1 F2 F1 96(3) . 14_456 ?
F1 F2 F1 90(3) 3_565 14_456 ?
B1 F2 F1 56.4(13) . 14_456 ?
F4 F3 F4 103(4) 2_665 . ?
F4 F3 B2 66.2(16) 2_665 . ?
F4 F3 B2 60.7(13) . . ?
F4 F3 F4 99(3) 2_665 15 ?
F4 F3 F4 88(3) . 15 ?
B2 F3 F4 50.9(10) . 15 ?
F3 F4 F3 134(2) 3_565 . ?
F3 F4 B2 72.6(17) 3_565 . ?
F3 F4 B2 65.5(15) . . ?
F3 F4 F3 89(3) 3_565 14_455 ?
F3 F4 F3 81(2) . 14_455 ?
B2 F4 F3 54.0(13) . 14_455 ?
F3 F4 F4 104(3) 3_565 2_665 ?
B2 F4 F4 49.8(15) . 2_665 ?
F3 F4 F4 91.8(16) 14_455 2_665 ?
F3 F4 F4 92(2) . 3_565 ?
B2 F4 F4 49.8(15) . 3_565 ?
F3 F4 F4 97.9(12) 14_455 3_565 ?
F4 F4 F4 60.000(6) 2_665 3_565 ?
B3 F5 O4 64.5(13) . . ?
B3 F7 O4 64.5(12) . . ?
O5 O1 O2 131(5) . . ?
O5 O1 O3 110(4) . . ?
O3 O2 O1 123(3) . . ?
O3 O2 O5 109(2) . . ?
F7 O4 F5 102.7(16) . . ?
F7 O4 B3 57.0(11) . . ?
F5 O4 B3 56.3(10) . . ?
C4 N1 C1 116.0(5) . . ?
C4 N1 Cu1 121.2(4) . 15_556 ?
C1 N1 Cu1 122.8(4) . 15_556 ?
C1 N2 C2 118.5(5) . . ?
C1 N2 Cu1 127.3(4) . . ?
C2 N2 Cu1 114.1(4) . . ?
C9 N3 C5 116.9(6) . . ?
C9 N3 Cu1 127.3(4) . . ?
C5 N3 Cu1 115.8(4) . . ?
C12 N4 C15 115.2(6) . . ?
C12 N4 Cu2 121.3(4) . 14_455 ?
C15 N4 Cu2 123.5(4) . 14_455 ?
C12 N5 C13 117.3(5) . . ?
C12 N5 Cu2 127.6(4) . . ?
C13 N5 Cu2 115.1(4) . . ?
C20 N6 C16 118.3(6) . . ?
C20 N6 Cu2 126.2(5) . . ?
C16 N6 Cu2 115.4(4) . . ?
N2 C1 N1 124.8(5) . . ?
N2 C1 H1 117.6 . . ?
N1 C1 H1 117.6 . . ?
N2 C2 C3 120.6(5) . . ?
N2 C2 C5 116.3(5) . . ?
C3 C2 C5 123.1(5) . . ?
C4 C3 C2 117.2(6) . . ?
C4 C3 H2 121.4 . . ?
C2 C3 H2 121.4 . . ?
N1 C4 C3 122.9(6) . . ?
N1 C4 H3 118.6 . . ?
C3 C4 H3 118.6 . . ?
N3 C5 C6 121.7(6) . . ?
N3 C5 C2 115.4(5) . . ?
C6 C5 C2 122.9(5) . . ?
C5 C6 C7 118.1(6) . . ?
C5 C6 H4 121.0 . . ?
C7 C6 H4 121.0 . . ?
C8 C7 C6 120.5(7) . . ?
C8 C7 H5 119.7 . . ?
C6 C7 H5 119.7 . . ?
C9 C8 C7 118.7(7) . . ?
C9 C8 H6 120.6 . . ?
C7 C8 H6 120.6 . . ?
C8 C9 N3 124.1(7) . . ?
C8 C9 H7 118.0 . . ?
N3 C9 H7 118.0 . . ?
C11 C10 Cu1 71.6(6) . . ?
C11 C10 H8 116.4 . . ?
Cu1 C10 H8 116.4 . . ?
C11 C10 H9 116.4 . . ?
