# Electronic Supplementary Material (ESI) for Dalton Transactions.
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# 
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#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_[Mn(DPFN)2][NO3]2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Mn(DPFN)2][NO3]2'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C60 H40 F4 Mn N12 2+, 2(N O3 1-), 1.5(C4 H8 O), 0.5(C H4 O)'
_chemical_formula_sum            'C66.5 H54 F4 Mn N14 O8'
_chemical_formula_weight         1308.17

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.4808(5)
_cell_length_b                   25.9908(10)
_cell_length_c                   17.5035(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.029(2)
_cell_angle_gamma                90.00
_cell_volume                     5949.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9360
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.33

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2588
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51309
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.35
_reflns_number_total             10866
_reflns_number_gt                7963
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_refine_special_details          SQUEEZE
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.160 0.230 -0.035 102 30 '0.5 CH3OH, 0.5 C4H8O'
2 0.160 0.270 0.465 102 30 '0.5 CH3OH, 0.5 C4H8O'
3 0.840 0.770 0.035 102 30 '0.5 CH3OH, 0.5 C4H8O'
4 0.840 0.730 0.535 102 30 '0.5 CH3OH, 0.5 C4H8O'
_platon_squeeze_details          
;
The unit cell contains one highly disordered solvate site
containing a 50:50 mixture of methanol and tetrahydrofuran
which has been treated as a diffuse contrbution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0588P)²+1.0606P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10866
_refine_ls_number_parameters     821
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.44121(18) 0.58586(9) 0.37814(14) 0.0231(6) Uani 1 1 d . . .
C2 C 0.4458(2) 0.58562(10) 0.45925(14) 0.0278(6) Uani 1 1 d . . .
H2 H 0.5053 0.5758 0.4956 0.033 Uiso 1 1 calc R . .
C3 C 0.3612(2) 0.60010(10) 0.48334(14) 0.0268(6) Uani 1 1 d . . .
H3 H 0.3627 0.6004 0.5367 0.032 Uiso 1 1 calc R . .
C4 C 0.1779(2) 0.62860(9) 0.44546(14) 0.0240(6) Uani 1 1 d . . .
H4 H 0.1713 0.6275 0.4971 0.029 Uiso 1 1 calc R . .
C5 C 0.09842(19) 0.64348(9) 0.38654(14) 0.0235(6) Uani 1 1 d . . .
H5 H 0.0367 0.6532 0.3971 0.028 Uiso 1 1 calc R . .
C6 C 0.11096(18) 0.64405(9) 0.30786(13) 0.0202(5) Uani 1 1 d . . .
C7 C 0.27462(17) 0.61493(9) 0.34786(13) 0.0187(5) Uani 1 1 d . . .
C8 C 0.27147(19) 0.61463(9) 0.42779(13) 0.0217(5) Uani 1 1 d . . .
C9 C 0.53300(18) 0.56856(10) 0.34771(14) 0.0257(6) Uani 1 1 d . . .
C10 C 0.02373(18) 0.66455(10) 0.24229(13) 0.0219(5) Uani 1 1 d . . .
C11 C 0.51116(17) 0.51867(9) 0.30051(13) 0.0203(5) Uani 1 1 d . . .
C12 C 0.56530(19) 0.47416(10) 0.32600(14) 0.0256(6) Uani 1 1 d . . .
H12 H 0.6169 0.4742 0.3722 0.031 Uiso 1 1 calc R . .
C13 C 0.54210(19) 0.43005(10) 0.28244(15) 0.0261(6) Uani 1 1 d . . .
H13 H 0.5777 0.3997 0.2987 0.031 Uiso 1 1 calc R . .
C14 C 0.46506(19) 0.43127(10) 0.21403(14) 0.0238(6) Uani 1 1 d . . .
H14 H 0.4476 0.4018 0.1837 0.029 Uiso 1 1 calc R . .
C15 C 0.41467(18) 0.47699(9) 0.19162(13) 0.0199(5) Uani 1 1 d . . .
H15 H 0.3630 0.4777 0.1455 0.024 Uiso 1 1 calc R . .
C16 C 0.57162(19) 0.61076(10) 0.30190(16) 0.0285(6) Uani 1 1 d . . .
C17 C 0.6687(2) 0.63151(11) 0.3299(2) 0.0408(8) Uani 1 1 d . . .
H17 H 0.7100 0.6209 0.3779 0.049 Uiso 1 1 calc R . .
C18 C 0.7023(2) 0.66782(12) 0.2853(3) 0.0551(10) Uani 1 1 d . . .
H18 H 0.7666 0.6826 0.3031 0.066 Uiso 1 1 calc R . .
C19 C 0.6401(2) 0.68232(11) 0.2139(2) 0.0516(9) Uani 1 1 d . . .
H19 H 0.6626 0.7061 0.1821 0.062 Uiso 1 1 calc R . .
C20 C 0.5442(2) 0.66094(10) 0.19049(19) 0.0362(7) Uani 1 1 d . . .
H20 H 0.5018 0.6714 0.1429 0.043 Uiso 1 1 calc R . .
C21 C 0.00070(18) 0.71955(10) 0.26414(14) 0.0237(6) Uani 1 1 d . . .
C22 C 0.0611(2) 0.75997(11) 0.25265(17) 0.0353(7) Uani 1 1 d . . .
H22 H 0.1131 0.7547 0.2270 0.042 Uiso 1 1 calc R . .
C23 C 0.0444(2) 0.80803(11) 0.27916(18) 0.0398(7) Uani 1 1 d . . .
H23 H 0.0847 0.8358 0.2718 0.048 Uiso 1 1 calc R . .
C24 C -0.0329(2) 0.81438(11) 0.31671(17) 0.0355(7) Uani 1 1 d . . .
H24 H -0.0473 0.8467 0.3343 0.043 Uiso 1 1 calc R . .
C25 C -0.0886(2) 0.77195(11) 0.32785(17) 0.0369(7) Uani 1 1 d . . .
H25 H -0.1397 0.7764 0.3547 0.044 Uiso 1 1 calc R . .
C26 C -0.06758(19) 0.62856(9) 0.22235(14) 0.0221(5) Uani 1 1 d . . .
C27 C -0.1422(2) 0.63526(11) 0.15265(15) 0.0297(6) Uani 1 1 d . . .
H27 H -0.1389 0.6629 0.1196 0.036 Uiso 1 1 calc R . .
C28 C -0.2213(2) 0.60022(11) 0.13334(16) 0.0342(7) Uani 1 1 d . . .
H28 H -0.2715 0.6035 0.0867 0.041 Uiso 1 1 calc R . .
C29 C -0.2245(2) 0.56026(11) 0.18438(16) 0.0352(7) Uani 1 1 d . . .
H29 H -0.2767 0.5360 0.1728 0.042 Uiso 1 1 calc R . .
C30 C -0.1488(2) 0.55699(10) 0.25288(16) 0.0328(6) Uani 1 1 d . . .
H30 H -0.1519 0.5301 0.2873 0.039 Uiso 1 1 calc R . .
C31 C 0.13352(18) 0.58185(9) 0.06999(13) 0.0211(5) Uani 1 1 d . . .
C32 C 0.02960(18) 0.57007(10) 0.03886(14) 0.0226(6) Uani 1 1 d . . .
H32 H -0.0072 0.5859 -0.0069 0.027 Uiso 1 1 calc R . .
C33 C -0.01596(18) 0.53513(10) 0.07701(13) 0.0221(6) Uani 1 1 d . . .
H33 H -0.0845 0.5267 0.0573 0.027 Uiso 1 1 calc R . .
C34 C 0.00268(18) 0.47403(10) 0.18999(14) 0.0243(6) Uani 1 1 d . . .
H34 H -0.0645 0.4627 0.1731 0.029 Uiso 1 1 calc R . .
C35 C 0.06441(18) 0.45452(9) 0.25647(14) 0.0237(6) Uani 1 1 d . . .
H35 H 0.0404 0.4296 0.2856 0.028 Uiso 1 1 calc R . .
C36 C 0.16620(18) 0.47279(9) 0.28090(14) 0.0197(5) Uani 1 1 d . . .
C37 C 0.14344(17) 0.52653(9) 0.17501(13) 0.0175(5) Uani 1 1 d . . .
C38 C 0.04078(17) 0.51167(9) 0.14643(13) 0.0197(5) Uani 1 1 d . . .
C39 C 0.18919(18) 0.61924(10) 0.02810(13) 0.0243(6) Uani 1 1 d . . .
C40 C 0.23819(18) 0.45106(9) 0.35544(14) 0.0214(5) Uani 1 1 d . . .
C41 C 0.21534(19) 0.66988(10) 0.07219(14) 0.0254(6) Uani 1 1 d . . .
C42 C 0.1739(2) 0.71610(11) 0.04052(17) 0.0371(7) Uani 1 1 d . . .
H42 H 0.1275 0.7171 -0.0084 0.045 Uiso 1 1 calc R . .
C43 C 0.2027(2) 0.76037(12) 0.0827(2) 0.0453(8) Uani 1 1 d . . .
H43 H 0.1758 0.7919 0.0624 0.054 Uiso 1 1 calc R . .
C44 C 0.2717(2) 0.75830(10) 0.15531(19) 0.0378(7) Uani 1 1 d . . .
H44 H 0.2929 0.7880 0.1842 0.045 Uiso 1 1 calc R . .
C45 C 0.3079(2) 0.71057(10) 0.18343(16) 0.0290(6) Uani 1 1 d . . .
H45 H 0.3527 0.7086 0.2329 0.035 Uiso 1 1 calc R . .
C46 C 0.28305(19) 0.59604(9) 0.00704(13) 0.0229(6) Uani 1 1 d . . .
C47 C 0.2879(2) 0.59064(10) -0.07058(14) 0.0299(6) Uani 1 1 d . . .
H47 H 0.2316 0.5981 -0.1116 0.036 Uiso 1 1 calc R . .
C48 C 0.3782(2) 0.57397(12) -0.08569(16) 0.0361(7) Uani 1 1 d . . .
H48 H 0.3833 0.5703 -0.1374 0.043 Uiso 1 1 calc R . .
C49 C 0.4607(2) 0.56275(11) -0.02469(15) 0.0316(6) Uani 1 1 d . . .
H49 H 0.5227 0.5524 -0.0341 0.038 Uiso 1 1 calc R . .
C50 C 0.4484(2) 0.56741(10) 0.05140(15) 0.0271(6) Uani 1 1 d . . .
H50 H 0.5030 0.5586 0.0930 0.033 Uiso 1 1 calc R . .
C51 C 0.18542(18) 0.44805(10) 0.42304(14) 0.0238(6) Uani 1 1 d . . .
C52 C 0.19601(19) 0.48680(10) 0.47788(14) 0.0256(6) Uani 1 1 d . . .
H52 H 0.2388 0.5146 0.4760 0.031 Uiso 1 1 calc R . .
C53 C 0.1424(2) 0.48413(11) 0.53602(15) 0.0312(6) Uani 1 1 d . . .
H53 H 0.1491 0.5098 0.5740 0.037 Uiso 1 1 calc R . .
C54 C 0.0789(2) 0.44262(12) 0.53622(16) 0.0363(7) Uani 1 1 d . . .
H54 H 0.0417 0.4395 0.5743 0.044 Uiso 1 1 calc R . .
C55 C 0.0719(2) 0.40579(12) 0.47864(17) 0.0409(7) Uani 1 1 d . . .
H55 H 0.0281 0.3781 0.4786 0.049 Uiso 1 1 calc R . .
C56 C 0.28751(18) 0.40045(10) 0.34030(15) 0.0245(6) Uani 1 1 d . . .
C57 C 0.2696(2) 0.37706(10) 0.26700(15) 0.0283(6) Uani 1 1 d . . .
H57 H 0.2212 0.3904 0.2244 0.034 Uiso 1 1 calc R . .
C58 C 0.3250(2) 0.33348(11) 0.25832(18) 0.0374(7) Uani 1 1 d . . .
H58 H 0.3136 0.3168 0.2100 0.045 Uiso 1 1 calc R . .
C59 C 0.3967(2) 0.31532(11) 0.3218(2) 0.0428(8) Uani 1 1 d . . .
H59 H 0.4366 0.2868 0.3172 0.051 Uiso 1 1 calc R . .
C60 C 0.4082(2) 0.34051(11) 0.39319(19) 0.0435(8) Uani 1 1 d . . .
H60 H 0.4557 0.3275 0.4366 0.052 Uiso 1 1 calc R . .
N1 N 0.35930(14) 0.60007(7) 0.32416(11) 0.0185(4) Uani 1 1 d . . .
N2 N 0.19468(14) 0.62986(7) 0.28836(11) 0.0180(4) Uani 1 1 d . . .
N3 N 0.43698(14) 0.52056(7) 0.23361(11) 0.0176(4) Uani 1 1 d . . .
N4 N 0.50902(16) 0.62550(8) 0.23355(13) 0.0275(5) Uani 1 1 d . . .
N5 N -0.07051(17) 0.59043(8) 0.27292(12) 0.0274(5) Uani 1 1 d . . .
N6 N -0.07363(16) 0.72448(8) 0.30229(13) 0.0304(5) Uani 1 1 d . . .
N7 N 0.18922(14) 0.56147(7) 0.13630(10) 0.0184(4) Uani 1 1 d . . .
N8 N 0.20560(14) 0.50761(7) 0.24200(11) 0.0173(4) Uani 1 1 d . . .
N9 N 0.28167(15) 0.66690(8) 0.14296(11) 0.0221(5) Uani 1 1 d . . .
N10 N 0.36216(15) 0.58395(8) 0.06795(11) 0.0217(5) Uani 1 1 d . . .
N11 N 0.12457(18) 0.40737(9) 0.42212(13) 0.0363(6) Uani 1 1 d . . .
N12 N 0.35513(17) 0.38242(9) 0.40335(14) 0.0362(6) Uani 1 1 d . . .
F1 F 0.61126(11) 0.55773(6) 0.41332(8) 0.0381(4) Uani 1 1 d . . .
F2 F 0.06022(10) 0.66854(5) 0.17355(7) 0.0266(3) Uani 1 1 d . . .
F3 F 0.12073(11) 0.63115(6) -0.04363(8) 0.0348(4) Uani 1 1 d . . .
F4 F 0.32001(10) 0.48596(5) 0.37824(7) 0.0226(3) Uani 1 1 d . . .
Mn1 Mn 0.34319(3) 0.591068(13) 0.19585(2) 0.01758(11) Uani 1 1 d . . .
N13 N 0.2350(2) 0.39641(12) 0.06223(13) 0.0425(7) Uani 1 1 d . . .
O1 O 0.2141(3) 0.44051(13) 0.0615(2) 0.1323(18) Uani 1 1 d . . .
O2 O 0.1698(2) 0.36453(15) 0.06944(18) 0.1173(14) Uani 1 1 d . . .
O3 O 0.31842(17) 0.38264(13) 0.05711(13) 0.0774(9) Uani 1 1 d . . .
N14 N 0.78131(16) 0.39718(8) 0.30089(12) 0.0272(5) Uani 1 1 d . . .
O4 O 0.73732(15) 0.36579(7) 0.24902(10) 0.0361(5) Uani 1 1 d . . .
O5 O 0.83256(19) 0.43191(9) 0.28158(14) 0.0616(7) Uani 1 1 d . . .
O6 O 0.77071(14) 0.39278(8) 0.36927(10) 0.0369(5) Uani 1 1 d . . .
C61A C 0.6486(3) 0.24919(19) 0.0902(3) 0.0891(15) Uani 0.508(9) 1 d P A 1
H61A H 0.6944 0.2278 0.0690 0.107 Uiso 0.508(9) 1 calc PR A 1
H61B H 0.6893 0.2720 0.1294 0.107 Uiso 0.508(9) 1 calc PR A 1
C62A C 0.5836(4) 0.27845(19) 0.0286(3) 0.1021(18) Uani 0.508(9) 1 d P A 1
H62A H 0.5419 0.2580 -0.0135 0.123 Uiso 0.508(9) 1 calc PR A 1
H62B H 0.6174 0.3064 0.0083 0.123 Uiso 0.508(9) 1 calc PR A 1
C63A C 0.5181(7) 0.2977(3) 0.1078(6) 0.080(3) Uani 0.508(9) 1 d P A 1
H63A H 0.5639 0.3123 0.1541 0.096 Uiso 0.508(9) 1 calc PR A 1
H63B H 0.4588 0.3195 0.0891 0.096 Uiso 0.508(9) 1 calc PR A 1
C64A C 0.4925(3) 0.24345(19) 0.1172(3) 0.0943(16) Uani 0.508(9) 1 d P A 1
H64A H 0.4662 0.2388 0.1636 0.113 Uiso 0.508(9) 1 calc PR A 1
H64B H 0.4420 0.2313 0.0714 0.113 Uiso 0.508(9) 1 calc PR A 1
C61B C 0.6486(3) 0.24919(19) 0.0902(3) 0.0891(15) Uani 0.492(9) 1 d P A 2
H61C H 0.6944 0.2278 0.0690 0.107 Uiso 0.492(9) 1 calc PR A 2
H61D H 0.6893 0.2720 0.1294 0.107 Uiso 0.492(9) 1 calc PR A 2
C62B C 0.5836(4) 0.27845(19) 0.0286(3) 0.1021(18) Uani 0.492(9) 1 d P A 2
H62C H 0.6093 0.3134 0.0296 0.123 Uiso 0.492(9) 1 calc PR A 2
H62D H 0.5846 0.2634 -0.0219 0.123 Uiso 0.492(9) 1 calc PR A 2
C63B C 0.4870(5) 0.2794(2) 0.0367(4) 0.042(2) Uani 0.492(9) 1 d P A 2
H63C H 0.4401 0.2647 -0.0090 0.050 Uiso 0.492(9) 1 calc PR A 2
H63D H 0.4656 0.3143 0.0443 0.050 Uiso 0.492(9) 1 calc PR A 2
C64B C 0.4925(3) 0.24345(19) 0.1172(3) 0.0943(16) Uani 0.492(9) 1 d P A 2
H64C H 0.4930 0.2647 0.1628 0.113 Uiso 0.492(9) 1 calc PR A 2
H64D H 0.4356 0.2196 0.1093 0.113 Uiso 0.492(9) 1 calc PR A 2
O7 O 0.5844(2) 0.21783(10) 0.12506(16) 0.0755(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.320(3) . ?
C1 C2 1.406(3) . ?
C1 C9 1.529(3) . ?
C2 C3 1.362(4) . ?
C2 H2 0.9300 . ?
C3 C8 1.407(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(3) . ?
C4 C8 1.417(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.428(3) . ?
C5 H5 0.9300 . ?
C6 N2 1.309(3) . ?
C6 C10 1.526(3) . ?
C7 N2 1.361(3) . ?
C7 N1 1.362(3) . ?
C7 C8 1.410(3) . ?
C9 F1 1.387(3) . ?
C9 C16 1.523(4) . ?
C9 C11 1.528(3) . ?
C10 F2 1.410(3) . ?
C10 C26 1.518(3) . ?
C10 C21 1.531(3) . ?
C11 N3 1.344(3) . ?
C11 C12 1.383(3) . ?
C12 C13 1.370(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.378(3) . ?
C14 H14 0.9300 . ?
C15 N3 1.344(3) . ?
C15 H15 0.9300 . ?
C16 N4 1.342(3) . ?
C16 C17 1.391(4) . ?
C17 C18 1.370(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.376(4) . ?
C19 H19 0.9300 . ?
C20 N4 1.347(3) . ?
C20 H20 0.9300 . ?
C21 N6 1.338(3) . ?
C21 C22 1.373(4) . ?
C22 C23 1.370(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.370(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(4) . ?
C24 H24 0.9300 . ?
C25 N6 1.344(3) . ?
C25 H25 0.9300 . ?
C26 N5 1.336(3) . ?
C26 C27 1.391(3) . ?
C27 C28 1.380(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.378(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.376(4) . ?
C29 H29 0.9300 . ?
C30 N5 1.347(3) . ?
C30 H30 0.9300 . ?
C31 N7 1.330(3) . ?
C31 C32 1.408(3) . ?
C31 C39 1.520(3) . ?
C32 C33 1.359(4) . ?
C32 H32 0.9300 . ?
C33 C38 1.408(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.354(3) . ?
C34 C38 1.411(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.417(3) . ?
C35 H35 0.9300 . ?
C36 N8 1.319(3) . ?
C36 C40 1.533(3) . ?
C37 N8 1.357(3) . ?
C37 N7 1.366(3) . ?
C37 C38 1.407(3) . ?
C39 F3 1.401(3) . ?
C39 C41 1.523(4) . ?
C39 C46 1.525(3) . ?
C40 F4 1.409(3) . ?
C40 C51 1.523(3) . ?
C40 C56 1.526(4) . ?
C41 N9 1.343(3) . ?
C41 C42 1.383(3) . ?
C42 C43 1.372(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.381(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.379(4) . ?
C44 H44 0.9300 . ?
C45 N9 1.339(3) . ?
C45 H45 0.9300 . ?
C46 N10 1.350(3) . ?
C46 C47 1.383(3) . ?
C47 C48 1.376(4) . ?
C47 H47 0.9300 . ?
C48 C49 1.373(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.387(3) . ?
C49 H49 0.9300 . ?
C50 N10 1.336(3) . ?
C50 H50 0.9300 . ?
C51 N11 1.336(3) . ?
C51 C52 1.375(3) . ?
C52 C53 1.386(4) . ?
C52 H52 0.9300 . ?
C53 C54 1.378(4) . ?
C53 H53 0.9300 . ?
C54 C55 1.376(4) . ?
C54 H54 0.9300 . ?
C55 N11 1.351(4) . ?
C55 H55 0.9300 . ?
C56 N12 1.334(3) . ?
C56 C57 1.387(3) . ?
C57 C58 1.385(4) . ?
C57 H57 0.9300 . ?
C58 C59 1.368(4) . ?
C58 H58 0.9300 . ?
C59 C60 1.385(4) . ?
C59 H59 0.9300 . ?
C60 N12 1.339(4) . ?
C60 H60 0.9300 . ?
N1 Mn1 2.2156(18) . ?
N3 Mn1 2.2335(19) . ?
N4 Mn1 2.349(2) . ?
N7 Mn1 2.2220(19) . ?
N9 Mn1 2.249(2) . ?
N10 Mn1 2.3215(19) . ?
N13 O1 1.180(4) . ?
N13 O3 1.204(3) . ?
N13 O2 1.237(4) . ?
N14 O5 1.233(3) . ?
N14 O6 1.245(3) . ?
N14 O4 1.257(3) . ?
C61A O7 1.429(5) . ?
C61A C62A 1.432(6) . ?
C61A H61A 0.9700 . ?
C61A H61B 0.9700 . ?
C62A C63A 1.882(10) . ?
C62A H62A 0.9700 . ?
C62A H62B 0.9700 . ?
C63A C64A 1.470(9) . ?
C63A H63A 0.9700 . ?
C63A H63B 0.9700 . ?
C64A O7 1.383(5) . ?
C64A H64A 0.9700 . ?
C64A H64B 0.9700 . ?
C63B H63C 0.9700 . ?
C63B H63D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.3(2) . . ?
N1 C1 C9 116.1(2) . . ?
C2 C1 C9 120.6(2) . . ?
C3 C2 C1 118.4(2) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C8 120.3(2) . . ?
C2 C3 H3 119.9 . . ?
C8 C3 H3 119.9 . . ?
C5 C4 C8 119.3(2) . . ?
C5 C4 H4 120.3 . . ?
C8 C4 H4 120.3 . . ?
C4 C5 C6 118.8(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
N2 C6 C5 124.0(2) . . ?
N2 C6 C10 117.3(2) . . ?
C5 C6 C10 118.6(2) . . ?
N2 C7 N1 114.48(19) . . ?
N2 C7 C8 123.5(2) . . ?
N1 C7 C8 122.0(2) . . ?
C3 C8 C7 117.4(2) . . ?
C3 C8 C4 125.4(2) . . ?
C7 C8 C4 117.2(2) . . ?
F1 C9 C16 107.1(2) . . ?
F1 C9 C11 106.5(2) . . ?
C16 C9 C11 111.9(2) . . ?
F1 C9 C1 106.79(19) . . ?
C16 C9 C1 112.4(2) . . ?
C11 C9 C1 111.8(2) . . ?
F2 C10 C26 106.28(18) . . ?
F2 C10 C6 107.62(18) . . ?
C26 C10 C6 113.1(2) . . ?
F2 C10 C21 106.16(18) . . ?
C26 C10 C21 115.5(2) . . ?
C6 C10 C21 107.70(19) . . ?
N3 C11 C12 122.3(2) . . ?
N3 C11 C9 116.4(2) . . ?
C12 C11 C9 121.2(2) . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 119.0(2) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.8(2) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N3 C15 C14 122.8(2) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N4 C16 C17 122.6(3) . . ?
N4 C16 C9 117.0(2) . . ?
C17 C16 C9 120.4(3) . . ?
C18 C17 C16 118.6(3) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
N4 C20 C19 122.9(3) . . ?
N4 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
N6 C21 C22 122.8(2) . . ?
N6 C21 C10 115.8(2) . . ?
C22 C21 C10 121.0(2) . . ?
C23 C22 C21 119.8(3) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 118.6(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C23 C24 C25 118.5(3) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
N6 C25 C24 123.9(3) . . ?
N6 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
N5 C26 C27 122.9(2) . . ?
N5 C26 C10 117.2(2) . . ?
C27 C26 C10 119.9(2) . . ?
C28 C27 C26 118.9(3) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C29 C28 C27 118.9(3) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
C30 C29 C28 118.6(3) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
N5 C30 C29 123.8(3) . . ?
N5 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
N7 C31 C32 123.3(2) . . ?
N7 C31 C39 115.8(2) . . ?
C32 C31 C39 120.9(2) . . ?
C33 C32 C31 118.8(2) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C38 119.8(2) . . ?
C32 C33 H33 120.1 . . ?
C38 C33 H33 120.1 . . ?
C35 C34 C38 119.7(2) . . ?
C35 C34 H34 120.2 . . ?
C38 C34 H34 120.2 . . ?
C34 C35 C36 118.8(2) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
N8 C36 C35 123.8(2) . . ?
N8 C36 C40 116.17(19) . . ?
C35 C36 C40 120.0(2) . . ?
N8 C37 N7 114.24(19) . . ?
N8 C37 C38 123.8(2) . . ?
N7 C37 C38 122.0(2) . . ?
C37 C38 C33 118.0(2) . . ?
C37 C38 C34 117.0(2) . . ?
C33 C38 C34 125.0(2) . . ?
F3 C39 C31 106.17(19) . . ?
F3 C39 C41 106.52(19) . . ?
C31 C39 C41 112.87(19) . . ?
F3 C39 C46 106.00(18) . . ?
C31 C39 C46 113.5(2) . . ?
C41 C39 C46 111.1(2) . . ?
F4 C40 C51 107.10(18) . . ?
F4 C40 C56 105.07(18) . . ?
C51 C40 C56 113.3(2) . . ?
F4 C40 C36 107.13(18) . . ?
C51 C40 C36 111.20(19) . . ?
C56 C40 C36 112.49(19) . . ?
N9 C41 C42 122.3(3) . . ?
N9 C41 C39 116.0(2) . . ?
C42 C41 C39 121.7(2) . . ?
C43 C42 C41 118.6(3) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C42 C43 C44 120.2(3) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C45 C44 C43 117.7(3) . . ?
C45 C44 H44 121.2 . . ?
C43 C44 H44 121.2 . . ?
N9 C45 C44 123.2(3) . . ?
N9 C45 H45 118.4 . . ?
C44 C45 H45 118.4 . . ?
N10 C46 C47 122.4(2) . . ?
N10 C46 C39 116.4(2) . . ?
C47 C46 C39 121.1(2) . . ?
C48 C47 C46 118.4(2) . . ?
C48 C47 H47 120.8 . . ?
C46 C47 H47 120.8 . . ?
C49 C48 C47 120.3(2) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 117.7(2) . . ?
C48 C49 H49 121.1 . . ?
C50 C49 H49 121.1 . . ?
N10 C50 C49 123.3(2) . . ?
N10 C50 H50 118.3 . . ?
C49 C50 H50 118.3 . . ?
N11 C51 C52 123.2(2) . . ?
N11 C51 C40 115.6(2) . . ?
C52 C51 C40 121.1(2) . . ?
C51 C52 C53 119.5(2) . . ?
C51 C52 H52 120.3 . . ?
C53 C52 H52 120.3 . . ?
C54 C53 C52 118.4(3) . . ?
C54 C53 H53 120.8 . . ?
C52 C53 H53 120.8 . . ?
C55 C54 C53 118.4(3) . . ?
C55 C54 H54 120.8 . . ?
C53 C54 H54 120.8 . . ?
N11 C55 C54 124.0(3) . . ?
N11 C55 H55 118.0 . . ?
C54 C55 H55 118.0 . . ?
N12 C56 C57 122.8(2) . . ?
N12 C56 C40 113.5(2) . . ?
C57 C56 C40 123.6(2) . . ?
C58 C57 C56 118.8(3) . . ?
C58 C57 H57 120.6 . . ?
C56 C57 H57 120.6 . . ?
C59 C58 C57 119.1(3) . . ?
C59 C58 H58 120.4 . . ?
C57 C58 H58 120.4 . . ?
C58 C59 C60 118.2(3) . . ?
C58 C59 H59 120.9 . . ?
C60 C59 H59 120.9 . . ?
N12 C60 C59 123.9(3) . . ?
N12 C60 H60 118.1 . . ?
C59 C60 H60 118.1 . . ?
C1 N1 C7 118.6(2) . . ?
C1 N1 Mn1 123.74(16) . . ?
C7 N1 Mn1 117.09(14) . . ?
C6 N2 C7 116.97(19) . . ?
C11 N3 C15 117.8(2) . . ?
C11 N3 Mn1 122.43(15) . . ?
C15 N3 Mn1 119.60(15) . . ?
C16 N4 C20 117.6(2) . . ?
C16 N4 Mn1 119.44(16) . . ?
C20 N4 Mn1 122.91(19) . . ?
C26 N5 C30 117.0(2) . . ?
C21 N6 C25 116.4(2) . . ?
C31 N7 C37 118.0(2) . . ?
C31 N7 Mn1 122.49(16) . . ?
C37 N7 Mn1 118.70(14) . . ?
C36 N8 C37 116.93(19) . . ?
C45 N9 C41 118.1(2) . . ?
C45 N9 Mn1 120.09(17) . . ?
C41 N9 Mn1 121.79(16) . . ?
C50 N10 C46 117.8(2) . . ?
C50 N10 Mn1 122.69(16) . . ?
C46 N10 Mn1 119.51(15) . . ?
C51 N11 C55 116.5(2) . . ?
C56 N12 C60 117.1(2) . . ?
N1 Mn1 N7 111.28(7) . . ?
N1 Mn1 N3 82.96(7) . . ?
N7 Mn1 N3 104.61(7) . . ?
N1 Mn1 N9 105.10(7) . . ?
N7 Mn1 N9 84.32(7) . . ?
N3 Mn1 N9 165.17(7) . . ?
N1 Mn1 N10 168.31(7) . . ?
N7 Mn1 N10 80.14(7) . . ?
N3 Mn1 N10 91.90(7) . . ?
N9 Mn1 N10 77.80(7) . . ?
N1 Mn1 N4 79.76(7) . . ?
N7 Mn1 N4 168.73(7) . . ?
N3 Mn1 N4 78.32(7) . . ?
N9 Mn1 N4 90.72(7) . . ?
N10 Mn1 N4 88.93(7) . . ?
O1 N13 O3 120.9(4) . . ?
O1 N13 O2 118.5(4) . . ?
O3 N13 O2 120.6(4) . . ?
O5 N14 O6 122.2(2) . . ?
O5 N14 O4 118.3(2) . . ?
O6 N14 O4 119.4(2) . . ?
O7 C61A C62A 107.5(4) . . ?
O7 C61A H61A 110.2 . . ?
C62A C61A H61A 110.2 . . ?
O7 C61A H61B 110.2 . . ?
C62A C61A H61B 110.2 . . ?
H61A C61A H61B 108.5 . . ?
C61A C62A C63A 84.1(4) . . ?
C61A C62A H62A 114.6 . . ?
C63A C62A H62A 114.6 . . ?
C61A C62A H62B 114.6 . . ?
C63A C62A H62B 114.6 . . ?
H62A C62A H62B 111.7 . . ?
C64A C63A C62A 89.6(5) . . ?
C64A C63A H63A 113.7 . . ?
C62A C63A H63A 113.7 . . ?
C64A C63A H63B 113.7 . . ?
C62A C63A H63B 113.7 . . ?
H63A C63A H63B 111.0 . . ?
O7 C64A C63A 104.1(4) . . ?
O7 C64A H64A 110.9 . . ?
C63A C64A H64A 110.9 . . ?
O7 C64A H64B 110.9 . . ?
C63A C64A H64B 110.9 . . ?
H64A C64A H64B 109.0 . . ?
H63C C63B H63D 109.1 . . ?
C64A O7 C61A 107.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.064
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol, tetrahydrofuran'
_chemical_properties_physical    Hygroscopic
_database_code_depnum_ccdc_archive 'CCDC 1022461'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[Co2(u-Cl)2Cl(CH3OH)(DPFN)]2[CoCl4]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Co2(u-Cl)2Cl(CH3OH)(DPFN)]2[CoCl4]'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C31 H24 Cl3 Co2 F2 N6 O 1+, 0.5(Cl4 Co 2-), 1.875(C H4 O), 0.25(C4 H8 O)'
_chemical_formula_sum            'C33.875 H34 Cl5 Co2.50 F2 N6 O3.125'
_chemical_formula_weight         937.75

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.6956(16)
_cell_length_b                   15.6624(18)
_cell_length_c                   21.613(3)
_cell_angle_alpha                82.3800(10)
_cell_angle_beta                 73.2410(10)
_cell_angle_gamma                64.5290(10)
_cell_volume                     4007.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.71

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1899
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            113204
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.35
_reflns_number_total             14648
_reflns_number_gt                11429
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The CoCl4 2- counterion is disordered over three sites and the site consisting of atoms Cl7 Cl8 Cl9 Cl11 Co5A was modeled with occupancy of 0.45, the site consisting of atoms Cl7 Cl8 Cl10 Cl12 Co5B was modeled with occupancy of 0.45, and the site consisting of atoms Cl8 Cl9 Cl11 Cl13 Co5C was modeled with occupancy of 0.1.  Due to the low structure occupancy factor and high disorder, atom Cl13 was refined isotropically.

 The methanol solvate molecule sites consisting of atoms C65 O5, C66 O6, C67 O7, and C68 O8 were found to be partially occupied and were modeled with structure occupancy factors of 0.5 for C65 O5, C66 O6, and C67 O7, and structure occupancy factors of 0.25 for C66 O6.  Due to the low structure occupancy factors and high disorder, the atoms C68 O8 were refined isotropically and the C68 O8 bond length was restrained to a chemically appropriate value.

 The diethyl ether solvate molecule site consisting of atoms C69 C70 C71 C72 O9 was found to be partially occupied and was modeled with structure occupancy factors of 0.5.  Due to disorder of this molecule, bond and angle restraints were applied to atoms C69 C70 C71 C72 O9 to chemically appropriate values.  Due to severe anisotropy in the atomic displacement parameters, isotropic restraints with esd values of 0.1 were applied to atoms C71 C72.