Cu1 C10 H9 116.4 . . ?
H8 C10 H9 113.4 . . ?
C10 C11 Cu1 71.0(6) . . ?
C10 C11 H10 116.5 . . ?
Cu1 C11 H10 116.5 . . ?
C10 C11 H11 116.5 . . ?
Cu1 C11 H11 116.5 . . ?
H10 C11 H11 113.5 . . ?
N5 C12 N4 126.7(6) . . ?
N5 C12 H12 116.6 . . ?
N4 C12 H12 116.6 . . ?
N5 C13 C14 120.4(6) . . ?
N5 C13 C16 114.3(6) . . ?
C14 C13 C16 125.3(5) . . ?
C15 C14 C13 118.1(6) . . ?
C15 C14 H13 120.9 . . ?
C13 C14 H13 120.9 . . ?
C14 C15 N4 122.2(6) . . ?
C14 C15 H14 118.9 . . ?
N4 C15 H14 118.9 . . ?
N6 C16 C17 122.8(6) . . ?
N6 C16 C13 117.2(5) . . ?
C17 C16 C13 119.9(6) . . ?
C18 C17 C16 116.8(7) . . ?
C18 C17 H15 121.6 . . ?
C16 C17 H15 121.6 . . ?
C19 C18 C17 119.8(7) . . ?
C19 C18 H16 120.1 . . ?
C17 C18 H16 120.1 . . ?
C18 C19 C20 119.5(7) . . ?
C18 C19 H17 120.2 . . ?
C20 C19 H17 120.2 . . ?
N6 C20 C19 122.7(7) . . ?
N6 C20 H18 118.7 . . ?
C19 C20 H18 118.7 . . ?
C22 C21 Cu2 71.2(6) . . ?
C22 C21 H19 116.5 . . ?
Cu2 C21 H19 116.5 . . ?
C22 C21 H20 116.5 . . ?
Cu2 C21 H20 116.5 . . ?
H19 C21 H20 113.5 . . ?
C21 C22 Cu2 70.8(5) . . ?
C21 C22 H21 116.5 . . ?
Cu2 C22 H21 116.5 . . ?
C21 C22 H22 116.5 . . ?
Cu2 C22 H22 116.5 . . ?
H21 C22 H22 113.5 . . ?
F2 B1 F2 179.995(8) 15_556 3_565 ?
F2 B1 F2 88(3) 15_556 2_665 ?
F2 B1 F2 92(3) 3_565 2_665 ?
F2 B1 F2 92(3) 15_556 14_456 ?
F2 B1 F2 88(3) 3_565 14_456 ?
F2 B1 F2 179.994(15) 2_665 14_456 ?
F2 B1 F2 88(3) 15_556 . ?
F2 B1 F2 92(3) 3_565 . ?
F2 B1 F2 92(3) 2_665 . ?
F2 B1 F2 88(3) 14_456 . ?
F2 B1 F2 92(3) 15_556 13_566 ?
F2 B1 F2 88(3) 3_565 13_566 ?
F2 B1 F2 88(3) 2_665 13_566 ?
F2 B1 F2 92(3) 14_456 13_566 ?
F2 B1 F2 180(4) . 13_566 ?
F2 B1 F1 52.4(16) 15_556 14_456 ?
F2 B1 F1 127.6(16) 3_565 14_456 ?
F2 B1 F1 135.2(19) 2_665 14_456 ?
F2 B1 F1 45(2) 14_456 14_456 ?
F2 B1 F1 69.3(19) . 14_456 ?
F2 B1 F1 110.7(19) 13_566 14_456 ?
F2 B1 F1 127.6(16) 15_556 2_665 ?
F2 B1 F1 52.4(16) 3_565 2_665 ?
F2 B1 F1 135.2(19) 14_456 2_665 ?
F2 B1 F1 110.7(19) . 2_665 ?
F2 B1 F1 69.3(19) 13_566 2_665 ?
F1 B1 F1 179.995(7) 14_456 2_665 ?
F2 B1 F1 135.2(19) 15_556 3_565 ?
F2 B1 F1 110.7(19) 2_665 3_565 ?
F2 B1 F1 69.3(19) 14_456 3_565 ?
F2 B1 F1 52.4(16) . 3_565 ?
F2 B1 F1 127.6(16) 13_566 3_565 ?
F1 B1 F1 90.3(11) 14_456 3_565 ?
F1 B1 F1 89.7(11) 2_665 3_565 ?
F2 B1 F1 69.3(19) 15_556 . ?
F2 B1 F1 110.7(19) 3_565 . ?
F2 B1 F1 52.4(16) 2_665 . ?
F2 B1 F1 127.6(16) 14_456 . ?
F2 B1 F1 45(2) . . ?
F2 B1 F1 135(2) 13_566 . ?
F1 B1 F1 90.3(11) 14_456 . ?
F1 B1 F1 89.7(11) 2_665 . ?
F1 B1 F1 89.7(11) 3_565 . ?
F2 B1 F1 135.2(19) 3_565 15_556 ?
F2 B1 F1 69.3(19) 2_665 15_556 ?
F2 B1 F1 110.7(19) 14_456 15_556 ?
F2 B1 F1 127.6(16) . 15_556 ?
F2 B1 F1 52.4(16) 13_566 15_556 ?
F1 B1 F1 89.7(11) 14_456 15_556 ?
F1 B1 F1 90.3(11) 2_665 15_556 ?
F1 B1 F1 180.0(12) 3_565 15_556 ?
F1 B1 F1 90.3(11) . 15_556 ?
F2 B1 F1 110.7(19) 15_556 13_566 ?
F2 B1 F1 69.3(19) 3_565 13_566 ?
F2 B1 F1 127.6(16) 2_665 13_566 ?
F2 B1 F1 52.4(16) 14_456 13_566 ?
F2 B1 F1 135(2) . 13_566 ?
F2 B1 F1 45(2) 13_566 13_566 ?
F1 B1 F1 89.7(11) 14_456 13_566 ?
F1 B1 F1 90.3(11) 2_665 13_566 ?
F1 B1 F1 90.3(12) 3_565 13_566 ?
F1 B1 F1 180.0(8) . 13_566 ?
F1 B1 F1 89.7(11) 15_556 13_566 ?
F4 B2 F4 80(3) 13_565 14_455 ?
F4 B2 F4 179.998(12) 13_565 . ?
F4 B2 F4 100(3) 14_455 . ?
F4 B2 F4 100(3) 13_565 2_665 ?
F4 B2 F4 179.994(11) 14_455 2_665 ?
F4 B2 F4 80(3) . 2_665 ?
F4 B2 F4 100(3) 13_565 3_565 ?
F4 B2 F4 100(3) 14_455 3_565 ?
F4 B2 F4 80(3) . 3_565 ?
F4 B2 F4 80(3) 2_665 3_565 ?
F4 B2 F4 80(3) 13_565 15 ?
F4 B2 F4 80(3) 14_455 15 ?
F4 B2 F4 100(3) . 15 ?
F4 B2 F4 100(3) 2_665 15 ?
F4 B2 F4 179.995(8) 3_565 15 ?
F4 B2 F3 54(2) 13_565 13_565 ?
F4 B2 F3 126(2) . 13_565 ?
F4 B2 F3 138.8(19) 2_665 13_565 ?
F4 B2 F3 75.1(18) 3_565 13_565 ?
F4 B2 F3 104.9(18) 15 13_565 ?
F4 B2 F3 104.9(18) 14_455 15 ?
F4 B2 F3 138.8(19) . 15 ?
F4 B2 F3 75.1(18) 2_665 15 ?
F4 B2 F3 126(2) 3_565 15 ?
F4 B2 F3 54(2) 15 15 ?
F3 B2 F3 93.4(9) 13_565 15 ?
F4 B2 F3 126(2) 13_565 . ?
F4 B2 F3 138.8(19) 14_455 . ?
F4 B2 F3 54(2) . . ?
F4 B2 F3 104.9(18) 3_565 . ?
F4 B2 F3 75.1(18) 15 . ?
F3 B2 F3 179.996(3) 13_565 . ?
F3 B2 F3 86.6(9) 15 . ?
F4 B2 F3 138.8(19) 13_565 3_565 ?
F4 B2 F3 75.1(18) 14_455 3_565 ?