All hydrogen atoms were modeled with a constrained riding model except for H1A and H2A bound to cobalt-coordinated methanol ligands which were located from the electron density map.  The bond length for H2A O2 was restrained to a chemically appropiate value.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0721P)²+11.0402P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14648
_refine_ls_number_parameters     1039
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1529
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3368(3) 0.6922(3) 0.44469(19) 0.0223(8) Uani 1 1 d . . .
C2 C 0.3187(3) 0.6225(3) 0.42091(19) 0.0249(8) Uani 1 1 d . . .
H2 H 0.2461 0.6335 0.4184 0.030 Uiso 1 1 calc R . .
C3 C 0.4068(3) 0.5396(3) 0.4017(2) 0.0260(9) Uani 1 1 d . . .
H3 H 0.3968 0.4907 0.3862 0.031 Uiso 1 1 calc R . .
C4 C 0.6071(3) 0.4425(3) 0.3819(2) 0.0262(9) Uani 1 1 d . . .
H4 H 0.5981 0.3929 0.3665 0.031 Uiso 1 1 calc R . .
C5 C 0.7101(3) 0.4328(3) 0.3818(2) 0.0273(9) Uani 1 1 d . . .
H5 H 0.7747 0.3772 0.3657 0.033 Uiso 1 1 calc R . .
C6 C 0.7190(3) 0.5074(3) 0.40609(19) 0.0235(8) Uani 1 1 d . . .
C7 C 0.5275(3) 0.5992(3) 0.42909(18) 0.0214(8) Uani 1 1 d . . .
C8 C 0.5134(3) 0.5263(3) 0.40489(19) 0.0230(8) Uani 1 1 d . . .
C9 C 0.2328(3) 0.7851(3) 0.4659(2) 0.0290(9) Uani 1 1 d . . .
C10 C 0.8402(3) 0.4927(3) 0.4021(2) 0.0268(9) Uani 1 1 d . . .
C11 C 0.1985(3) 0.7969(3) 0.5390(2) 0.0280(9) Uani 1 1 d . . .
C12 C 0.0950(3) 0.8031(3) 0.5766(2) 0.0331(10) Uani 1 1 d . . .
H12 H 0.0413 0.8019 0.5575 0.040 Uiso 1 1 calc R . .
C13 C 0.0718(4) 0.8109(3) 0.6429(2) 0.0362(10) Uani 1 1 d . . .
H13 H 0.0019 0.8144 0.6701 0.043 Uiso 1 1 calc R . .
C14 C 0.1517(4) 0.8134(3) 0.6690(2) 0.0373(11) Uani 1 1 d . . .
H14 H 0.1376 0.8185 0.7143 0.045 Uiso 1 1 calc R . .
C15 C 0.2520(4) 0.8085(3) 0.6282(2) 0.0312(9) Uani 1 1 d . . .
H15 H 0.3062 0.8112 0.6461 0.037 Uiso 1 1 calc R . .
C16 C 0.2462(3) 0.8707(3) 0.4286(2) 0.0277(9) Uani 1 1 d . . .
C17 C 0.1896(3) 0.9168(3) 0.3815(2) 0.0326(10) Uani 1 1 d . . .
H17 H 0.1435 0.8939 0.3698 0.039 Uiso 1 1 calc R . .
C18 C 0.2023(4) 0.9967(3) 0.3523(2) 0.0387(11) Uani 1 1 d . . .
H18 H 0.1665 1.0286 0.3190 0.046 Uiso 1 1 calc R . .
C19 C 0.2675(4) 1.0299(3) 0.3717(3) 0.0406(11) Uani 1 1 d . . .
H19 H 0.2739 1.0866 0.3539 0.049 Uiso 1 1 calc R . .
C20 C 0.3228(4) 0.9784(3) 0.4175(2) 0.0327(10) Uani 1 1 d . . .
H20 H 0.3691 1.0002 0.4303 0.039 Uiso 1 1 calc R . .
C21 C 0.8606(3) 0.4842(3) 0.4689(2) 0.0256(9) Uani 1 1 d . . .
C22 C 0.9428(3) 0.4040(3) 0.4874(2) 0.0294(9) Uani 1 1 d . . .
H22 H 0.9908 0.3535 0.4582 0.035 Uiso 1 1 calc R . .
C23 C 0.9530(3) 0.3994(3) 0.5499(2) 0.0326(10) Uani 1 1 d . . .
H23 H 1.0077 0.3450 0.5644 0.039 Uiso 1 1 calc R . .
C24 C 0.8827(3) 0.4749(3) 0.5908(2) 0.0303(9) Uani 1 1 d . . .
H24 H 0.8872 0.4724 0.6341 0.036 Uiso 1 1 calc R . .
C25 C 0.8059(3) 0.5541(3) 0.5677(2) 0.0275(9) Uani 1 1 d . . .
H25 H 0.7599 0.6070 0.5952 0.033 Uiso 1 1 calc R . .
C26 C 0.8709(3) 0.5667(3) 0.3590(2) 0.0269(9) Uani 1 1 d . . .
C27 C 0.9481(4) 0.5433(4) 0.2996(2) 0.0368(11) Uani 1 1 d . . .
H27 H 0.9834 0.4802 0.2845 0.044 Uiso 1 1 calc R . .
C28 C 0.9727(4) 0.6136(4) 0.2628(2) 0.0453(13) Uani 1 1 d . . .
H28 H 1.0252 0.5999 0.2217 0.054 Uiso 1 1 calc R . .
C29 C 0.9198(4) 0.7049(4) 0.2867(2) 0.0424(12) Uani 1 1 d . . .
H29 H 0.9366 0.7544 0.2625 0.051 Uiso 1 1 calc R . .
C30 C 0.8429(4) 0.7229(3) 0.3456(2) 0.0334(10) Uani 1 1 d . . .
H30 H 0.8061 0.7856 0.3615 0.040 Uiso 1 1 calc R . .
C31 C 0.4696(4) 0.9320(4) 0.5784(3) 0.0470(13) Uani 1 1 d . . .
H31A H 0.4644 0.9056 0.6224 0.071 Uiso 1 1 calc R . .
H31B H 0.4502 0.9998 0.5797 0.071 Uiso 1 1 calc R . .
H31C H 0.5463 0.9000 0.5517 0.071 Uiso 1 1 calc R . .
N1 N 0.4359(3) 0.6826(2) 0.45028(16) 0.0227(7) Uani 1 1 d . . .
N2 N 0.6326(3) 0.5880(2) 0.42986(16) 0.0224(7) Uani 1 1 d . . .
N3 N 0.2759(3) 0.7999(2) 0.56389(17) 0.0270(7) Uani 1 1 d . . .
N4 N 0.3144(3) 0.8990(2) 0.44499(18) 0.0287(8) Uani 1 1 d . . .
N5 N 0.7943(3) 0.5585(2) 0.50754(16) 0.0240(7) Uani 1 1 d . . .
N6 N 0.8176(3) 0.6548(2) 0.38153(16) 0.0260(7) Uani 1 1 d . . .
F1 F 0.14409(19) 0.77819(17) 0.45083(13) 0.0323(6) Uani 1 1 d . . .
F2 F 0.91071(19) 0.40561(17) 0.37363(12) 0.0343(6) Uani 1 1 d . . .
Cl1 Cl 0.54001(8) 0.70100(7) 0.56706(5) 0.0244(2) Uani 1 1 d . . .
Cl2 Cl 0.57591(8) 0.81935(7) 0.41875(5) 0.0264(2) Uani 1 1 d . . .
Cl3 Cl 0.76677(8) 0.77015(7) 0.51369(5) 0.0311(2) Uani 1 1 d . . .
Co1 Co 0.42260(4) 0.80534(4) 0.50075(3) 0.02350(14) Uani 1 1 d . . .
Co2 Co 0.69115(4) 0.68481(4) 0.47027(3) 0.02259(13) Uani 1 1 d . . .
O1 O 0.3948(3) 0.9182(2) 0.55175(16) 0.0334(7) Uani 1 1 d . . .
H1A H 0.342(5) 0.961(4) 0.554(3) 0.052(18) Uiso 1 1 d . . .
C32 C 0.4146(5) 0.7139(4) 0.9572(2) 0.0456(12) Uani 1 1 d . . .
C33 C 0.5118(5) 0.6695(4) 0.9088(2) 0.0624(17) Uani 1 1 d . . .
H33 H 0.5150 0.6888 0.8650 0.075 Uiso 1 1 calc R . .
C34 C 0.6014(5) 0.5988(5) 0.9248(3) 0.0647(18) Uani 1 1 d . . .
H34 H 0.6682 0.5676 0.8925 0.078 Uiso 1 1 calc R . .
C35 C 0.6866(5) 0.5027(4) 1.0082(3) 0.0551(14) Uani 1 1 d . . .
H35 H 0.7539 0.4705 0.9764 0.066 Uiso 1 1 calc R . .
C36 C 0.6800(5) 0.4811(4) 1.0718(2) 0.0485(13) Uani 1 1 d . . .
H36 H 0.7425 0.4345 1.0853 0.058 Uiso 1 1 calc R . .
C37 C 0.5783(4) 0.5293(3) 1.1169(2) 0.0374(11) Uani 1 1 d . . .
C38 C 0.4936(4) 0.6197(3) 1.0376(2) 0.0367(10) Uani 1 1 d . . .
C39 C 0.5940(5) 0.5723(4) 0.9901(2) 0.0467(13) Uani 1 1 d . . .
C40 C 0.3167(5) 0.7950(4) 0.9348(2) 0.0529(14) Uani 1 1 d . . .
C41 C 0.5762(4) 0.5028(3) 1.1888(2) 0.0395(11) Uani 1 1 d . . .
C43 C 0.1713(6) 0.7746(4) 0.8951(3) 0.0676(19) Uani 1 1 d . . .
H43 H 0.2038 0.7892 0.8522 0.081 Uiso 1 1 calc R . .
C44 C 0.0785(7) 0.7543(5) 0.9090(4) 0.081(2) Uani 1 1 d . . .
H44 H 0.0457 0.7551 0.8756 0.098 Uiso 1 1 calc R . .
C42 C 0.2157(5) 0.7732(4) 0.9457(3) 0.0522(14) Uani 1 1 d . . .
C45 C 0.0340(6) 0.7329(5) 0.9715(4) 0.076(2) Uani 1 1 d . . .
H45 H -0.0293 0.7181 0.9818 0.092 Uiso 1 1 calc R . .
C46 C 0.0835(5) 0.7333(5) 1.0192(3) 0.0628(16) Uani 1 1 d . . .
H46 H 0.0533 0.7180 1.0624 0.075 Uiso 1 1 calc R . .
C47 C 0.2857(5) 0.8901(4) 0.9638(2) 0.0458(12) Uani 1 1 d . . .
C48 C 0.2975(5) 0.9654(5) 0.9260(3) 0.0578(15) Uani 1 1 d . . .
H48 H 0.3268 0.9594 0.8805 0.069 Uiso 1 1 calc R . .
C49 C 0.2659(5) 1.0497(5) 0.9560(3) 0.0607(15) Uani 1 1 d . . .
H49 H 0.2722 1.1029 0.9313 0.073 Uiso 1 1 calc R . .
C50 C 0.2252(5) 1.0551(4) 1.0220(3) 0.0558(15) Uani 1 1 d . . .
H50 H 0.2038 1.1117 1.0438 0.067 Uiso 1 1 calc R . .
C51 C 0.2160(5) 0.9769(4) 1.0561(3) 0.0517(14) Uani 1 1 d . . .
H51 H 0.1874 0.9812 1.1017 0.062 Uiso 1 1 calc R . .
C52 C 0.4972(4) 0.4560(3) 1.2197(2) 0.0394(11) Uani 1 1 d . . .
C53 C 0.5351(5) 0.3637(4) 1.2443(2) 0.0466(13) Uani 1 1 d . . .
H53 H 0.6118 0.3284 1.2436 0.056 Uiso 1 1 calc R . .
C54 C 0.4578(6) 0.3256(4) 1.2697(2) 0.0549(15) Uani 1 1 d . . .
H54 H 0.4807 0.2634 1.2875 0.066 Uiso 1 1 calc R . .
C55 C 0.3483(6) 0.3772(4) 1.2693(2) 0.0526(15) Uani 1 1 d . . .
H55 H 0.2953 0.3504 1.2852 0.063 Uiso 1 1 calc R . .
C56 C 0.3156(5) 0.4686(4) 1.2455(2) 0.0475(13) Uani 1 1 d . . .
H56 H 0.2390 0.5049 1.2465 0.057 Uiso 1 1 calc R . .
C57 C 0.5585(4) 0.5865(4) 1.2258(2) 0.0374(11) Uani 1 1 d . . .
C58 C 0.6434(4) 0.5898(4) 1.2463(2) 0.0403(11) Uani 1 1 d . . .
H58 H 0.7157 0.5391 1.2382 0.048 Uiso 1 1 calc R . .
C59 C 0.6198(5) 0.6695(4) 1.2792(2) 0.0439(12) Uani 1 1 d . . .
H59 H 0.6769 0.6750 1.2928 0.053 Uiso 1 1 calc R . .
C60 C 0.5136(4) 0.7404(4) 1.2920(2) 0.0418(11) Uani 1 1 d . . .
H60 H 0.4957 0.7944 1.3157 0.050 Uiso 1 1 calc R . .
C61 C 0.4332(4) 0.7317(4) 1.2699(2) 0.0384(11) Uani 1 1 d . . .
H61 H 0.3597 0.7808 1.2786 0.046 Uiso 1 1 calc R . .
C62 C -0.0175(6) 0.9367(6) 1.1023(3) 0.081(2) Uani 1 1 d . . .
H62A H -0.0207 0.9962 1.1144 0.121 Uiso 1 1 calc R . .
H62B H -0.0906 0.9344 1.1207 0.121 Uiso 1 1 calc R . .
H62C H 0.0020 0.9328 1.0552 0.121 Uiso 1 1 calc R . .
N7 N 0.4023(4) 0.6910(3) 1.02007(18) 0.0391(9) Uani 1 1 d . . .
N8 N 0.4865(3) 0.5963(3) 1.10237(17) 0.0350(9) Uani 1 1 d . . .
N9 N 0.1728(4) 0.7548(3) 1.0064(2) 0.0524(12) Uani 1 1 d . . .
N10 N 0.2457(4) 0.8951(3) 1.0278(2) 0.0468(11) Uani 1 1 d . . .
N11 N 0.3891(4) 0.5083(3) 1.22087(18) 0.0408(10) Uani 1 1 d . . .
N12 N 0.4556(3) 0.6562(3) 1.23648(18) 0.0363(9) Uani 1 1 d . . .
F3 F 0.3550(3) 0.8050(2) 0.86800(14) 0.0674(10) Uani 1 1 d . . .
F4 F 0.6832(2) 0.4341(2) 1.18943(14) 0.0481(7) Uani 1 1 d . . .
Cl4 Cl 0.21448(11) 0.63877(10) 1.13813(6) 0.0467(3) Uani 1 1 d . . .
Cl5 Cl 0.30154(12) 0.81004(9) 1.15842(6) 0.0476(3) Uani 1 1 d . . .
Cl6 Cl 0.19132(10) 0.69916(9) 1.29563(5) 0.0413(3) Uani 1 1 d . . .
Co3 Co 0.23246(6) 0.77563(5) 1.07998(3) 0.04209(18) Uani 1 1 d . . .
Co4 Co 0.33488(6) 0.65252(5) 1.19536(3) 0.03731(17) Uani 1 1 d . . .
O2 O 0.0648(3) 0.8596(3) 1.12673(19) 0.0569(10) Uani 1 1 d D . .
H2A H 0.054(6) 0.870(5) 1.1678(13) 0.08(2) Uiso 1 1 d D . .
Cl7 Cl 1.08458(13) 0.63159(12) 0.77695(8) 0.0558(4) Uani 0.90 1 d P . .
Cl8 Cl 0.83642(16) 0.73715(14) 0.70735(16) 0.1119(9) Uani 1 1 d . . .
Cl9 Cl 0.8760(5) 0.8677(4) 0.8068(3) 0.0691(15) Uani 0.55 1 d P . .
Cl10 Cl 0.8261(5) 0.7010(5) 0.9028(2) 0.113(2) Uani 0.45 1 d P . .
Cl11 Cl 0.7949(7) 0.6626(8) 0.8657(5) 0.253(6) Uani 0.55 1 d P A .
Cl12 Cl 0.9058(5) 0.8895(5) 0.8015(3) 0.0619(17) Uani 0.45 1 d P A .
Cl13 Cl 0.6074(15) 0.8500(14) 0.8171(11) 0.083(5) Uiso 0.10 1 d PD A 1
Co5C Co 0.8174(16) 0.7591(9) 0.7952(6) 0.134(8) Uani 0.10 1 d PD A 1
Co5A Co 0.8956(3) 0.72493(17) 0.78754(14) 0.0448(6) Uani 0.45 1 d P A 2
Co5B Co 0.9106(3) 0.7374(3) 0.80304(16) 0.0696(12) Uani 0.45 1 d P A 2
C63 C 0.0377(10) 0.9488(7) 0.2568(4) 0.119(4) Uani 1 1 d . B 2
H63B H -0.0165 0.9850 0.2949 0.178 Uiso 1 1 calc R B 2
H63A H 0.0314 0.9895 0.2183 0.178 Uiso 1 1 calc R B 2
H63C H 0.1136 0.9259 0.2622 0.178 Uiso 1 1 calc R B 2
O3 O 0.0164(5) 0.8737(3) 0.2499(2) 0.099(2) Uani 1 1 d . B 2
H3A H 0.0656 0.8237 0.2604 0.149 Uiso 1 1 calc R B 2
C64 C 0.8967(4) 0.9260(4) 0.4317(3) 0.0551(15) Uani 1 1 d . C 2
H64B H 0.9042 0.9845 0.4141 0.083 Uiso 1 1 calc R C 2
H64C H 0.9582 0.8720 0.4068 0.083 Uiso 1 1 calc R C 2
H64A H 0.8995 0.9183 0.4770 0.083 Uiso 1 1 calc R C 2
O4 O 0.7931(2) 0.9306(2) 0.42778(16) 0.0373(7) Uani 1 1 d . C 2
H4A H 0.7780 0.8890 0.4521 0.056 Uiso 1 1 calc R C 2
C65 C 0.074(2) 0.4478(17) 0.8921(12) 0.130(7) Uiso 0.50 1 d P D 1
H65B H 0.0893 0.4757 0.8491 0.196 Uiso 0.50 1 calc PR D 1
H65C H 0.1035 0.3789 0.8886 0.196 Uiso 0.50 1 calc PR D 1
H65A H 0.1090 0.4634 0.9198 0.196 Uiso 0.50 1 calc PR D 1
O5 O -0.0386(18) 0.4829(13) 0.9184(13) 0.279(17) Uani 0.50 1 d P D 1
H5A H -0.0717 0.5169 0.8908 0.418 Uiso 0.50 1 calc PR D 1
C66 C 0.2368(14) 0.9781(9) 0.7325(6) 0.091(6) Uani 0.50 1 d P . .
H66B H 0.1634 0.9967 0.7638 0.137 Uiso 0.50 1 calc PR . .
H66A H 0.2272 0.9854 0.6886 0.137 Uiso 0.50 1 calc PR . .
H66C H 0.2723 1.0184 0.7375 0.137 Uiso 0.50 1 calc PR . .
O6 O 0.3020(7) 0.8868(5) 0.7430(3) 0.0527(19) Uani 0.50 1 d P . .
H6A H 0.3619 0.8830 0.7487 0.079 Uiso 0.50 1 calc PR . .
C67 C 0.4404(18) 1.0327(12) 0.7524(10) 0.132(9) Uani 0.50 1 d P . .
H67A H 0.3651 1.0745 0.7481 0.198 Uiso 0.50 1 calc PR . .
H67B H 0.4955 1.0323 0.7116 0.198 Uiso 0.50 1 calc PR . .
H67C H 0.4558 1.0557 0.7869 0.198 Uiso 0.50 1 calc PR . .
O7 O 0.4472(10) 0.9431(8) 0.7671(5) 0.094(4) Uani 0.50 1 d P . .
H7A H 0.4085 0.9322 0.7478 0.141 Uiso 0.50 1 calc PR . .
C68 C 0.596(3) 0.938(2) 0.8702(19) 0.103(11) Uiso 0.25 1 d PD E 2
H68C H 0.6717 0.9363 0.8520 0.155 Uiso 0.25 1 calc PR E 2
H68A H 0.5746 0.9475 0.9170 0.155 Uiso 0.25 1 calc PR E 2
H68B H 0.5432 0.9905 0.8504 0.155 Uiso 0.25 1 calc PR E 2
O8 O 0.596(3) 0.856(2) 0.8581(16) 0.128(10) Uiso 0.25 1 d PD E 2
H8A H 0.5379 0.8667 0.8473 0.192 Uiso 0.25 1 calc PR E 2
C69 C 0.2447(14) 0.3002(13) 0.8993(7) 0.097(6) Uani 0.50 1 d PD F 2
H69A H 0.2739 0.3475 0.8777 0.117 Uiso 0.50 1 calc PR F 2
H69B H 0.1989 0.3229 0.9434 0.117 Uiso 0.50 1 calc PR F 2
C70 C 0.1803(19) 0.2908(17) 0.8655(11) 0.141(8) Uiso 0.50 1 d PD F 2
H70B H 0.2285 0.2553 0.8259 0.211 Uiso 0.50 1 calc PR F 2
H70A H 0.1292 0.3536 0.8541 0.211 Uiso 0.50 1 calc PR F 2
H70C H 0.1369 0.2568 0.8920 0.211 Uiso 0.50 1 calc PR F 2
C71 C 0.374(3) 0.2364(16) 0.9437(17) 0.205(18) Uani 0.50 1 d PDU F 2
H71A H 0.4066 0.2825 0.9242 0.246 Uiso 0.50 1 calc PR F 2
H71B H 0.3176 0.2634 0.9844 0.246 Uiso 0.50 1 calc PR F 2
C72 C 0.445(3) 0.166(3) 0.9549(18) 0.25(2) Uani 0.50 1 d PDU F 2
H72C H 0.4372 0.1126 0.9414 0.377 Uiso 0.50 1 calc PR F 2
H72B H 0.4386 0.1614 1.0015 0.377 Uiso 0.50 1 calc PR F 2
H72A H 0.5180 0.1655 0.9315 0.377 Uiso 0.50 1 calc PR F 2
O9 O 0.3252(14) 0.2218(10) 0.9028(11) 0.183(9) Uani 0.50 1 d PD F 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.338(5) . ?
C1 C2 1.404(5) . ?
C1 C9 1.541(5) . ?
C2 C3 1.350(6) . ?
C2 H2 0.9500 . ?
C3 C8 1.405(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.353(6) . ?
C4 C8 1.405(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(5) . ?
C5 H5 0.9500 . ?
C6 N2 1.339(5) . ?
C6 C10 1.552(5) . ?
C7 N2 1.379(5) . ?
C7 N1 1.381(5) . ?
C7 C8 1.421(5) . ?
C9 F1 1.395(4) . ?
C9 C16 1.524(6) . ?
C9 C11 1.524(6) . ?
C10 F2 1.385(4) . ?
C10 C26 1.515(6) . ?
C10 C21 1.526(6) . ?
C11 N3 1.339(5) . ?
C11 C12 1.385(6) . ?
C12 C13 1.385(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(6) . ?
C14 H14 0.9500 . ?
C15 N3 1.343(6) . ?
C15 H15 0.9500 . ?
C16 N4 1.335(5) . ?
C16 C17 1.391(6) . ?
C17 C18 1.382(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(6) . ?
C19 H19 0.9500 . ?
C20 N4 1.342(6) . ?
C20 H20 0.9500 . ?
C21 N5 1.337(5) . ?
C21 C22 1.384(6) . ?
C22 C23 1.386(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.382(6) . ?
C24 H24 0.9500 . ?
C25 N5 1.344(5) . ?
C25 H25 0.9500 . ?
C26 N6 1.334(5) . ?
C26 C27 1.383(6) . ?
C27 C28 1.375(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.369(7) . ?
C29 H29 0.9500 . ?
C30 N6 1.343(6) . ?
C30 H30 0.9500 . ?
C31 O1 1.412(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 Co1 2.250(3) . ?
N2 Co2 2.346(3) . ?
N3 Co1 2.108(3) . ?
N4 Co1 2.120(3) . ?
N5 Co2 2.095(3) . ?
N6 Co2 2.126(3) . ?
Cl1 Co1 2.3995(11) . ?
Cl1 Co2 2.4326(11) . ?
Cl2 Co2 2.3878(11) . ?
Cl2 Co1 2.3968(12) . ?
Cl3 Co2 2.4132(11) . ?
Co1 O1 2.045(3) . ?
O1 H1A 0.74(6) . ?
C32 N7 1.340(6) . ?
C32 C33 1.393(8) . ?
C32 C40 1.547(8) . ?
C33 C34 1.352(8) . ?
C33 H33 0.9500 . ?
C34 C39 1.405(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.357(7) . ?
C35 C39 1.391(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.403(7) . ?
C36 H36 0.9500 . ?
C37 N8 1.337(6) . ?
C37 C41 1.548(6) . ?
C38 N7 1.383(6) . ?
C38 N8 1.386(6) . ?
C38 C39 1.415(7) . ?
C40 F3 1.399(6) . ?
C40 C42 1.511(9) . ?
C40 C47 1.530(7) . ?
C41 F4 1.399(6) . ?
C41 C52 1.514(7) . ?
C41 C57 1.519(6) . ?
C43 C44 1.382(11) . ?
C43 C42 1.390(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.374(11) . ?