F4 B2 F3 104.9(18) 2_665 3_565 ?
F4 B2 F3 54(2) 3_565 3_565 ?
F4 B2 F3 126(2) 15 3_565 ?
F3 B2 F3 86.6(9) 13_565 3_565 ?
F3 B2 F3 180.0(11) 15 3_565 ?
F3 B2 F3 93.4(9) . 3_565 ?
F4 B2 F3 75.1(18) 13_565 2_665 ?
F4 B2 F3 126(2) 14_455 2_665 ?
F4 B2 F3 104.9(18) . 2_665 ?
F4 B2 F3 54(2) 2_665 2_665 ?
F4 B2 F3 138.8(19) 15 2_665 ?
F3 B2 F3 86.6(9) 13_565 2_665 ?
F3 B2 F3 86.6(9) 15 2_665 ?
F3 B2 F3 93.4(9) . 2_665 ?
F3 B2 F3 93.4(9) 3_565 2_665 ?
F4 B2 F3 104.9(18) 13_565 14_455 ?
F4 B2 F3 54(2) 14_455 14_455 ?
F4 B2 F3 75.1(18) . 14_455 ?
F4 B2 F3 126(2) 2_665 14_455 ?
F4 B2 F3 138.8(19) 3_565 14_455 ?
F3 B2 F3 93.4(9) 13_565 14_455 ?
F3 B2 F3 93.4(9) 15 14_455 ?
F3 B2 F3 86.6(9) . 14_455 ?
F3 B2 F3 86.6(9) 3_565 14_455 ?
F3 B2 F3 179.995(5) 2_665 14_455 ?
F8 B3 F6 114.7(9) . . ?
F8 B3 F5 111.9(8) . . ?
F6 B3 F5 106.7(9) . . ?
F8 B3 F7 107.6(9) . . ?
F6 B3 F7 109.3(8) . . ?
F5 B3 F7 106.3(10) . . ?
F8 B3 O4 94.0(11) . . ?
F6 B3 O4 151.3(12) . . ?
F5 B3 O4 59.2(10) . . ?
F7 B3 O4 58.5(10) . . ?
F9 B4 F11 110.0(12) . . ?
F9 B4 F12 120.6(17) . . ?
F11 B4 F12 101.2(14) . . ?
F9 B4 F10 110.2(15) . . ?
F11 B4 F10 109.7(12) . . ?
F12 B4 F10 104.5(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F2 F1 F2 F1 9(10) 2_665 . . 3_565 ?
B1 F1 F2 F1 43(4) . . . 3_565 ?
F2 F1 F2 F1 93(6) 15_556 . . 3_565 ?
F2 F1 F2 B1 -33(6) 2_665 . . . ?
F2 F1 F2 B1 50(2) 15_556 . . . ?
F2 F1 F2 F1 -84(6) 2_665 . . 14_456 ?
B1 F1 F2 F1 -50.6(10) . . . 14_456 ?
F2 F1 F2 F1 0(3) 15_556 . . 14_456 ?
F4 F3 F4 F3 28(10) 2_665 . . 3_565 ?
B2 F3 F4 F3 -26(6) . . . 3_565 ?
F4 F3 F4 F3 -71(8) 15 . . 3_565 ?
F4 F3 F4 B2 53(4) 2_665 . . . ?
F4 F3 F4 B2 -45(2) 15 . . . ?
F4 F3 F4 F3 108(4) 2_665 . . 14_455 ?
B2 F3 F4 F3 54.4(8) . . . 14_455 ?
F4 F3 F4 F3 9.3(18) 15 . . 14_455 ?
B2 F3 F4 F4 -53(4) . . . 2_665 ?
F4 F3 F4 F4 -98(3) 15 . . 2_665 ?
F4 F3 F4 F4 10(3) 2_665 . . 3_565 ?
B2 F3 F4 F4 -43.2(11) . . . 3_565 ?
F4 F3 F4 F4 -88.2(16) 15 . . 3_565 ?
O5 O1 O2 O3 -47(6) . . . . ?
O3 O1 O2 O5 47(7) . . . . ?
O5 O2 O3 O1 -15(2) . . . . ?
O5 O1 O3 O2 144(6) . . . . ?
B3 F7 O4 F5 34.4(12) . . . . ?
B3 F5 O4 F7 -34.7(12) . . . . ?
O3 O1 O5 O2 -21(3) . . . . ?
O3 O2 O5 O1 140(6) . . . . ?
C10 Cu1 N2 C1 73.6(6) . . . . ?
C11 Cu1 N2 C1 36.4(7) . . . . ?
N1 Cu1 N2 C1 -82.2(5) 14_456 . . . ?
N3 Cu1 N2 C1 178.5(5) . . . . ?
C10 Cu1 N2 C2 -106.8(5) . . . . ?
C11 Cu1 N2 C2 -143.9(5) . . . . ?
N1 Cu1 N2 C2 97.4(4) 14_456 . . . ?
N3 Cu1 N2 C2 -1.9(4) . . . . ?
C10 Cu1 N3 C9 -73.0(7) . . . . ?
C11 Cu1 N3 C9 -45.0(8) . . . . ?
N1 Cu1 N3 C9 78.3(5) 14_456 . . . ?
N2 Cu1 N3 C9 -179.7(5) . . . . ?
C10 Cu1 N3 C5 109.6(6) . . . . ?
C11 Cu1 N3 C5 137.6(6) . . . . ?
N1 Cu1 N3 C5 -99.1(4) 14_456 . . . ?
N2 Cu1 N3 C5 3.0(4) . . . . ?
N4 Cu2 N5 C12 -77.3(5) 15 . . . ?
C21 Cu2 N5 C12 76.1(6) . . . . ?
C22 Cu2 N5 C12 40.9(7) . . . . ?
N6 Cu2 N5 C12 178.2(5) . . . . ?
N4 Cu2 N5 C13 105.2(4) 15 . . . ?
C21 Cu2 N5 C13 -101.4(5) . . . . ?
C22 Cu2 N5 C13 -136.6(5) . . . . ?
N6 Cu2 N5 C13 0.7(4) . . . . ?
N4 Cu2 N6 C20 77.7(6) 15 . . . ?
C21 Cu2 N6 C20 -78.3(7) . . . . ?
C22 Cu2 N6 C20 -49.5(8) . . . . ?
N5 Cu2 N6 C20 178.0(6) . . . . ?
N4 Cu2 N6 C16 -100.0(5) 15 . . . ?
C21 Cu2 N6 C16 103.9(6) . . . . ?
C22 Cu2 N6 C16 132.8(6) . . . . ?
N5 Cu2 N6 C16 0.3(4) . . . . ?
C2 N2 C1 N1 -0.7(8) . . . . ?
Cu1 N2 C1 N1 179.0(4) . . . . ?
C4 N1 C1 N2 0.1(9) . . . . ?
Cu1 N1 C1 N2 -179.5(4) 15_556 . . . ?
C1 N2 C2 C3 1.0(8) . . . . ?
Cu1 N2 C2 C3 -178.7(5) . . . . ?
C1 N2 C2 C5 -179.7(5) . . . . ?
Cu1 N2 C2 C5 0.6(6) . . . . ?
N2 C2 C3 C4 -0.7(9) . . . . ?
C5 C2 C3 C4 179.9(6) . . . . ?
C1 N1 C4 C3 0.1(9) . . . . ?
Cu1 N1 C4 C3 179.7(5) 15_556 . . . ?
C2 C3 C4 N1 0.2(10) . . . . ?
C9 N3 C5 C6 0.4(9) . . . . ?
Cu1 N3 C5 C6 178.1(5) . . . . ?
C9 N3 C5 C2 178.8(5) . . . . ?
Cu1 N3 C5 C2 -3.5(6) . . . . ?
N2 C2 C5 N3 1.9(8) . . . . ?
C3 C2 C5 N3 -178.8(6) . . . . ?
N2 C2 C5 C6 -179.8(5) . . . . ?
C3 C2 C5 C6 -0.4(9) . . . . ?
N3 C5 C6 C7 -1.1(9) . . . . ?
C2 C5 C6 C7 -179.3(6) . . . . ?
C5 C6 C7 C8 1.2(10) . . . . ?
C6 C7 C8 C9 -0.6(11) . . . . ?
C7 C8 C9 N3 -0.1(11) . . . . ?