C44 H44 0.9500 . ?
C42 N9 1.323(7) . ?
C45 C46 1.390(8) . ?
C45 H45 0.9500 . ?
C46 N9 1.349(8) . ?
C46 H46 0.9500 . ?
C47 N10 1.332(6) . ?
C47 C48 1.384(8) . ?
C48 C49 1.388(9) . ?
C48 H48 0.9500 . ?
C49 C50 1.373(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.377(8) . ?
C50 H50 0.9500 . ?
C51 N10 1.341(7) . ?
C51 H51 0.9500 . ?
C52 N11 1.343(7) . ?
C52 C53 1.397(7) . ?
C53 C54 1.379(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.365(9) . ?
C54 H54 0.9500 . ?
C55 C56 1.379(8) . ?
C55 H55 0.9500 . ?
C56 N11 1.351(6) . ?
C56 H56 0.9500 . ?
C57 N12 1.337(6) . ?
C57 C58 1.382(7) . ?
C58 C59 1.386(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.373(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.382(7) . ?
C60 H60 0.9500 . ?
C61 N12 1.342(6) . ?
C61 H61 0.9500 . ?
C62 O2 1.418(7) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N7 Co3 2.216(4) . ?
N8 Co4 2.370(4) . ?
N9 Co3 2.102(4) . ?
N10 Co3 2.103(5) . ?
N11 Co4 2.102(4) . ?
N12 Co4 2.114(4) . ?
Cl4 Co3 2.4076(15) . ?
Cl4 Co4 2.4181(13) . ?
Cl5 Co4 2.3773(15) . ?
Cl5 Co3 2.3800(13) . ?
Cl6 Co4 2.4131(14) . ?
Co3 O2 2.107(4) . ?
O2 H2A 0.88(2) . ?
Cl7 Co5B 2.195(4) . ?
Cl7 Co5A 2.319(3) . ?
Cl8 Co5C 1.897(14) . ?
Cl8 Co5A 2.071(4) . ?
Cl8 Co5B 2.554(4) . ?
Cl9 Cl12 0.615(6) . ?
Cl9 Co5B 1.894(6) . ?
Cl9 Co5A 2.216(5) . ?
Cl9 Co5C 2.24(2) . ?
Cl10 Cl11 1.317(13) . ?
Cl10 Co5B 2.261(6) . ?
Cl10 Co5C 2.399(14) . ?
Cl10 Co5A 2.437(5) . ?
Cl11 Co5C 2.054(13) . ?
Cl11 Co5A 2.255(6) . ?
Cl11 Co5B 2.377(7) . ?
Cl12 Co5B 2.350(8) . ?
Cl12 Co5A 2.700(6) . ?
Cl13 Co5C 2.528(17) . ?
Co5A Co5B 0.532(3) . ?
C63 O3 1.363(10) . ?
C63 H63B 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63C 0.9800 . ?
O3 H3A 0.8400 . ?
C64 O4 1.416(6) . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C64 H64A 0.9800 . ?
O4 H4A 0.8400 . ?
C65 O5 1.36(3) . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C65 H65A 0.9800 . ?
O5 H5A 0.8400 . ?
C66 O6 1.352(14) . ?
C66 H66B 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66C 0.9800 . ?
O6 H6A 0.8400 . ?
C67 O7 1.367(18) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
O7 H7A 0.8400 . ?
C68 O8 1.352(19) . ?
C68 H68C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
O8 H8A 0.8400 . ?
C69 O9 1.259(15) . ?
C69 C70 1.360(16) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 H70B 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.16(4) . ?
C71 O9 1.349(18) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72C 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72A 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.8(4) . . ?
N1 C1 C9 119.3(3) . . ?
C2 C1 C9 115.9(3) . . ?
C3 C2 C1 118.5(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C8 119.3(4) . . ?
C2 C3 H3 120.3 . . ?
C8 C3 H3 120.3 . . ?
C5 C4 C8 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C8 C4 H4 120.2 . . ?
C4 C5 C6 118.1(4) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 124.9(3) . . ?
N2 C6 C10 119.9(3) . . ?
C5 C6 C10 115.1(3) . . ?
N2 C7 N1 119.9(3) . . ?
N2 C7 C8 120.3(3) . . ?
N1 C7 C8 119.9(3) . . ?
C3 C8 C4 120.1(4) . . ?
C3 C8 C7 120.0(4) . . ?
C4 C8 C7 119.8(3) . . ?
F1 C9 C16 106.3(3) . . ?
F1 C9 C11 105.8(3) . . ?
C16 C9 C11 113.1(3) . . ?
F1 C9 C1 107.2(3) . . ?
C16 C9 C1 112.4(3) . . ?
C11 C9 C1 111.5(3) . . ?
F2 C10 C26 107.4(3) . . ?
F2 C10 C21 105.2(3) . . ?
C26 C10 C21 113.7(3) . . ?
F2 C10 C6 106.7(3) . . ?
C26 C10 C6 111.3(3) . . ?
C21 C10 C6 112.0(3) . . ?
N3 C11 C12 122.7(4) . . ?
N3 C11 C9 115.2(4) . . ?
C12 C11 C9 122.1(4) . . ?
C13 C12 C11 118.4(4) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C14 C13 C12 119.1(4) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C15 C14 C13 119.0(4) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N3 C15 C14 122.4(4) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N4 C16 C17 122.6(4) . . ?
N4 C16 C9 115.4(4) . . ?
C17 C16 C9 122.0(4) . . ?
C18 C17 C16 118.2(4) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 118.2(4) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N4 C20 C19 123.0(4) . . ?
N4 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N5 C21 C22 123.0(4) . . ?
N5 C21 C10 115.7(3) . . ?
C22 C21 C10 121.3(4) . . ?
C21 C22 C23 118.1(4) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 119.3(4) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 119.0(4) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
N5 C25 C24 122.0(4) . . ?
N5 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
N6 C26 C27 122.8(4) . . ?
N6 C26 C10 115.9(3) . . ?
C27 C26 C10 121.2(4) . . ?
C28 C27 C26 118.5(5) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C27 C28 C29 119.0(5) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 119.1(5) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
N6 C30 C29 122.3(5) . . ?
N6 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
O1 C31 H31A 109.5 . . ?
O1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 N1 C7 117.5(3) . . ?
C1 N1 Co1 112.6(2) . . ?
C7 N1 Co1 129.7(2) . . ?
C6 N2 C7 117.3(3) . . ?
C6 N2 Co2 111.4(2) . . ?
C7 N2 Co2 131.2(2) . . ?
C11 N3 C15 118.3(4) . . ?
C11 N3 Co1 119.1(3) . . ?
C15 N3 Co1 122.3(3) . . ?
C16 N4 C20 118.2(4) . . ?
C16 N4 Co1 118.1(3) . . ?
C20 N4 Co1 123.0(3) . . ?
C21 N5 C25 118.5(3) . . ?
C21 N5 Co2 120.0(3) . . ?
C25 N5 Co2 121.0(3) . . ?
C26 N6 C30 118.3(4) . . ?
C26 N6 Co2 119.7(3) . . ?
C30 N6 Co2 121.9(3) . . ?
Co1 Cl1 Co2 84.15(4) . . ?
Co2 Cl2 Co1 85.19(4) . . ?
O1 Co1 N3 88.37(13) . . ?
O1 Co1 N4 89.27(13) . . ?
N3 Co1 N4 85.00(14) . . ?
O1 Co1 N1 174.25(13) . . ?
N3 Co1 N1 85.97(12) . . ?
N4 Co1 N1 89.25(12) . . ?
O1 Co1 Cl2 93.80(10) . . ?
N3 Co1 Cl2 172.63(10) . . ?
N4 Co1 Cl2 87.99(10) . . ?
N1 Co1 Cl2 91.70(9) . . ?
O1 Co1 Cl1 89.77(10) . . ?
N3 Co1 Cl1 93.32(10) . . ?
N4 Co1 Cl1 178.08(11) . . ?
N1 Co1 Cl1 91.55(9) . . ?
Cl2 Co1 Cl1 93.73(4) . . ?
N5 Co2 N6 88.11(13) . . ?
N5 Co2 N2 84.74(12) . . ?
N6 Co2 N2 84.47(12) . . ?
N5 Co2 Cl2 174.06(10) . . ?
N6 Co2 Cl2 88.31(9) . . ?
N2 Co2 Cl2 90.21(8) . . ?
N5 Co2 Cl3 89.72(9) . . ?
N6 Co2 Cl3 93.94(9) . . ?
N2 Co2 Cl3 174.28(8) . . ?
Cl2 Co2 Cl3 95.25(4) . . ?
N5 Co2 Cl1 89.72(9) . . ?
N6 Co2 Cl1 171.36(9) . . ?
N2 Co2 Cl1 87.00(9) . . ?
Cl2 Co2 Cl1 93.12(4) . . ?
Cl3 Co2 Cl1 94.41(4) . . ?
C31 O1 Co1 128.6(3) . . ?
C31 O1 H1A 112(5) . . ?
Co1 O1 H1A 119(5) . . ?
N7 C32 C33 124.4(5) . . ?
N7 C32 C40 119.6(5) . . ?
C33 C32 C40 116.0(5) . . ?
C34 C33 C32 119.4(5) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C39 118.9(5) . . ?
C33 C34 H34 120.6 . . ?
C39 C34 H34 120.6 . . ?
C36 C35 C39 119.3(5) . . ?
C36 C35 H35 120.3 . . ?
C39 C35 H35 120.3 . . ?
C35 C36 C37 118.2(5) . . ?
C35 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N8 C37 C36 125.0(4) . . ?
N8 C37 C41 119.0(4) . . ?
C36 C37 C41 116.0(4) . . ?
N7 C38 N8 119.2(4) . . ?
N7 C38 C39 120.6(4) . . ?
N8 C38 C39 120.2(4) . . ?
C35 C39 C34 120.0(5) . . ?
C35 C39 C38 120.3(5) . . ?
C34 C39 C38 119.7(5) . . ?
F3 C40 C42 106.7(4) . . ?
F3 C40 C47 105.9(5) . . ?
C42 C40 C47 111.8(5) . . ?
F3 C40 C32 106.7(4) . . ?
C42 C40 C32 112.9(5) . . ?
C47 C40 C32 112.2(4) . . ?
F4 C41 C52 105.5(4) . . ?
F4 C41 C57 106.1(4) . . ?
C52 C41 C57 114.6(4) . . ?
F4 C41 C37 106.4(4) . . ?
C52 C41 C37 112.5(4) . . ?
C57 C41 C37 111.0(4) . . ?
C44 C43 C42 118.1(7) . . ?
C44 C43 H43 121.0 . . ?
C42 C43 H43 121.0 . . ?
C45 C44 C43 119.5(6) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
N9 C42 C43 123.4(6) . . ?
N9 C42 C40 115.1(4) . . ?
C43 C42 C40 121.4(6) . . ?
C44 C45 C46 118.7(7) . . ?
C44 C45 H45 120.7 . . ?
C46 C45 H45 120.7 . . ?
N9 C46 C45 122.3(7) . . ?
N9 C46 H46 118.8 . . ?
C45 C46 H46 118.8 . . ?
N10 C47 C48 122.7(5) . . ?
N10 C47 C40 115.1(5) . . ?
C48 C47 C40 122.3(5) . . ?
C47 C48 C49 118.7(5) . . ?
C47 C48 H48 120.7 . . ?
C49 C48 H48 120.7 . . ?
C50 C49 C48 118.9(6) . . ?
C50 C49 H49 120.6 . . ?
C48 C49 H49 120.6 . . ?
C49 C50 C51 118.8(5) . . ?
C49 C50 H50 120.6 . . ?
C51 C50 H50 120.6 . . ?
N10 C51 C50 123.0(5) . . ?
N10 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
N11 C52 C53 122.5(5) . . ?
N11 C52 C41 115.6(4) . . ?
C53 C52 C41 121.9(5) . . ?
C54 C53 C52 117.9(6) . . ?
C54 C53 H53 121.0 . . ?
C52 C53 H53 121.0 . . ?
C55 C54 C53 120.0(5) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C55 C56 119.2(5) . . ?
C54 C55 H55 120.4 . . ?
C56 C55 H55 120.4 . . ?
N11 C56 C55 122.1(6) . . ?
N11 C56 H56 118.9 . . ?
C55 C56 H56 118.9 . . ?
N12 C57 C58 122.8(4) . . ?
N12 C57 C41 115.2(4) . . ?
C58 C57 C41 122.0(5) . . ?
C57 C58 C59 117.9(5) . . ?
C57 C58 H58 121.0 . . ?
C59 C58 H58 121.0 . . ?
C60 C59 C58 119.7(5) . . ?
C60 C59 H59 120.1 . . ?
C58 C59 H59 120.1 . . ?
C59 C60 C61 118.8(5) . . ?
C59 C60 H60 120.6 . . ?
C61 C60 H60 120.6 . . ?
N12 C61 C60 122.1(5) . . ?
N12 C61 H61 119.0 . . ?
C60 C61 H61 119.0 . . ?
O2 C62 H62A 109.5 . . ?
O2 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
O2 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C32 N7 C38 117.1(4) . . ?
C32 N7 Co3 112.6(3) . . ?
C38 N7 Co3 130.3(3) . . ?
C37 N8 C38 116.8(4) . . ?
C37 N8 Co4 112.1(3) . . ?
C38 N8 Co4 131.0(3) . . ?
C42 N9 C46 118.0(5) . . ?
C42 N9 Co3 119.3(4) . . ?
C46 N9 Co3 122.3(4) . . ?
C47 N10 C51 117.9(5) . . ?
C47 N10 Co3 119.1(3) . . ?
C51 N10 Co3 122.9(4) . . ?
C52 N11 C56 118.1(5) . . ?
C52 N11 Co4 120.1(3) . . ?
C56 N11 Co4 121.4(4) . . ?
C57 N12 C61 118.6(4) . . ?
C57 N12 Co4 120.6(3) . . ?
C61 N12 Co4 120.6(3) . . ?
Co3 Cl4 Co4 83.47(4) . . ?
Co4 Cl5 Co3 84.95(5) . . ?
N9 Co3 N10 87.55(18) . . ?
N9 Co3 O2 87.48(17) . . ?
N10 Co3 O2 89.83(18) . . ?
N9 Co3 N7 86.27(16) . . ?
N10 Co3 N7 87.25(16) . . ?
O2 Co3 N7 173.20(15) . . ?
N9 Co3 Cl5 175.37(15) . . ?
N10 Co3 Cl5 87.81(12) . . ?
O2 Co3 Cl5 92.60(11) . . ?
N7 Co3 Cl5 93.42(10) . . ?
N9 Co3 Cl4 91.07(14) . . ?
N10 Co3 Cl4 178.57(12) . . ?
O2 Co3 Cl4 89.74(13) . . ?
N7 Co3 Cl4 93.02(11) . . ?
Cl5 Co3 Cl4 93.57(5) . . ?
N11 Co4 N12 87.52(16) . . ?
N11 Co4 N8 83.51(15) . . ?
N12 Co4 N8 84.56(14) . . ?
N11 Co4 Cl5 171.57(13) . . ?
N12 Co4 Cl5 87.63(12) . . ?
N8 Co4 Cl5 89.17(10) . . ?
N11 Co4 Cl6 92.45(12) . . ?
N12 Co4 Cl6 92.02(11) . . ?
N8 Co4 Cl6 174.80(10) . . ?
Cl5 Co4 Cl6 94.61(5) . . ?
N11 Co4 Cl4 90.69(12) . . ?
N12 Co4 Cl4 173.45(11) . . ?
N8 Co4 Cl4 88.98(10) . . ?
Cl5 Co4 Cl4 93.37(5) . . ?
Cl6 Co4 Cl4 94.35(5) . . ?
C62 O2 Co3 129.6(4) . . ?
C62 O2 H2A 109(5) . . ?
Co3 O2 H2A 113(5) . . ?
Co5B Cl7 Co5A 13.18(8) . . ?
Co5C Cl8 Co5A 27.1(6) . . ?
Co5C Cl8 Co5B 27.3(6) . . ?
Co5A Cl8 Co5B 5.53(14) . . ?
Cl12 Cl9 Co5B 132.0(13) . . ?
Cl12 Cl9 Co5A 137.2(12) . . ?
Co5B Cl9 Co5A 11.88(13) . . ?
Cl12 Cl9 Co5C 158.9(13) . . ?
Co5B Cl9 Co5C 33.3(4) . . ?
Co5A Cl9 Co5C 24.5(4) . . ?
Cl11 Cl10 Co5B 78.4(4) . . ?
Cl11 Cl10 Co5C 58.8(6) . . ?
Co5B Cl10 Co5C 30.4(5) . . ?
Cl11 Cl10 Co5A 66.2(3) . . ?
Co5B Cl10 Co5A 12.28(9) . . ?
Co5C Cl10 Co5A 22.5(4) . . ?
Cl10 Cl11 Co5C 87.9(8) . . ?
Cl10 Cl11 Co5A 81.5(4) . . ?
Co5C Cl11 Co5A 24.7(5) . . ?
Cl10 Cl11 Co5B 68.7(4) . . ?
Co5C Cl11 Co5B 31.1(6) . . ?
Co5A Cl11 Co5B 12.85(9) . . ?
Cl9 Cl12 Co5B 36.8(10) . . ?
Cl9 Cl12 Co5A 33.9(10) . . ?
Co5B Cl12 Co5A 9.14(11) . . ?
Cl8 Co5C Cl11 120.6(9) . . ?
Cl8 Co5C Cl9 112.7(6) . . ?
Cl11 Co5C Cl9 123.9(9) . . ?
Cl8 Co5C Cl10 150.4(7) . . ?
Cl11 Co5C Cl10 33.3(4) . . ?
Cl9 Co5C Cl10 90.6(7) . . ?
Cl8 Co5C Cl13 93.9(10) . . ?
Cl11 Co5C Cl13 89.7(8) . . ?
Cl9 Co5C Cl13 103.5(7) . . ?
Cl10 Co5C Cl13 98.2(7) . . ?
Co5B Co5A Cl8 152.4(7) . . ?
Co5B Co5A Cl9 47.1(7) . . ?
Cl8 Co5A Cl9 107.0(2) . . ?
Co5B Co5A Cl11 96.8(8) . . ?
Cl8 Co5A Cl11 105.0(3) . . ?
Cl9 Co5A Cl11 115.8(4) . . ?
Co5B Co5A Cl7 70.1(7) . . ?
Cl8 Co5A Cl7 116.84(15) . . ?
Cl9 Co5A Cl7 103.8(2) . . ?
Cl11 Co5A Cl7 108.9(3) . . ?
Co5B Co5A Cl10 64.6(7) . . ?
Cl8 Co5A Cl10 134.2(2) . . ?
Cl9 Co5A Cl10 90.1(2) . . ?
Cl11 Co5A Cl10 32.3(3) . . ?
Cl7 Co5A Cl10 98.69(19) . . ?
Co5B Co5A Cl12 44.5(7) . . ?
Cl8 Co5A Cl12 108.3(2) . . ?
Cl9 Co5A Cl12 8.9(3) . . ?
Cl11 Co5A Cl12 122.8(4) . . ?
Cl7 Co5A Cl12 95.66(17) . . ?
Cl10 Co5A Cl12 95.0(2) . . ?
Co5A Co5B Cl9 121.1(8) . . ?
Co5A Co5B Cl7 96.8(7) . . ?
Cl9 Co5B Cl7 121.4(3) . . ?
Co5A Co5B Cl10 103.1(7) . . ?
Cl9 Co5B Cl10 104.7(3) . . ?
Cl7 Co5B Cl10 108.2(3) . . ?
Co5A Co5B Cl12 126.3(8) . . ?
Cl9 Co5B Cl12 11.2(3) . . ?
Cl7 Co5B Cl12 110.2(2) . . ?
Cl10 Co5B Cl12 110.6(3) . . ?
Co5A Co5B Cl11 70.3(7) . . ?
Cl9 Co5B Cl11 124.5(4) . . ?
Cl7 Co5B Cl11 108.9(3) . . ?
Cl10 Co5B Cl11 32.9(3) . . ?
Cl12 Co5B Cl11 134.3(4) . . ?
Co5A Co5B Cl8 22.0(6) . . ?
Cl9 Co5B Cl8 100.5(3) . . ?
Cl7 Co5B Cl8 103.71(13) . . ?
Cl10 Co5B Cl8 119.18(19) . . ?
Cl12 Co5B Cl8 104.6(2) . . ?
Cl11 Co5B Cl8 88.1(3) . . ?
O3 C63 H63B 109.5 . . ?
O3 C63 H63A 109.5 . . ?
H63B C63 H63A 109.5 . . ?
O3 C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
C63 O3 H3A 109.5 . . ?
O4 C64 H64B 109.5 . . ?
O4 C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O4 C64 H64A 109.5 . . ?
H64B C64 H64A 109.5 . . ?
H64C C64 H64A 109.5 . . ?
C64 O4 H4A 109.5 . . ?
O5 C65 H65B 109.5 . . ?
O5 C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O5 C65 H65A 109.5 . . ?
H65B C65 H65A 109.5 . . ?
H65C C65 H65A 109.5 . . ?
C65 O5 H5A 109.5 . . ?
O6 C66 H66B 109.5 . . ?
O6 C66 H66A 109.5 . . ?
H66B C66 H66A 109.5 . . ?
O6 C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
C66 O6 H6A 109.5 . . ?
O7 C67 H67A 109.5 . . ?
O7 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
O7 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C67 O7 H7A 109.5 . . ?
O8 C68 H68C 109.5 . . ?
O8 C68 H68A 109.4 . . ?
H68C C68 H68A 109.5 . . ?
O8 C68 H68B 109.5 . . ?
H68C C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C68 O8 H8A 109.4 . . ?
O9 C69 C70 109.9(18) . . ?
O9 C69 H69A 109.7 . . ?
C70 C69 H69A 109.7 . . ?
O9 C69 H69B 109.7 . . ?
C70 C69 H69B 109.7 . . ?
H69A C69 H69B 108.2 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70A 109.5 . . ?
H70B C70 H70A 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
C72 C71 O9 111(3) . . ?
C72 C71 H71A 109.4 . . ?
O9 C71 H71A 109.4 . . ?
C72 C71 H71B 109.4 . . ?
O9 C71 H71B 109.4 . . ?
H71A C71 H71B 108.0 . . ?
C71 C72 H72C 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72C C72 H72B 109.5 . . ?
C71 C72 H72A 109.5 . . ?
H72C C72 H72A 109.5 . . ?
H72B C72 H72A 109.5 . . ?
C69 O9 C71 104.8(18) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.101
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol, diethylether'
_chemical_properties_physical    Hygroscopic
_database_code_depnum_ccdc_archive 'CCDC 1022462'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[Ni2(u-Cl)2Cl(CH3OH)(DPFN)][Cl]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Ni2(u-Cl)2Cl(CH3OH)(DPFN)][Cl]'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C31 H24 Cl3 F2 N6 Ni2 O 1+, Cl 1-, 3.25(C H4 O)'
_chemical_formula_sum            'C34.25 H37 Cl4 F2 N6 Ni2 O4.25'
_chemical_formula_weight         897.89