C5 N3 C9 C8 0.2(10) . . . . ?
Cu1 N3 C9 C8 -177.1(5) . . . . ?
N1 Cu1 C10 C11 14.1(14) 14_456 . . . ?
N3 Cu1 C10 C11 148.2(9) . . . . ?
N2 Cu1 C10 C11 -128.4(10) . . . . ?
N1 Cu1 C11 C10 -170.6(9) 14_456 . . . ?
N3 Cu1 C11 C10 -47.6(13) . . . . ?
N2 Cu1 C11 C10 70.2(11) . . . . ?
C13 N5 C12 N4 0.7(9) . . . . ?
Cu2 N5 C12 N4 -176.8(4) . . . . ?
C15 N4 C12 N5 0.9(9) . . . . ?
Cu2 N4 C12 N5 179.3(5) 14_455 . . . ?
C12 N5 C13 C14 -0.4(9) . . . . ?
Cu2 N5 C13 C14 177.4(5) . . . . ?
C12 N5 C13 C16 -179.2(5) . . . . ?
Cu2 N5 C13 C16 -1.4(7) . . . . ?
N5 C13 C14 C15 -1.5(10) . . . . ?
C16 C13 C14 C15 177.2(7) . . . . ?
C13 C14 C15 N4 3.2(12) . . . . ?
C12 N4 C15 C14 -2.8(10) . . . . ?
Cu2 N4 C15 C14 178.8(6) 14_455 . . . ?
C20 N6 C16 C17 1.6(10) . . . . ?
Cu2 N6 C16 C17 179.5(5) . . . . ?
C20 N6 C16 C13 -179.1(6) . . . . ?
Cu2 N6 C16 C13 -1.1(7) . . . . ?
N5 C13 C16 N6 1.7(8) . . . . ?
C14 C13 C16 N6 -177.1(6) . . . . ?
N5 C13 C16 C17 -178.9(6) . . . . ?
C14 C13 C16 C17 2.3(10) . . . . ?
N6 C16 C17 C18 0.0(10) . . . . ?
C13 C16 C17 C18 -179.4(6) . . . . ?
C16 C17 C18 C19 -1.3(11) . . . . ?
C17 C18 C19 C20 1.0(12) . . . . ?
C16 N6 C20 C19 -1.8(11) . . . . ?
Cu2 N6 C20 C19 -179.5(6) . . . . ?
C18 C19 C20 N6 0.6(12) . . . . ?
N4 Cu2 C21 C22 3.6(11) 15 . . . ?
N6 Cu2 C21 C22 145.7(8) . . . . ?
N5 Cu2 C21 C22 -132.9(8) . . . . ?
N4 Cu2 C22 C21 -177.7(7) 15 . . . ?
N6 Cu2 C22 C21 -49.1(11) . . . . ?
N5 Cu2 C22 C21 63.9(9) . . . . ?
F1 F2 B1 F2 -62.4(17) . . . 15_556 ?
F1 F2 B1 F2 158(4) 3_565 . . 15_556 ?
F1 F2 B1 F2 50(2) 14_456 . . 15_556 ?
F1 F2 B1 F2 117.6(17) . . . 3_565 ?
F1 F2 B1 F2 -22(4) 3_565 . . 3_565 ?
F1 F2 B1 F2 -130(2) 14_456 . . 3_565 ?
F1 F2 B1 F2 25(5) . . . 2_665 ?
F1 F2 B1 F2 -114.6(10) 3_565 . . 2_665 ?
F1 F2 B1 F2 138(3) 14_456 . . 2_665 ?
F1 F2 B1 F2 -155(5) . . . 14_456 ?
F1 F2 B1 F2 65.4(10) 3_565 . . 14_456 ?
F1 F2 B1 F2 -42(3) 14_456 . . 14_456 ?
F1 F2 B1 F1 -113(3) . . . 14_456 ?
F1 F2 B1 F1 107(3) 3_565 . . 14_456 ?
F1 F2 B1 F1 67(3) . . . 2_665 ?
F1 F2 B1 F1 -73(3) 3_565 . . 2_665 ?
F1 F2 B1 F1 180.00(4) 14_456 . . 2_665 ?