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.8504(5)
_cell_length_b                   13.3500(6)
_cell_length_c                   23.8878(10)
_cell_angle_alpha                97.747(2)
_cell_angle_beta                 93.565(2)
_cell_angle_gamma                102.721(2)
_cell_volume                     3636.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9848
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.39

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1606
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7908
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40932
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.45
_reflns_number_total             13562
_reflns_number_gt                8982
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The coordinated methanol ligand consisting of atoms C62 O2 is significantly disordered preventing location of the hydroxyl hydrogen atom and atom C62 was treated with a tight isotropic restraint.

The chloride anion modeled by Cl8A and Cl8B is disordered over two sites refined against each other to a total structure occupancy factor of 1.

All hydrogen atoms were modeled with a constrained riding model except for H1A bound to the nickel-coordinated methanol ligand which was located from the electron density map.  The bond length for H1A O2 was restrained to a chemically appropiate value.

Due to initial indication of monoclinic unit cell symmetry, data collection was not optimized for the triclinic unit cell of the crystal, resulting in a low data completeness of 0.948. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 0.000 0.000 720 232 '13 CH3OH'
_platon_squeeze_details          
;
The unit cell contains a large solvent void containing disordered methanol and ether molecules which has been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0655P)²+4.9814P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13562
_refine_ls_number_parameters     846
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1515
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1513(4) 0.7354(4) 0.00745(18) 0.0209(10) Uani 1 1 d . . .
C2 C 0.0397(4) 0.7324(4) -0.0182(2) 0.0240(11) Uani 1 1 d . . .
H2 H 0.0312 0.7719 -0.0478 0.029 Uiso 1 1 calc R . .
C3 C -0.0537(4) 0.6736(4) -0.0005(2) 0.0238(11) Uani 1 1 d . . .
H3 H -0.1292 0.6697 -0.0178 0.029 Uiso 1 1 calc R . .
C4 C -0.1361(4) 0.5598(4) 0.0653(2) 0.0250(11) Uani 1 1 d . . .
H4 H -0.2121 0.5571 0.0491 0.030 Uiso 1 1 calc R . .
C5 C -0.1209(4) 0.5078(4) 0.1093(2) 0.0268(11) Uani 1 1 d . . .
H5 H -0.1854 0.4687 0.1247 0.032 Uiso 1 1 calc R . .
C6 C -0.0056(4) 0.5138(4) 0.1314(2) 0.0243(11) Uani 1 1 d . . .
C7 C 0.0755(4) 0.6209(4) 0.06822(19) 0.0193(10) Uani 1 1 d . . .
C8 C -0.0384(4) 0.6176(4) 0.04403(19) 0.0231(11) Uani 1 1 d . . .
C9 C 0.2541(4) 0.8032(4) -0.01582(19) 0.0213(10) Uani 1 1 d . . .
C10 C 0.0059(4) 0.4522(4) 0.1808(2) 0.0318(13) Uani 1 1 d . . .
C11 C 0.3306(4) 0.8869(4) 0.0292(2) 0.0233(11) Uani 1 1 d . . .
C12 C 0.3436(4) 0.9903(4) 0.0270(2) 0.0277(11) Uani 1 1 d . . .
H12 H 0.3027 1.0131 -0.0024 0.033 Uiso 1 1 calc R . .
C13 C 0.4178(4) 1.0618(4) 0.0684(2) 0.0339(13) Uani 1 1 d . . .
H13 H 0.4288 1.1343 0.0678 0.041 Uiso 1 1 calc R . .
C14 C 0.4755(4) 1.0250(4) 0.1107(2) 0.0351(13) Uani 1 1 d . . .
H14 H 0.5263 1.0720 0.1398 0.042 Uiso 1 1 calc R . .
C15 C 0.4579(4) 0.9194(4) 0.1099(2) 0.0336(13) Uani 1 1 d . . .
H15 H 0.4982 0.8941 0.1385 0.040 Uiso 1 1 calc R . .
C16 C 0.3229(4) 0.7367(4) -0.04862(19) 0.0203(10) Uani 1 1 d . . .
C17 C 0.3313(4) 0.7337(4) -0.1064(2) 0.0237(11) Uani 1 1 d . . .
H17 H 0.2929 0.7741 -0.1275 0.028 Uiso 1 1 calc R . .
C18 C 0.3968(4) 0.6706(4) -0.1326(2) 0.0238(11) Uani 1 1 d . . .
H18 H 0.4044 0.6670 -0.1722 0.029 Uiso 1 1 calc R . .
C19 C 0.4513(4) 0.6127(4) -0.10055(19) 0.0228(11) Uani 1 1 d . . .
H19 H 0.4966 0.5690 -0.1180 0.027 Uiso 1 1 calc R . .
C20 C 0.4396(4) 0.6187(4) -0.0438(2) 0.0262(11) Uani 1 1 d . . .
H20 H 0.4778 0.5791 -0.0222 0.031 Uiso 1 1 calc R . .
C21 C 0.0695(4) 0.5213(4) 0.2342(2) 0.0285(12) Uani 1 1 d . . .
C22 C 0.0160(5) 0.5342(5) 0.2835(2) 0.0456(16) Uani 1 1 d . . .
H22 H -0.0623 0.4991 0.2853 0.055 Uiso 1 1 calc R . .
C23 C 0.0797(6) 0.5998(5) 0.3304(3) 0.0513(17) Uani 1 1 d . . .
H23 H 0.0453 0.6112 0.3649 0.062 Uiso 1 1 calc R . .
C24 C 0.1909(5) 0.6468(5) 0.3261(2) 0.0407(14) Uani 1 1 d . . .
H24 H 0.2359 0.6913 0.3579 0.049 Uiso 1 1 calc R . .
C25 C 0.2401(5) 0.6307(4) 0.2758(2) 0.0345(13) Uani 1 1 d . . .
H25 H 0.3188 0.6639 0.2734 0.041 Uiso 1 1 calc R . .
C26 C 0.0595(4) 0.3607(4) 0.1649(2) 0.0258(11) Uani 1 1 d . . .
C27 C 0.0031(5) 0.2604(4) 0.1702(2) 0.0360(13) Uani 1 1 d . . .
H27 H -0.0709 0.2461 0.1845 0.043 Uiso 1 1 calc R . .
C28 C 0.0583(5) 0.1822(4) 0.1538(2) 0.0390(14) Uani 1 1 d . . .
H28 H 0.0229 0.1124 0.1570 0.047 Uiso 1 1 calc R . .
C29 C 0.1665(5) 0.2057(4) 0.1325(2) 0.0335(13) Uani 1 1 d . . .
H29 H 0.2048 0.1523 0.1202 0.040 Uiso 1 1 calc R . .
C30 C 0.2159(4) 0.3075(4) 0.1300(2) 0.0278(12) Uani 1 1 d . . .
H30 H 0.2898 0.3241 0.1159 0.033 Uiso 1 1 calc R . .
C31 C 0.5947(5) 0.6750(5) 0.1270(3) 0.0459(16) Uani 1 1 d . . .
H31A H 0.6393 0.7349 0.1537 0.069 Uiso 1 1 calc R . .
H31B H 0.6478 0.6351 0.1103 0.069 Uiso 1 1 calc R . .
H31C H 0.5389 0.6308 0.1471 0.069 Uiso 1 1 calc R . .
N1 N 0.1712(3) 0.6801(3) 0.04822(15) 0.0160(8) Uani 1 1 d . . .
N2 N 0.0897(3) 0.5660(3) 0.11222(15) 0.0204(9) Uani 1 1 d . . .
N3 N 0.3852(3) 0.8511(3) 0.06989(16) 0.0243(9) Uani 1 1 d . . .
N4 N 0.3748(3) 0.6798(3) -0.01750(16) 0.0232(9) Uani 1 1 d . . .
N5 N 0.1787(3) 0.5693(3) 0.23047(17) 0.0260(9) Uani 1 1 d . . .
N6 N 0.1646(3) 0.3847(3) 0.14658(15) 0.0204(9) Uani 1 1 d . . .
F1 F 0.2082(2) 0.8565(2) -0.05500(11) 0.0278(6) Uani 1 1 d . . .
F2 F -0.1071(2) 0.4129(2) 0.19447(13) 0.0391(8) Uani 1 1 d . . .
Cl1 Cl 0.33775(10) 0.71984(9) 0.16649(5) 0.0261(3) Uani 1 1 d . . .
Cl2 Cl 0.32368(9) 0.51075(9) 0.06505(5) 0.0203(2) Uani 1 1 d . . .
Cl3 Cl 0.40918(10) 0.49986(10) 0.20807(5) 0.0259(3) Uani 1 1 d . . .
Ni1 Ni 0.35619(5) 0.69302(5) 0.06852(2) 0.02084(16) Uani 1 1 d . . .
Ni2 Ni 0.25108(5) 0.53990(5) 0.15539(2) 0.01973(15) Uani 1 1 d . . .
O1 O 0.5344(3) 0.7100(3) 0.08346(15) 0.0352(9) Uani 1 1 d D . .
H1A H 0.584(6) 0.741(6) 0.060(3) 0.11(3) Uiso 1 1 d D . .
C32 C 0.4845(5) 0.7365(4) 0.5365(2) 0.0368(13) Uani 1 1 d . . .
C33 C 0.3670(5) 0.6862(4) 0.5238(2) 0.0410(14) Uani 1 1 d . . .
H33 H 0.3102 0.7014 0.5479 0.049 Uiso 1 1 calc R . .
C34 C 0.3370(5) 0.6146(4) 0.4757(2) 0.0383(14) Uani 1 1 d . . .
H34 H 0.2583 0.5785 0.4657 0.046 Uiso 1 1 calc R . .
C35 C 0.3944(4) 0.5252(4) 0.3905(2) 0.0364(13) Uani 1 1 d . . .
H35 H 0.3162 0.4878 0.3802 0.044 Uiso 1 1 calc R . .
C36 C 0.4779(4) 0.5116(4) 0.3563(2) 0.0326(12) Uani 1 1 d . . .
H36 H 0.4588 0.4686 0.3204 0.039 Uiso 1 1 calc R . .
C37 C 0.5925(4) 0.5619(4) 0.3747(2) 0.0296(12) Uani 1 1 d . . .
C38 C 0.5411(4) 0.6454(4) 0.4575(2) 0.0299(12) Uani 1 1 d . . .
C39 C 0.4236(4) 0.5948(4) 0.4413(2) 0.0311(12) Uani 1 1 d . . .
C40 C 0.5116(5) 0.8205(5) 0.5906(2) 0.0416(14) Uani 1 1 d . . .
C41 C 0.6845(4) 0.5364(4) 0.3356(2) 0.0328(13) Uani 1 1 d . . .
C42 C 0.5816(5) 0.7870(4) 0.6372(2) 0.0426(15) Uani 1 1 d . . .
C43 C 0.5420(6) 0.7760(5) 0.6903(2) 0.0500(17) Uani 1 1 d . . .
H43 H 0.4691 0.7896 0.6989 0.060 Uiso 1 1 calc R . .
C44 C 0.6108(6) 0.7450(5) 0.7298(3) 0.0575(18) Uani 1 1 d . . .
H44 H 0.5859 0.7371 0.7663 0.069 Uiso 1 1 calc R . .
C45 C 0.7166(6) 0.7256(5) 0.7163(3) 0.0584(19) Uani 1 1 d . . .
H45 H 0.7644 0.7027 0.7429 0.070 Uiso 1 1 calc R . .
C46 C 0.7509(6) 0.7401(5) 0.6634(3) 0.0541(17) Uani 1 1 d . . .
H46 H 0.8243 0.7282 0.6544 0.065 Uiso 1 1 calc R . .
C47 C 0.5696(5) 0.9269(4) 0.5763(2) 0.0420(15) Uani 1 1 d . . .
C48 C 0.5134(6) 1.0073(5) 0.5818(3) 0.0490(16) Uani 1 1 d . . .
H48 H 0.4372 0.9987 0.5935 0.059 Uiso 1 1 calc R . .
C49 C 0.5758(6) 1.1033(5) 0.5688(3) 0.0528(17) Uani 1 1 d . . .
H49 H 0.5415 1.1615 0.5715 0.063 Uiso 1 1 calc R . .
C50 C 0.6854(6) 1.1120(5) 0.5526(3) 0.0482(16) Uani 1 1 d . . .
H50 H 0.7276 1.1767 0.5445 0.058 Uiso 1 1 calc R . .
C51 C 0.7348(6) 1.0287(4) 0.5480(2) 0.0460(15) Uani 1 1 d . . .
H51 H 0.8113 1.0362 0.5367 0.055 Uiso 1 1 calc R . .
C52 C 0.7612(4) 0.4758(5) 0.3631(2) 0.0315(13) Uani 1 1 d . . .
C53 C 0.7683(4) 0.3777(5) 0.3381(2) 0.0367(13) Uani 1 1 d . . .
H53 H 0.7226 0.3444 0.3039 0.044 Uiso 1 1 calc R . .
C54 C 0.8442(5) 0.3301(5) 0.3648(2) 0.0444(15) Uani 1 1 d . . .
H54 H 0.8539 0.2640 0.3483 0.053 Uiso 1 1 calc R . .
C55 C 0.9058(5) 0.3796(5) 0.4155(2) 0.0432(15) Uani 1 1 d . . .
H55 H 0.9560 0.3467 0.4351 0.052 Uiso 1 1 calc R . .
C56 C 0.8941(4) 0.4774(5) 0.4378(2) 0.0407(14) Uani 1 1 d . . .
H56 H 0.9379 0.5114 0.4725 0.049 Uiso 1 1 calc R . .
C57 C 0.7572(5) 0.6296(4) 0.3152(2) 0.0362(13) Uani 1 1 d . . .
C58 C 0.7571(5) 0.6396(5) 0.2581(2) 0.0493(16) Uani 1 1 d . . .
H58 H 0.7069 0.5894 0.2302 0.059 Uiso 1 1 calc R . .
C59 C 0.8308(6) 0.7234(6) 0.2431(3) 0.0602(19) Uani 1 1 d . . .
H59 H 0.8321 0.7326 0.2043 0.072 Uiso 1 1 calc R . .
C60 C 0.9032(6) 0.7942(6) 0.2841(3) 0.0579(19) Uani 1 1 d . . .
H60 H 0.9564 0.8514 0.2737 0.069 Uiso 1 1 calc R . .
C61 C 0.8990(5) 0.7826(5) 0.3404(3) 0.0509(16) Uani 1 1 d . . .
H61 H 0.9471 0.8336 0.3687 0.061 Uiso 1 1 calc R . .
C62 C 1.0187(12) 0.9091(11) 0.5747(5) 0.189(6) Uani 1 1 d DU . .
H62A H 1.0755 0.9161 0.6074 0.283 Uiso 1 1 calc R . .
H62B H 1.0336 0.9734 0.5580 0.283 Uiso 1 1 calc R . .
H62C H 1.0256 0.8510 0.5463 0.283 Uiso 1 1 calc R . .
N7 N 0.5703(4) 0.7184(3) 0.50664(18) 0.0350(11) Uani 1 1 d . . .
N8 N 0.6270(3) 0.6258(3) 0.42347(17) 0.0274(10) Uani 1 1 d . . .
N9 N 0.6856(4) 0.7703(3) 0.62414(19) 0.0386(12) Uani 1 1 d . . .
N10 N 0.6757(4) 0.9339(4) 0.55951(19) 0.0434(12) Uani 1 1 d . . .
N11 N 0.8231(3) 0.5255(4) 0.41219(17) 0.0335(11) Uani 1 1 d . . .
N12 N 0.8277(4) 0.7000(4) 0.35572(19) 0.0399(12) Uani 1 1 d . . .
F3 F 0.4065(3) 0.8270(3) 0.61054(14) 0.0517(9) Uani 1 1 d . . .
F4 F 0.6254(2) 0.4701(3) 0.28765(12) 0.0401(8) Uani 1 1 d . . .
Cl4 Cl 0.80355(11) 0.64500(11) 0.53464(6) 0.0376(3) Uani 1 1 d . . .
Cl5 Cl 0.79973(16) 0.84996(12) 0.46085(7) 0.0608(5) Uani 1 1 d . . .
Cl6 Cl 1.02907(12) 0.72688(14) 0.45765(6) 0.0553(5) Uani 1 1 d . . .
Ni3 Ni 0.82039(6) 0.67743(6) 0.43949(3) 0.03634(19) Uani 1 1 d . . .
Ni4 Ni 0.73978(6) 0.80309(6) 0.54731(3) 0.0425(2) Uani 1 1 d . . .
O2 O 0.8937(4) 0.8880(4) 0.5943(2) 0.0818(16) Uani 1 1 d D . .
Cl7 Cl 0.6995(2) 0.16221(16) 0.23022(7) 0.0797(6) Uani 1 1 d . . .
Cl8A Cl 0.7134(10) 0.7859(7) 0.0091(3) 0.028(3) Uani 0.46(6) 1 d P A 1
Cl8B Cl 0.740(2) 0.807(2) 0.0275(19) 0.084(6) Uani 0.54(6) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.338(6) . ?
C1 C2 1.412(6) . ?
C1 C9 1.533(6) . ?
C2 C3 1.336(6) . ?
C2 H2 0.9500 . ?
C3 C8 1.405(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.358(7) . ?
C4 C8 1.407(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.415(6) . ?
C5 H5 0.9500 . ?
C6 N2 1.333(6) . ?
C6 C10 1.543(7) . ?
C7 N2 1.382(6) . ?
C7 N1 1.384(6) . ?
C7 C8 1.424(6) . ?
C9 F1 1.402(5) . ?
C9 C16 1.509(6) . ?
C9 C11 1.528(7) . ?
C10 F2 1.402(5) . ?
C10 C26 1.512(7) . ?
C10 C21 1.517(7) . ?
C11 N3 1.333(6) . ?