F1 F2 B1 F1 140(5) . . . 3_565 ?
F1 F2 B1 F1 -107(3) 14_456 . . 3_565 ?
F1 F2 B1 F1 -140(5) 3_565 . . . ?
F1 F2 B1 F1 113(3) 14_456 . . . ?
F1 F2 B1 F1 -40(5) . . . 15_556 ?
F1 F2 B1 F1 180.000(14) 3_565 . . 15_556 ?
F1 F2 B1 F1 73(3) 14_456 . . 15_556 ?
F1 F2 B1 F1 179.998(8) . . . 13_566 ?
F1 F2 B1 F1 40(5) 3_565 . . 13_566 ?
F1 F2 B1 F1 -67(3) 14_456 . . 13_566 ?
F2 F1 B1 F2 109(4) . . . 15_556 ?
F2 F1 B1 F2 -104(3) 2_665 . . 15_556 ?
F2 F1 B1 F2 -71(4) . . . 3_565 ?
F2 F1 B1 F2 76(3) 2_665 . . 3_565 ?
F2 F1 B1 F2 179.997(7) 15_556 . . 3_565 ?
F2 F1 B1 F2 -147(7) . . . 2_665 ?
F2 F1 B1 F2 104(3) 15_556 . . 2_665 ?
F2 F1 B1 F2 33(7) . . . 14_456 ?
F2 F1 B1 F2 180.001(19) 2_665 . . 14_456 ?
F2 F1 B1 F2 -76(3) 15_556 . . 14_456 ?
F2 F1 B1 F2 147(7) 2_665 . . . ?
F2 F1 B1 F2 -109(4) 15_556 . . . ?
F2 F1 B1 F2 180.002(6) . . . 13_566 ?
F2 F1 B1 F2 -33(7) 2_665 . . 13_566 ?
F2 F1 B1 F2 71(4) 15_556 . . 13_566 ?
F2 F1 B1 F1 60(3) . . . 14_456 ?
F2 F1 B1 F1 149(4) . . . 15_556 ?
F2 F1 B1 F1 -63(3) 2_665 . . 15_556 ?
F2 F1 B1 F1 40.5(18) 15_556 . . 15_556 ?
F3 F4 B2 F4 -54(2) 3_565 . . 14_455 ?
F3 F4 B2 F4 145(3) . . . 14_455 ?
F3 F4 B2 F4 48(3) 14_455 . . 14_455 ?
F4 F4 B2 F4 179.997(13) 2_665 . . 14_455 ?
F4 F4 B2 F4 -98(2) 3_565 . . 14_455 ?
F3 F4 B2 F4 126(2) 3_565 . . 2_665 ?
F3 F4 B2 F4 -35(3) . . . 2_665 ?
F3 F4 B2 F4 -132(3) 14_455 . . 2_665 ?
F4 F4 B2 F4 82(2) 3_565 . . 2_665 ?
F3 F4 B2 F4 44(4) 3_565 . . 3_565 ?
F3 F4 B2 F4 -116.6(16) . . . 3_565 ?
F3 F4 B2 F4 147(2) 14_455 . . 3_565 ?
F4 F4 B2 F4 -82(2) 2_665 . . 3_565 ?
F3 F4 B2 F4 -136(4) 3_565 . . 15 ?
F3 F4 B2 F4 63.4(16) . . . 15 ?
F3 F4 B2 F4 -33(2) 14_455 . . 15 ?
F4 F4 B2 F4 98(2) 2_665 . . 15 ?
F4 F4 B2 F4 180.000(17) 3_565 . . 15 ?
F3 F4 B2 F3 -19(5) 3_565 . . 13_565 ?
F3 F4 B2 F3 179.998(3) . . . 13_565 ?
F3 F4 B2 F3 83(2) 14_455 . . 13_565 ?
F4 F4 B2 F3 -145(3) 2_665 . . 13_565 ?
F4 F4 B2 F3 -63.4(16) 3_565 . . 13_565 ?
F3 F4 B2 F3 180.002(2) 3_565 . . 15 ?
F3 F4 B2 F3 19(5) . . . 15 ?
F3 F4 B2 F3 -78(3) 14_455 . . 15 ?
F4 F4 B2 F3 54(2) 2_665 . . 15 ?