C11 C12 1.362(7) . ?
C12 C13 1.390(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9500 . ?
C15 N3 1.344(6) . ?
C15 H15 0.9500 . ?
C16 N4 1.344(6) . ?
C16 C17 1.386(6) . ?
C17 C18 1.383(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.364(7) . ?
C19 H19 0.9500 . ?
C20 N4 1.361(6) . ?
C20 H20 0.9500 . ?
C21 N5 1.325(6) . ?
C21 C22 1.380(7) . ?
C22 C23 1.390(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.346(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.379(7) . ?
C24 H24 0.9500 . ?
C25 N5 1.332(6) . ?
C25 H25 0.9500 . ?
C26 N6 1.333(6) . ?
C26 C27 1.385(7) . ?
C27 C28 1.375(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.395(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.368(7) . ?
C29 H29 0.9500 . ?
C30 N6 1.335(6) . ?
C30 H30 0.9500 . ?
C31 O1 1.413(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 Ni1 2.180(3) . ?
N2 Ni2 2.233(4) . ?
N3 Ni1 2.057(4) . ?
N4 Ni1 2.068(4) . ?
N5 Ni2 2.063(4) . ?
N6 Ni2 2.075(4) . ?
Cl1 Ni1 2.3504(13) . ?
Cl1 Ni2 2.3672(13) . ?
Cl2 Ni1 2.3674(13) . ?
Cl2 Ni2 2.3877(12) . ?
Cl3 Ni2 2.3893(13) . ?
Ni1 O1 2.076(3) . ?
O1 H1A 0.90(2) . ?
C32 N7 1.325(7) . ?
C32 C33 1.400(8) . ?
C32 C40 1.559(8) . ?
C33 C34 1.365(8) . ?
C33 H33 0.9500 . ?
C34 C39 1.403(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.350(7) . ?
C35 C39 1.398(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(7) . ?
C36 H36 0.9500 . ?
C37 N8 1.331(6) . ?
C37 C41 1.542(7) . ?
C38 N8 1.390(6) . ?
C38 N7 1.392(7) . ?
C38 C39 1.411(7) . ?
C40 F3 1.377(6) . ?
C40 C42 1.520(8) . ?
C40 C47 1.528(8) . ?
C41 F4 1.393(6) . ?
C41 C57 1.507(8) . ?
C41 C52 1.518(7) . ?
C42 N9 1.348(7) . ?
C42 C43 1.394(8) . ?
C43 C44 1.373(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.383(10) . ?
C44 H44 0.9500 . ?
C45 C46 1.376(9) . ?
C45 H45 0.9500 . ?
C46 N9 1.338(8) . ?
C46 H46 0.9500 . ?
C47 N10 1.332(7) . ?
C47 C48 1.378(8) . ?
C48 C49 1.415(8) . ?
C48 H48 0.9500 . ?
C49 C50 1.363(9) . ?
C49 H49 0.9500 . ?
C50 C51 1.361(9) . ?
C50 H50 0.9500 . ?
C51 N10 1.376(7) . ?
C51 H51 0.9500 . ?
C52 N11 1.349(6) . ?
C52 C53 1.387(8) . ?
C53 C54 1.381(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.382(8) . ?
C55 H55 0.9500 . ?
C56 N11 1.331(7) . ?
C56 H56 0.9500 . ?
C57 N12 1.352(7) . ?
C57 C58 1.389(8) . ?
C58 C59 1.364(9) . ?
C58 H58 0.9500 . ?
C59 C60 1.371(10) . ?
C59 H59 0.9500 . ?
C60 C61 1.377(8) . ?
C60 H60 0.9500 . ?
C61 N12 1.341(7) . ?
C61 H61 0.9500 . ?
C62 O2 1.559(12) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N7 Ni4 2.172(4) . ?
N8 Ni3 2.235(4) . ?
N9 Ni4 2.052(5) . ?
N10 Ni4 2.046(5) . ?
N11 Ni3 2.053(5) . ?
N12 Ni3 2.068(4) . ?
Cl4 Ni4 2.3824(16) . ?
Cl4 Ni3 2.3828(14) . ?
Cl5 Ni4 2.3445(17) . ?
Cl5 Ni3 2.3606(18) . ?
Cl6 Ni3 2.4103(15) . ?
Ni4 O2 2.088(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
N1 C1 C2 124.1(4) . . ?
N1 C1 C9 119.5(4) . . ?
C2 C1 C9 116.3(4) . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C8 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C8 C3 H3 120.5 . . ?
C5 C4 C8 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
C8 C4 H4 120.2 . . ?
C4 C5 C6 117.7(4) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
N2 C6 C5 125.1(4) . . ?
N2 C6 C10 119.7(4) . . ?
C5 C6 C10 115.2(4) . . ?
N2 C7 N1 120.3(4) . . ?
N2 C7 C8 119.7(4) . . ?
N1 C7 C8 119.9(4) . . ?
C3 C8 C4 119.8(4) . . ?
C3 C8 C7 120.1(4) . . ?
C4 C8 C7 120.1(4) . . ?
F1 C9 C16 106.3(4) . . ?
F1 C9 C11 105.8(4) . . ?
C16 C9 C11 112.5(4) . . ?
F1 C9 C1 107.3(3) . . ?
C16 C9 C1 110.7(4) . . ?
C11 C9 C1 113.7(4) . . ?
F2 C10 C26 107.5(4) . . ?
F2 C10 C21 105.8(4) . . ?
C26 C10 C21 111.3(4) . . ?
F2 C10 C6 106.7(4) . . ?
C26 C10 C6 112.8(4) . . ?
C21 C10 C6 112.2(4) . . ?
N3 C11 C12 122.7(4) . . ?
N3 C11 C9 114.9(4) . . ?
C12 C11 C9 122.4(4) . . ?
C11 C12 C13 119.0(5) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 118.5(5) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C15 C14 C13 119.0(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N3 C15 C14 121.9(5) . . ?
N3 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N4 C16 C17 122.6(4) . . ?
N4 C16 C9 114.8(4) . . ?
C17 C16 C9 122.7(4) . . ?
C18 C17 C16 118.4(4) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C17 C18 C19 119.2(4) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 119.7(4) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
N4 C20 C19 121.8(4) . . ?
N4 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
N5 C21 C22 122.1(5) . . ?
N5 C21 C10 116.2(4) . . ?
C22 C21 C10 121.7(5) . . ?
C21 C22 C23 118.3(6) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 118.7(5) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 120.4(6) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
N5 C25 C24 120.9(5) . . ?
N5 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
N6 C26 C27 123.3(5) . . ?
N6 C26 C10 114.9(4) . . ?
C27 C26 C10 121.8(5) . . ?
C28 C27 C26 117.4(5) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 H27 121.3 . . ?
C27 C28 C29 120.0(5) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 118.2(5) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
N6 C30 C29 122.8(5) . . ?
N6 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
O1 C31 H31A 109.5 . . ?
O1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 N1 C7 117.4(4) . . ?
C1 N1 Ni1 112.1(3) . . ?
C7 N1 Ni1 130.4(3) . . ?
C6 N2 C7 117.8(4) . . ?
C6 N2 Ni2 111.7(3) . . ?
C7 N2 Ni2 130.4(3) . . ?
C11 N3 C15 118.8(4) . . ?
C11 N3 Ni1 118.7(3) . . ?
C15 N3 Ni1 122.5(3) . . ?
C16 N4 C20 118.4(4) . . ?
C16 N4 Ni1 118.4(3) . . ?
C20 N4 Ni1 123.2(3) . . ?
C21 N5 C25 119.4(4) . . ?
C21 N5 Ni2 118.6(3) . . ?
C25 N5 Ni2 121.9(3) . . ?
C26 N6 C30 118.3(4) . . ?
C26 N6 Ni2 118.8(3) . . ?
C30 N6 Ni2 122.4(3) . . ?
Ni1 Cl1 Ni2 86.14(4) . . ?
Ni1 Cl2 Ni2 85.30(4) . . ?
N3 Ni1 N4 87.63(15) . . ?
N3 Ni1 O1 88.60(15) . . ?
N4 Ni1 O1 88.68(14) . . ?
N3 Ni1 N1 89.34(14) . . ?
N4 Ni1 N1 88.28(14) . . ?
O1 Ni1 N1 176.40(13) . . ?
N3 Ni1 Cl1 88.64(11) . . ?
N4 Ni1 Cl1 176.27(12) . . ?
O1 Ni1 Cl1 91.08(10) . . ?
N1 Ni1 Cl1 91.82(10) . . ?
N3 Ni1 Cl2 178.86(11) . . ?
N4 Ni1 Cl2 91.24(11) . . ?
O1 Ni1 Cl2 91.24(11) . . ?
N1 Ni1 Cl2 90.77(10) . . ?
Cl1 Ni1 Cl2 92.49(4) . . ?
N5 Ni2 N6 89.98(15) . . ?
N5 Ni2 N2 86.42(14) . . ?
N6 Ni2 N2 86.40(14) . . ?
N5 Ni2 Cl1 87.59(12) . . ?
N6 Ni2 Cl1 176.20(11) . . ?
N2 Ni2 Cl1 90.53(10) . . ?
N5 Ni2 Cl2 175.68(11) . . ?
N6 Ni2 Cl2 90.65(10) . . ?
N2 Ni2 Cl2 89.35(10) . . ?
Cl1 Ni2 Cl2 91.56(4) . . ?
N5 Ni2 Cl3 88.87(11) . . ?
N6 Ni2 Cl3 88.86(11) . . ?
N2 Ni2 Cl3 173.31(10) . . ?
Cl1 Ni2 Cl3 94.02(5) . . ?
Cl2 Ni2 Cl3 95.42(4) . . ?
C31 O1 Ni1 127.7(3) . . ?
C31 O1 H1A 111(5) . . ?
Ni1 O1 H1A 121(5) . . ?
N7 C32 C33 125.5(5) . . ?
N7 C32 C40 119.5(5) . . ?
C33 C32 C40 114.9(5) . . ?
C34 C33 C32 117.8(5) . . ?
C34 C33 H33 121.1 . . ?
C32 C33 H33 121.1 . . ?
C33 C34 C39 119.2(5) . . ?
C33 C34 H34 120.4 . . ?
C39 C34 H34 120.4 . . ?
C36 C35 C39 119.6(5) . . ?
C36 C35 H35 120.2 . . ?
C39 C35 H35 120.2 . . ?
C35 C36 C37 118.5(5) . . ?
C35 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N8 C37 C36 124.9(5) . . ?
N8 C37 C41 119.2(4) . . ?
C36 C37 C41 115.8(5) . . ?
N8 C38 N7 119.9(4) . . ?
N8 C38 C39 120.3(5) . . ?
N7 C38 C39 119.8(5) . . ?
C35 C39 C34 120.3(5) . . ?
C35 C39 C38 119.5(5) . . ?
C34 C39 C38 120.2(5) . . ?
F3 C40 C42 106.7(4) . . ?
F3 C40 C47 108.1(5) . . ?
C42 C40 C47 112.8(5) . . ?
F3 C40 C32 106.7(4) . . ?
C42 C40 C32 111.0(5) . . ?
C47 C40 C32 111.2(5) . . ?
F4 C41 C57 106.9(4) . . ?
F4 C41 C52 105.8(4) . . ?
C57 C41 C52 110.7(4) . . ?
F4 C41 C37 107.4(4) . . ?
C57 C41 C37 114.2(5) . . ?
C52 C41 C37 111.3(4) . . ?
N9 C42 C43 122.1(6) . . ?
N9 C42 C40 115.6(5) . . ?
C43 C42 C40 122.4(6) . . ?
C44 C43 C42 118.5(7) . . ?
C44 C43 H43 120.8 . . ?
C42 C43 H43 120.8 . . ?
C43 C44 C45 119.8(6) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 118.4(6) . . ?
C46 C45 H45 120.8 . . ?
C44 C45 H45 120.8 . . ?
N9 C46 C45 123.0(7) . . ?
N9 C46 H46 118.5 . . ?
C45 C46 H46 118.5 . . ?
N10 C47 C48 124.6(6) . . ?
N10 C47 C40 114.7(5) . . ?
C48 C47 C40 120.6(6) . . ?
C47 C48 C49 116.2(6) . . ?
C47 C48 H48 121.9 . . ?
C49 C48 H48 121.9 . . ?
C50 C49 C48 119.7(6) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C51 C50 C49 120.6(6) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C50 C51 N10 121.0(6) . . ?
C50 C51 H51 119.5 . . ?
N10 C51 H51 119.5 . . ?
N11 C52 C53 123.2(5) . . ?
N11 C52 C41 115.2(5) . . ?
C53 C52 C41 121.6(5) . . ?
C54 C53 C52 117.8(5) . . ?
C54 C53 H53 121.1 . . ?
C52 C53 H53 121.1 . . ?
C55 C54 C53 119.1(6) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 119.7(6) . . ?
C54 C55 H55 120.1 . . ?
C56 C55 H55 120.1 . . ?
N11 C56 C55 122.0(5) . . ?
N11 C56 H56 119.0 . . ?
C55 C56 H56 119.0 . . ?
N12 C57 C58 121.9(5) . . ?
N12 C57 C41 115.7(4) . . ?
C58 C57 C41 122.3(5) . . ?
C59 C58 C57 118.4(6) . . ?
C59 C58 H58 120.8 . . ?
C57 C58 H58 120.8 . . ?
C58 C59 C60 119.6(6) . . ?
C58 C59 H59 120.2 . . ?
C60 C59 H59 120.2 . . ?
C59 C60 C61 120.3(6) . . ?
C59 C60 H60 119.9 . . ?
C61 C60 H60 119.9 . . ?
N12 C61 C60 120.6(6) . . ?
N12 C61 H61 119.7 . . ?
C60 C61 H61 119.7 . . ?
O2 C62 H62A 109.5 . . ?
O2 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
O2 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C32 N7 C38 117.3(5) . . ?
C32 N7 Ni4 112.4(4) . . ?
C38 N7 Ni4 130.1(4) . . ?
C37 N8 C38 117.0(4) . . ?
C37 N8 Ni3 112.8(3) . . ?
C38 N8 Ni3 130.1(3) . . ?
C46 N9 C42 118.2(5) . . ?
C46 N9 Ni4 123.7(4) . . ?
C42 N9 Ni4 117.9(4) . . ?
C47 N10 C51 117.8(5) . . ?
C47 N10 Ni4 119.2(4) . . ?
C51 N10 Ni4 122.9(4) . . ?
C56 N11 C52 118.2(5) . . ?
C56 N11 Ni3 122.1(4) . . ?
C52 N11 Ni3 119.3(4) . . ?
C61 N12 C57 119.1(5) . . ?
C61 N12 Ni3 122.2(4) . . ?
C57 N12 Ni3 118.6(4) . . ?
Ni4 Cl4 Ni3 84.21(5) . . ?
Ni4 Cl5 Ni3 85.54(6) . . ?
N11 Ni3 N12 87.05(18) . . ?
N11 Ni3 N8 86.28(16) . . ?
N12 Ni3 N8 89.13(16) . . ?
N11 Ni3 Cl5 172.69(13) . . ?
N12 Ni3 Cl5 87.74(14) . . ?
N8 Ni3 Cl5 88.53(12) . . ?
N11 Ni3 Cl4 91.47(12) . . ?
N12 Ni3 Cl4 177.22(14) . . ?
N8 Ni3 Cl4 88.43(11) . . ?
Cl5 Ni3 Cl4 93.52(6) . . ?
N11 Ni3 Cl6 91.92(12) . . ?
N12 Ni3 Cl6 91.90(13) . . ?
N8 Ni3 Cl6 177.87(12) . . ?
Cl5 Ni3 Cl6 93.37(7) . . ?
Cl4 Ni3 Cl6 90.49(5) . . ?
N10 Ni4 N9 88.45(19) . . ?
N10 Ni4 O2 88.4(2) . . ?
N9 Ni4 O2 85.32(19) . . ?
N10 Ni4 N7 88.55(18) . . ?
N9 Ni4 N7 89.22(17) . . ?
O2 Ni4 N7 173.8(2) . . ?
N10 Ni4 Cl5 88.39(14) . . ?
N9 Ni4 Cl5 176.77(14) . . ?
O2 Ni4 Cl5 93.91(16) . . ?
N7 Ni4 Cl5 91.38(12) . . ?
N10 Ni4 Cl4 176.55(14) . . ?
N9 Ni4 Cl4 89.24(14) . . ?
O2 Ni4 Cl4 94.00(17) . . ?
N7 Ni4 Cl4 88.85(13) . . ?
Cl5 Ni4 Cl4 93.94(6) . . ?
C62 O2 Ni4 127.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.102
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol, diethyl ether'
_chemical_properties_physical    Hygroscopic
_database_code_depnum_ccdc_archive 'CCDC 1022463'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[Cu4(u-Cl)6(DPFN)2][Cl]2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Cu4(u-Cl)6(DPFN)2][Cl]2'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C60 H40 Cl6 Cu4 F4 N12 2+, 2(Cl 1-), 2(C H4 O), 2(C4 H8 O)'
_chemical_formula_sum            'C70 H64 Cl8 Cu4 F4 N12 O4'
_chemical_formula_weight         1751.15

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   15.1594(6)
_cell_length_b                   21.5153(8)
_cell_length_c                   43.7045(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14254.6(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7104
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7783
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44697
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.34
_reflns_number_total             3262
_reflns_number_gt                2262
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically; hydrogen atoms were included 
 into the model at their geometrically calculated positions and refined using a riding model.
 
 The methanol solvate molecule sites consisting of atoms C17 O1, and C18 O2 were
 found to be partially occupied and were modeled with structure occupancy factors
 of 0.375 for C17 O1, and 0.125 for C18 O2 (which also lies on a 2-fold axis). 
 Isotropic restraint was applied to C18 and O2.
  
 The tetrahydrofuran solvate molecule site consisting of atoms C19 C20 C21 O3 was
 centered around a two-fold axis. C21 and O3 were found to occupy symmetry-related
 positions and were constrained to have equivalent positional and anisotropic 
 displacement parameters.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0609P)²+229.9214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3262
_refine_ls_number_parameters     256
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1526
_refine_ls_wR_factor_gt          0.1318
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.074
_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
C1 C 0.6291(5) 0.8845(2) 0.07245(12) 0.0573(18) Uani 1 1 d . . .
C2 C 0.6306(7) 0.9498(3) 0.07036(14) 0.102(4) Uani 1 1 d . . .
H2 H 0.6326 0.9700 0.0510 0.122 Uiso 1 1 calc R . .
C3 C 0.6292(9) 0.9829(3) 0.09658(16) 0.136(5) Uani 1 1 d . . .
H3 H 0.6310 1.0270 0.0960 0.163 Uiso 1 1 calc R . .
C4 C 0.6250 0.9516(4) 0.1250 0.093(5) Uani 1 2 d S . .
C5 C 0.6250 0.8860(3) 0.1250 0.054(2) Uani 1 2 d S . .
C6 C 0.6307(5) 0.8461(2) 0.04261(11) 0.0519(16) Uani 1 1 d . . .
C7 C 0.7147(4) 0.8078(2) 0.03959(11) 0.0436(14) Uani 1 1 d . . .
C8 C 0.7804(5) 0.8220(3) 0.01837(12) 0.059(2) Uani 1 1 d . . .
H8 H 0.7734 0.8562 0.0048 0.071 Uiso 1 1 calc R . .
C9 C 0.8553(5) 0.7863(3) 0.01715(14) 0.060(2) Uani 1 1 d . . .
H9 H 0.9007 0.7959 0.0029 0.072 Uiso 1 1 calc R . .
C10 C 0.8645(4) 0.7369(3) 0.03654(12) 0.0508(16) Uani 1 1 d . . .
H10 H 0.9159 0.7117 0.0360 0.061 Uiso 1 1 calc R . .
C11 C 0.7967(4) 0.7245(3) 0.05700(11) 0.0419(13) Uani 1 1 d . . .
H11 H 0.8027 0.6902 0.0705 0.050 Uiso 1 1 calc R . .
C12 C 0.5461(4) 0.8090(2) 0.03891(11) 0.0424(14) Uani 1 1 d . . .
C13 C 0.4848(5) 0.8247(3) 0.01708(12) 0.0522(16) Uani 1 1 d . . .
H13 H 0.4941 0.8595 0.0041 0.063 Uiso 1 1 calc R . .
C14 C 0.4096(5) 0.7890(3) 0.01435(13) 0.0596(19) Uani 1 1 d . . .
H14 H 0.3666 0.7991 -0.0007 0.072 Uiso 1 1 calc R . .
C15 C 0.3968(4) 0.7388(3) 0.03332(13) 0.0499(16) Uani 1 1 d . . .
H15 H 0.3451 0.7140 0.0317 0.060 Uiso 1 1 calc R . .
C16 C 0.4612(4) 0.7251(3) 0.05482(12) 0.0417(13) Uani 1 1 d . . .
H16 H 0.4532 0.6905 0.0680 0.050 Uiso 1 1 calc R . .
N1 N 0.6271(4) 0.85301(19) 0.09839(9) 0.0439(11) Uani 1 1 d . . .
N2 N 0.7225(3) 0.75911(19) 0.05851(8) 0.0367(10) Uani 1 1 d . . .
N3 N 0.5348(3) 0.75960(19) 0.05754(9) 0.0364(10) Uani 1 1 d . . .
F1 F 0.6322(3) 0.88885(14) 0.01864(7) 0.0689(12) Uani 1 1 d . . .
Cl2 Cl 0.6250 0.6250 0.05973(3) 0.0313(4) Uani 1 2 d S . .
Cl1 Cl 0.72851(9) 0.71416(6) 0.12554(3) 0.0394(3) Uani 1 1 d . . .
Cu1 Cu 0.62677(4) 0.73362(3) 0.087926(12) 0.0327(2) Uani 1 1 d . . .
Cl3 Cl 0.5546(4) 0.11665(17) 0.05236(8) 0.0863(16) Uani 0.50 1 d P . 1
C17 C 0.486(2) 0.1167(14) 0.0568(5) 0.17(2) Uani 0.38 1 d PDU A 2
H17A H 0.5262 0.1516 0.0534 0.258 Uiso 0.38 1 calc PR A 2
H17B H 0.4368 0.1192 0.0423 0.258 Uiso 0.38 1 calc PR A 2
H17C H 0.5176 0.0775 0.0538 0.258 Uiso 0.38 1 calc PR A 2
O1 O 0.4508(17) 0.1194(10) 0.0890(4) 0.169(11) Uani 0.38 1 d PDU A 2
H1A H 0.4111 0.0925 0.0912 0.253 Uiso 0.38 1 calc PR A 2
C18 C 0.532(2) 0.1250 0.1250 0.14(3) Uani 0.25 2 d SPDU B 1
H18A H 0.5535 0.0836 0.1306 0.215 Uiso 0.13 1 calc PR B 1
H18B H 0.5535 0.1556 0.1399 0.215 Uiso 0.13 1 calc PR B 1
H18C H 0.5535 0.1359 0.1045 0.215 Uiso 0.13 1 calc PR B 1
O2 O 0.4382(16) 0.1250 0.1250 0.109(14) Uani 0.25 2 d SPDU B 1
H2A H 0.4197 0.0983 0.1125 0.163 Uiso 0.13 1 calc PR B 1
C19 C 0.4067(17) 0.3290(9) 0.1383(4) 0.270(16) Uani 1 1 d . . .
H19A H 0.3796 0.2893 0.1448 0.324 Uiso 1 1 calc R C 1
H19B H 0.4712 0.3258 0.1414 0.324 Uiso 1 1 calc R C 1
C20 C 0.3750 0.3750 0.1553(4) 0.233(17) Uani 1 2 d SD . .
H20A H 0.3275 0.3587 0.1686 0.279 Uiso 0.50 1 calc PR . .
H20B H 0.4225 0.3913 0.1686 0.279 Uiso 0.50 1 calc PR . .
C21 C 0.3884(16) 0.3395(9) 0.1065(3) 0.310(18) Uani 0.50 1 d PD . 1
H21A H 0.3395 0.3129 0.0992 0.372 Uiso 0.50 1 calc PR . 1
H21B H 0.4413 0.3320 0.0937 0.372 Uiso 0.50 1 calc PR . 1
O3 O 0.3884(16) 0.3395(9) 0.1065(3) 0.310(18) Uani 0.50 1 d PD . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.321(7) . ?
C1 C2 1.410(8) . ?
C1 C6 1.544(7) . ?
C2 C3 1.349(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.414(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(11) . ?
C5 N1 1.363(5) . ?
C6 F1 1.394(5) . ?
C6 C12 1.520(9) . ?
C6 C7 1.523(9) . ?
C7 N2 1.339(6) . ?
C7 C8 1.396(8) . ?
C8 C9 1.372(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.367(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(7) . ?
C10 H10 0.9500 . ?
C11 N2 1.350(7) . ?
C11 H11 0.9500 . ?
C12 N3 1.349(7) . ?
C12 C13 1.373(8) . ?
C13 C14 1.381(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(7) . ?
C15 H15 0.9500 . ?
C16 N3 1.345(7) . ?
C16 H16 0.9500 . ?
N2 Cu1 2.015(4) . ?
N3 Cu1 2.005(4) . ?
Cl2 Cu1 2.6421(9) . ?
Cl1 Cu1 2.2927(14) . ?
C17 O1 1.503(19) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O1 H1A 0.8400 . ?
C18 O2 1.42(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O2 H2A 0.8400 . ?
C19 C20 1.33(2) . ?
C19 C21 1.44(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C19 1.33(2) 2 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C21 1.58(5) 2 ?
C21 H21A 0.9900 . ?
C21 H21B 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
N1 C1 C2 124.6(5) . . ?
N1 C1 C6 116.9(4) . . ?
C2 C1 C6 118.6(5) . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 C3 118.4(4) . 11_554 ?
C3 C4 C3 123.1(8) . 11_554 ?
N1 C5 N1 117.2(6) . 11_554 ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C4 121.4(3) 11_554 . ?
F1 C6 C12 106.3(5) . . ?
F1 C6 C7 106.1(5) . . ?
C12 C6 C7 114.3(4) . . ?
F1 C6 C1 106.4(4) . . ?
C12 C6 C1 111.0(5) . . ?
C7 C6 C1 112.0(5) . . ?
N2 C7 C8 121.3(6) . . ?
N2 C7 C6 116.3(5) . . ?
C8 C7 C6 122.4(5) . . ?
C9 C8 C7 119.6(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 118.3(7) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
N2 C11 C10 122.8(6) . . ?
N2 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
N3 C12 C13 121.8(6) . . ?
N3 C12 C6 117.2(5) . . ?
C13 C12 C6 121.0(5) . . ?
C12 C13 C14 118.8(6) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 120.1(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 118.4(6) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
N3 C16 C15 121.8(6) . . ?
N3 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C1 N1 C5 117.8(4) . . ?
C7 N2 C11 118.3(5) . . ?
C7 N2 Cu1 122.9(4) . . ?
C11 N2 Cu1 118.8(3) . . ?
C16 N3 C12 119.1(5) . . ?
C16 N3 Cu1 118.8(3) . . ?
C12 N3 Cu1 122.1(4) . . ?
Cu1 Cl2 Cu1 124.40(6) . 14 ?
Cu1 Cl1 Cu1 89.87(5) . 11_554 ?
N3 Cu1 N2 90.13(17) . . ?
N3 Cu1 Cl1 173.53(12) . . ?
N2 Cu1 Cl1 91.31(13) . . ?
N3 Cu1 Cl1 91.61(13) . 11_554 ?
N2 Cu1 Cl1 173.73(12) . 11_554 ?
Cl1 Cu1 Cl1 86.31(5) . 11_554 ?
N3 Cu1 Cl2 86.02(12) . . ?
N2 Cu1 Cl2 87.16(12) . . ?
Cl1 Cu1 Cl2 100.35(4) . . ?
Cl1 Cu1 Cl2 98.97(4) 11_554 . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C17 O1 H1A 109.5 . . ?
O2 C18 H18A 109.5 . . ?
O2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C18 O2 H2A 109.5 . . ?
C20 C19 C21 111(2) . . ?
C20 C19 H19A 109.5 . . ?
C21 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C21 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 C19 112(2) 2 . ?
C19 C20 H20A 109.2 2 . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 2 . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C19 C21 C21 101.6(12) . 2 ?
C19 C21 H21A 111.4 . . ?
C21 C21 H21A 111.4 2 . ?
C19 C21 H21B 111.4 . . ?
C21 C21 H21B 111.4 2 . ?
H21A C21 H21B 109.3 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.097
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol, diethylether'
_chemical_properties_physical    Hygroscopic
_database_code_depnum_ccdc_archive 'CCDC 1022464'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_[Cu2(u-OH)(u-OH2)(DPFN)(NO3)][NO3]2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Cu2(u-OH)(u-OH2)(DPFN)(NO3)][NO3]2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H25 Cu2 F2 N7 O6 2+, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C30 H29 Cu2 F2 N9 O14'
_chemical_formula_weight         904.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   21.1143(19)
_cell_length_b                   14.7530(13)
_cell_length_c                   23.299(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.1750(10)
_cell_angle_gamma                90.00
_cell_volume                     6970.2(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      25.35