F4 F4 B2 F3 136(4) 3_565 . . 15 ?
F3 F4 B2 F3 161(5) 3_565 . . . ?
F3 F4 B2 F3 -97(2) 14_455 . . . ?
F4 F4 B2 F3 35(3) 2_665 . . . ?
F4 F4 B2 F3 116.6(16) 3_565 . . . ?
F3 F4 B2 F3 -161(5) . . . 3_565 ?
F3 F4 B2 F3 102(3) 14_455 . . 3_565 ?
F4 F4 B2 F3 -126(2) 2_665 . . 3_565 ?
F4 F4 B2 F3 -44(4) 3_565 . . 3_565 ?
F3 F4 B2 F3 78(3) 3_565 . . 2_665 ?
F3 F4 B2 F3 -83(2) . . . 2_665 ?
F3 F4 B2 F3 180.002(18) 14_455 . . 2_665 ?
F4 F4 B2 F3 -48(3) 2_665 . . 2_665 ?
F4 F4 B2 F3 33(2) 3_565 . . 2_665 ?
F3 F4 B2 F3 -102(3) 3_565 . . 14_455 ?
F3 F4 B2 F3 97(2) . . . 14_455 ?
F4 F4 B2 F3 132(3) 2_665 . . 14_455 ?
F4 F4 B2 F3 -147(2) 3_565 . . 14_455 ?
F4 F3 B2 F4 59(6) 2_665 . . 13_565 ?
F4 F3 B2 F4 180.002(4) . . . 13_565 ?
F4 F3 B2 F4 -66(3) 15 . . 13_565 ?
F4 F3 B2 F4 180.003(9) 2_665 . . 14_455 ?
F4 F3 B2 F4 -59(6) . . . 14_455 ?
F4 F3 B2 F4 55(4) 15 . . 14_455 ?
F4 F3 B2 F4 -121(6) 2_665 . . . ?
F4 F3 B2 F4 114(3) 15 . . . ?
F4 F3 B2 F4 121(6) . . . 2_665 ?
F4 F3 B2 F4 -125(4) 15 . . 2_665 ?
F4 F3 B2 F4 -55(4) 2_665 . . 3_565 ?
F4 F3 B2 F4 66(3) . . . 3_565 ?
F4 F3 B2 F4 179.996(6) 15 . . 3_565 ?
F4 F3 B2 F4 125(4) 2_665 . . 15 ?
F4 F3 B2 F4 -114(3) . . . 15 ?
F4 F3 B2 F3 71(3) 2_665 . . 15 ?
F4 F3 B2 F3 -168(3) . . . 15 ?
F4 F3 B2 F3 -53(2) 15 . . 15 ?
F4 F3 B2 F3 -109(3) 2_665 . . 3_565 ?
F4 F3 B2 F3 12(3) . . . 3_565 ?
F4 F3 B2 F3 127(2) 15 . . 3_565 ?
F4 F3 B2 F3 -15(4) 2_665 . . 2_665 ?
F4 F3 B2 F3 106(2) . . . 2_665 ?
F4 F3 B2 F3 -140(2) 15 . . 2_665 ?
F4 F3 B2 F3 165(4) 2_665 . . 14_455 ?
F4 F3 B2 F3 -74(2) . . . 14_455 ?
F4 F3 B2 F3 40(2) 15 . . 14_455 ?
O4 F5 B3 F8 -81.2(13) . . . . ?
O4 F5 B3 F6 152.6(13) . . . . ?
O4 F5 B3 F7 36.0(11) . . . . ?
O4 F7 B3 F8 83.8(12) . . . . ?
O4 F7 B3 F6 -151.1(13) . . . . ?
O4 F7 B3 F5 -36.3(11) . . . . ?
F7 O4 B3 F8 -108.2(9) . . . . ?
F5 O4 B3 F8 113.2(9) . . . . ?
F7 O4 B3 F6 72(3) . . . . ?
F5 O4 B3 F6 -67(3) . . . . ?
F7 O4 B3 F5 138.6(12) . . . . ?
F5 O4 B3 F7 -138.6(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.091
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.157

#------------------------------------------------------------------------------
#------------------------------------------------------------------------------

### END