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42495
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.35
_reflns_number_total             6390
_reflns_number_gt                6036
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 Hydrogen atoms were placed at their geometrically calculated positions and
 refined using a riding model except hydrogen atoms of water molecules, aquo
 or hydroxo ligands which were located from the electron difference map.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0251P)²+11.9978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6390
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0558
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_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
N10 N 0.0000 0.61153(14) 0.2500 0.0224(5) Uani 1 2 d S . .
O12 O 0.00644(7) 0.56718(10) 0.20567(6) 0.0314(3) Uani 1 1 d . . .
O13 O 0.0000 0.69389(16) 0.2500 0.0741(10) Uani 1 2 d S . .
O14 O 0.13368(7) 0.63834(9) -0.05686(6) 0.0222(3) Uani 1 1 d . . .
O15 O -0.04740(7) 0.39848(12) 0.16308(6) 0.0292(3) Uani 1 1 d . . .
C1 C -0.00351(8) 0.84891(11) 0.12746(7) 0.0131(3) Uani 1 1 d . . .
C2 C 0.00410(8) 0.92364(11) 0.16688(7) 0.0157(3) Uani 1 1 d . . .
H2 H -0.0293 0.9685 0.1616 0.019 Uiso 1 1 calc R . .
C3 C 0.06048(8) 0.92954(11) 0.21251(7) 0.0165(3) Uani 1 1 d . . .
H3 H 0.0674 0.9796 0.2392 0.020 Uiso 1 1 calc R . .
C4 C 0.16627(8) 0.85824(11) 0.26821(7) 0.0169(3) Uani 1 1 d . . .
H4 H 0.1752 0.9054 0.2971 0.020 Uiso 1 1 calc R . .
C5 C 0.20929(8) 0.78792(11) 0.27316(7) 0.0159(3) Uani 1 1 d . . .
H5 H 0.2479 0.7841 0.3059 0.019 Uiso 1 1 calc R . .
C6 C 0.19465(8) 0.72078(11) 0.22813(7) 0.0133(3) Uani 1 1 d . . .
C7 C 0.09728(8) 0.78965(10) 0.17748(7) 0.0126(3) Uani 1 1 d . . .
C8 C 0.10853(8) 0.86079(11) 0.22000(7) 0.0146(3) Uani 1 1 d . . .
C9 C -0.06739(8) 0.84107(11) 0.07620(7) 0.0138(3) Uani 1 1 d . . .
C10 C 0.24166(8) 0.63982(11) 0.23252(7) 0.0140(3) Uani 1 1 d . . .
C11 C -0.05504(8) 0.85417(11) 0.01524(7) 0.0142(3) Uani 1 1 d . . .
C12 C -0.08055(9) 0.92825(12) -0.01971(8) 0.0187(3) Uani 1 1 d . . .
H12 H -0.1044 0.9736 -0.0055 0.022 Uiso 1 1 calc R . .
C13 C -0.07068(9) 0.93517(12) -0.07588(8) 0.0216(4) Uani 1 1 d . . .
H13 H -0.0880 0.9852 -0.1010 0.026 Uiso 1 1 calc R . .
C14 C -0.03521(9) 0.86829(12) -0.09491(8) 0.0200(4) Uani 1 1 d . . .
H14 H -0.0280 0.8716 -0.1333 0.024 Uiso 1 1 calc R . .
C15 C -0.01046(8) 0.79654(11) -0.05710(7) 0.0161(3) Uani 1 1 d . . .
H15 H 0.0141 0.7509 -0.0701 0.019 Uiso 1 1 calc R . .
C16 C -0.10562(8) 0.75365(11) 0.07753(7) 0.0140(3) Uani 1 1 d . . .
C17 C -0.16790(8) 0.75500(12) 0.08605(8) 0.0190(4) Uani 1 1 d . . .
H17 H -0.1877 0.8104 0.0925 0.023 Uiso 1 1 calc R . .
C18 C -0.20056(9) 0.67312(13) 0.08489(8) 0.0233(4) Uani 1 1 d . . .
H18 H -0.2436 0.6720 0.0900 0.028 Uiso 1 1 calc R . .
C19 C -0.17031(9) 0.59338(12) 0.07630(8) 0.0206(4) Uani 1 1 d . . .
H19 H -0.1918 0.5367 0.0759 0.025 Uiso 1 1 calc R . .
C20 C -0.10789(8) 0.59780(11) 0.06825(7) 0.0158(3) Uani 1 1 d . . .
H20 H -0.0867 0.5430 0.0627 0.019 Uiso 1 1 calc R . .
C21 C 0.27302(8) 0.63720(10) 0.18085(7) 0.0135(3) Uani 1 1 d . . .
C22 C 0.34023(8) 0.64957(11) 0.19066(8) 0.0173(3) Uani 1 1 d . . .
H22 H 0.3680 0.6613 0.2297 0.021 Uiso 1 1 calc R . .
C23 C 0.36603(8) 0.64434(12) 0.14204(8) 0.0204(4) Uani 1 1 d . . .
H23 H 0.4118 0.6537 0.1473 0.024 Uiso 1 1 calc R . .
C24 C 0.32483(8) 0.62545(12) 0.08609(8) 0.0183(3) Uani 1 1 d . . .
H24 H 0.3418 0.6208 0.0525 0.022 Uiso 1 1 calc R . .
C25 C 0.25830(8) 0.61343(11) 0.07994(7) 0.0155(3) Uani 1 1 d . . .
H25 H 0.2298 0.6000 0.0415 0.019 Uiso 1 1 calc R . .
C26 C 0.20755(8) 0.55054(11) 0.23906(7) 0.0132(3) Uani 1 1 d . . .
C27 C 0.22346(8) 0.50312(12) 0.29264(7) 0.0173(3) Uani 1 1 d . . .
H27 H 0.2565 0.5248 0.3264 0.021 Uiso 1 1 calc R . .
C28 C 0.18992(9) 0.42321(12) 0.29564(8) 0.0199(4) Uani 1 1 d . . .
H28 H 0.1995 0.3895 0.3318 0.024 Uiso 1 1 calc R . .
C29 C 0.14227(8) 0.39295(11) 0.24548(8) 0.0181(3) Uani 1 1 d . . .
H29 H 0.1193 0.3379 0.2466 0.022 Uiso 1 1 calc R . .
C30 C 0.12890(8) 0.44426(11) 0.19398(7) 0.0153(3) Uani 1 1 d . . .
H30 H 0.0959 0.4241 0.1597 0.018 Uiso 1 1 calc R . .
N1 N 0.04133(7) 0.78551(9) 0.13085(6) 0.0125(3) Uani 1 1 d . . .
N2 N 0.14176(6) 0.72113(9) 0.18159(6) 0.0129(3) Uani 1 1 d . . .
N3 N -0.01994(6) 0.78897(9) -0.00252(6) 0.0128(3) Uani 1 1 d . . .
N4 N -0.07621(7) 0.67659(9) 0.06807(6) 0.0127(3) Uani 1 1 d . . .
N5 N 0.23260(7) 0.62002(9) 0.12634(6) 0.0129(3) Uani 1 1 d . . .
N6 N 0.16104(6) 0.52177(9) 0.19075(6) 0.0130(3) Uani 1 1 d . . .
N7 N 0.18655(7) 0.40166(10) 0.08311(6) 0.0184(3) Uani 1 1 d . . .
N8 N 0.19667(7) 0.87422(9) 0.06508(6) 0.0145(3) Uani 1 1 d . . .
O1 O 0.10707(6) 0.68172(8) 0.04107(5) 0.0120(2) Uani 1 1 d . . .
O2 O 0.04473(5) 0.57691(7) 0.09864(5) 0.0122(2) Uani 1 1 d . . .
O3 O 0.14683(6) 0.46560(8) 0.05967(5) 0.0195(3) Uani 1 1 d . . .
O4 O 0.16603(8) 0.32261(9) 0.07930(7) 0.0363(3) Uani 1 1 d . . .
O5 O 0.24449(6) 0.42021(9) 0.10973(6) 0.0259(3) Uani 1 1 d . . .
O6 O -0.01903(7) 0.59508(9) -0.03711(6) 0.0190(3) Uani 1 1 d . . .
O7 O 0.13663(6) 0.85349(8) 0.05754(6) 0.0213(3) Uani 1 1 d . . .
O8 O 0.21307(6) 0.95488(8) 0.06965(6) 0.0240(3) Uani 1 1 d . . .
O9 O 0.23790(6) 0.81261(8) 0.06717(6) 0.0232(3) Uani 1 1 d . . .
F1 F -0.10792(5) 0.91218(6) 0.08347(4) 0.0171(2) Uani 1 1 d . . .
F2 F 0.29283(5) 0.65119(6) 0.28458(4) 0.0166(2) Uani 1 1 d . . .
Cu1 Cu 0.010916(9) 0.679841(12) 0.049120(8) 0.01079(6) Uani 1 1 d . . .
Cu2 Cu 0.137612(9) 0.597292(13) 0.115398(8) 0.01112(6) Uani 1 1 d . . .
H1A H 0.1132(12) 0.6650(16) 0.0090(11) 0.035(6) Uiso 1 1 d . . .
H1B H 0.1229(11) 0.7337(17) 0.0476(10) 0.031(6) Uiso 1 1 d . . .
H2A H 0.0355(10) 0.5823(14) 0.1264(10) 0.019(6) Uiso 1 1 d . . .
H6A H -0.0572(15) 0.5944(18) -0.0435(12) 0.048(8) Uiso 1 1 d . . .
H6B H -0.0133(13) 0.547(2) -0.0470(12) 0.050(9) Uiso 1 1 d . . .
H14A H 0.1084(13) 0.6293(16) -0.0867(12) 0.034(7) Uiso 1 1 d . . .
H14B H 0.1681(13) 0.6509(16) -0.0626(11) 0.036(7) Uiso 1 1 d . . .
H15A H -0.0261(12) 0.3587(18) 0.1809(11) 0.036(7) Uiso 1 1 d . . .
H15B H -0.0342(12) 0.4437(18) 0.1790(11) 0.037(7) Uiso 1 1 d . . .
N9 N 0.0000 0.19637(13) 0.2500 0.0163(4) Uani 1 2 d S . .
O10 O 0.02012(6) 0.23885(9) 0.21183(6) 0.0235(3) Uani 1 1 d . . .
O11 O 0.0000 0.11173(11) 0.2500 0.0242(4) Uani 1 2 d S . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
N10 O13 1.215(3) . ?
N10 O12 1.2616(17) . ?
N10 O12 1.2616(17) 2 ?
O14 H14A 0.76(3) . ?
O14 H14B 0.80(3) . ?
O15 H15A 0.78(3) . ?
O15 H15B 0.78(3) . ?
C1 N1 1.318(2) . ?
C1 C2 1.415(2) . ?
C1 C9 1.537(2) . ?
C2 C3 1.360(2) . ?
C2 H2 0.9500 . ?
C3 C8 1.411(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(2) . ?
C4 C8 1.409(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.413(2) . ?
C5 H5 0.9500 . ?
C6 N2 1.322(2) . ?
C6 C10 1.538(2) . ?
C7 N2 1.365(2) . ?
C7 N1 1.366(2) . ?
C7 C8 1.417(2) . ?
C9 F1 1.3937(18) . ?
C9 C11 1.526(2) . ?
C9 C16 1.527(2) . ?
C10 F2 1.3915(18) . ?
C10 C21 1.528(2) . ?
C10 C26 1.529(2) . ?
C11 N3 1.348(2) . ?
C11 C12 1.380(2) . ?
C12 C13 1.385(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(2) . ?
C14 H14 0.9500 . ?
C15 N3 1.346(2) . ?
C15 H15 0.9500 . ?
C16 N4 1.343(2) . ?
C16 C17 1.384(2) . ?
C17 C18 1.387(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(2) . ?
C19 H19 0.9500 . ?
C20 N4 1.342(2) . ?
C20 H20 0.9500 . ?
C21 N5 1.342(2) . ?
C21 C22 1.385(2) . ?
C22 C23 1.389(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(2) . ?
C24 H24 0.9500 . ?
C25 N5 1.341(2) . ?
C25 H25 0.9500 . ?
C26 N6 1.340(2) . ?
C26 C27 1.388(2) . ?
C27 C28 1.387(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.380(2) . ?
C29 H29 0.9500 . ?
C30 N6 1.343(2) . ?
C30 H30 0.9500 . ?
N1 Cu1 2.4056(13) . ?
N2 Cu2 2.3767(13) . ?
N3 Cu1 2.0069(13) . ?
N4 Cu1 2.0085(13) . ?
N5 Cu2 1.9787(14) . ?
N6 Cu2 2.0210(13) . ?
N7 O4 1.239(2) . ?
N7 O5 1.2384(19) . ?
N7 O3 1.2792(18) . ?
N8 O8 1.2357(18) . ?
N8 O9 1.2500(18) . ?
N8 O7 1.2678(18) . ?
O1 Cu2 2.0842(11) . ?
O1 Cu1 2.0905(12) . ?
O1 H1A 0.83(3) . ?
O1 H1B 0.83(3) . ?
O2 Cu2 1.9136(11) . ?
O2 Cu1 1.9204(11) . ?
O2 H2A 0.73(2) . ?
O3 Cu2 2.3747(12) . ?
O6 Cu1 2.3004(13) . ?
O6 H6A 0.78(3) . ?
O6 H6B 0.77(3) . ?
Cu1 Cu2 2.9534(3) . ?
N9 O11 1.249(3) . ?
N9 O10 1.2548(16) . ?
N9 O10 1.2548(16) 2 ?

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
O13 N10 O12 121.25(11) . . ?
O13 N10 O12 121.25(11) . 2 ?
O12 N10 O12 117.5(2) . 2 ?
H14A O14 H14B 109(2) . . ?
H15A O15 H15B 108(3) . . ?
N1 C1 C2 124.36(15) . . ?
N1 C1 C9 116.97(14) . . ?
C2 C1 C9 118.65(14) . . ?
C3 C2 C1 118.28(15) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C8 119.56(15) . . ?
C2 C3 H3 120.2 . . ?
C8 C3 H3 120.2 . . ?
C5 C4 C8 119.74(15) . . ?
C5 C4 H4 120.1 . . ?
C8 C4 H4 120.1 . . ?
C4 C5 C6 117.91(15) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
N2 C6 C5 124.49(15) . . ?
N2 C6 C10 116.08(14) . . ?
C5 C6 C10 119.42(14) . . ?
N2 C7 N1 116.65(14) . . ?
N2 C7 C8 121.43(14) . . ?
N1 C7 C8 121.92(15) . . ?
C4 C8 C3 123.39(15) . . ?
C4 C8 C7 118.47(15) . . ?
C3 C8 C7 118.12(15) . . ?
F1 C9 C11 106.72(12) . . ?
F1 C9 C16 106.70(12) . . ?
C11 C9 C16 110.75(13) . . ?
F1 C9 C1 106.53(12) . . ?
C11 C9 C1 111.92(13) . . ?
C16 C9 C1 113.73(13) . . ?
F2 C10 C21 106.76(13) . . ?
F2 C10 C26 106.85(12) . . ?
C21 C10 C26 112.11(13) . . ?
F2 C10 C6 107.11(12) . . ?
C21 C10 C6 112.37(13) . . ?
C26 C10 C6 111.25(13) . . ?
N3 C11 C12 122.80(15) . . ?
N3 C11 C9 116.53(14) . . ?
C12 C11 C9 120.65(14) . . ?
C11 C12 C13 118.64(16) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 119.16(16) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C15 C14 C13 118.94(16) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N3 C15 C14 122.41(15) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N4 C16 C17 122.50(15) . . ?
N4 C16 C9 116.14(14) . . ?
C17 C16 C9 121.32(15) . . ?
C16 C17 C18 118.14(16) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 119.85(16) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 118.45(16) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N4 C20 C19 122.40(15) . . ?
N4 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
N5 C21 C22 122.22(15) . . ?
N5 C21 C10 116.71(14) . . ?
C22 C21 C10 121.05(14) . . ?
C21 C22 C23 118.33(15) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 H22 120.8 . . ?
C24 C23 C22 119.64(16) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 118.62(16) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N5 C25 C24 122.30(15) . . ?
N5 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
N6 C26 C27 122.20(15) . . ?
N6 C26 C10 116.39(13) . . ?
C27 C26 C10 121.41(14) . . ?
C28 C27 C26 118.33(15) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C29 C28 C27 119.48(16) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C30 C29 C28 118.75(16) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
N6 C30 C29 122.13(15) . . ?
N6 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
C1 N1 C7 117.64(14) . . ?
C1 N1 Cu1 112.57(10) . . ?
C7 N1 Cu1 129.78(10) . . ?
C6 N2 C7 117.90(13) . . ?
C6 N2 Cu2 113.52(10) . . ?
C7 N2 Cu2 128.58(10) . . ?
C15 N3 C11 118.05(14) . . ?
C15 N3 Cu1 121.61(11) . . ?
C11 N3 Cu1 120.19(11) . . ?
C20 N4 C16 118.64(14) . . ?
C20 N4 Cu1 120.62(11) . . ?
C16 N4 Cu1 120.65(11) . . ?
C25 N5 C21 118.87(14) . . ?
C25 N5 Cu2 120.46(11) . . ?
C21 N5 Cu2 120.56(11) . . ?
C26 N6 C30 119.10(14) . . ?
C26 N6 Cu2 119.99(11) . . ?
C30 N6 Cu2 120.86(11) . . ?
O4 N7 O5 121.40(15) . . ?
O4 N7 O3 119.28(15) . . ?
O5 N7 O3 119.31(14) . . ?
O8 N8 O9 121.43(14) . . ?
O8 N8 O7 119.31(14) . . ?
O9 N8 O7 119.26(13) . . ?
Cu2 O1 Cu1 90.05(4) . . ?
Cu2 O1 H1A 118.7(16) . . ?
Cu1 O1 H1A 118.4(16) . . ?
Cu2 O1 H1B 112.6(15) . . ?
Cu1 O1 H1B 110.3(15) . . ?
H1A O1 H1B 106(2) . . ?
Cu2 O2 Cu1 100.76(5) . . ?
Cu2 O2 H2A 108.2(17) . . ?
Cu1 O2 H2A 107.4(17) . . ?
N7 O3 Cu2 120.91(9) . . ?
Cu1 O6 H6A 101(2) . . ?
Cu1 O6 H6B 138(2) . . ?
H6A O6 H6B 100(3) . . ?
O2 Cu1 N3 177.23(5) . . ?
O2 Cu1 N4 93.39(5) . . ?
N3 Cu1 N4 89.24(5) . . ?
O2 Cu1 O1 81.75(5) . . ?
N3 Cu1 O1 95.55(5) . . ?
N4 Cu1 O1 172.73(5) . . ?
O2 Cu1 O6 93.47(5) . . ?
N3 Cu1 O6 87.03(5) . . ?
N4 Cu1 O6 97.66(5) . . ?
O1 Cu1 O6 88.08(5) . . ?
O2 Cu1 N1 93.68(5) . . ?
N3 Cu1 N1 85.71(5) . . ?
N4 Cu1 N1 84.28(5) . . ?
O1 Cu1 N1 90.61(5) . . ?
O6 Cu1 N1 172.46(5) . . ?
O2 Cu1 Cu2 39.54(3) . . ?
N3 Cu1 Cu2 137.71(4) . . ?
N4 Cu1 Cu2 128.82(4) . . ?
O1 Cu1 Cu2 44.89(3) . . ?
O6 Cu1 Cu2 102.77(4) . . ?
N1 Cu1 Cu2 81.38(3) . . ?
O2 Cu2 N5 175.77(5) . . ?
O2 Cu2 N6 94.56(5) . . ?
N5 Cu2 N6 89.28(5) . . ?
O2 Cu2 O1 82.07(5) . . ?
N5 Cu2 O1 94.23(5) . . ?
N6 Cu2 O1 174.53(5) . . ?
O2 Cu2 O3 89.73(5) . . ?
N5 Cu2 O3 88.54(5) . . ?
N6 Cu2 O3 89.22(5) . . ?
O1 Cu2 O3 95.06(5) . . ?
O2 Cu2 N2 95.95(5) . . ?
N5 Cu2 N2 86.17(5) . . ?
N6 Cu2 N2 84.51(5) . . ?
O1 Cu2 N2 91.53(5) . . ?
O3 Cu2 N2 171.85(4) . . ?
O2 Cu2 Cu1 39.70(3) . . ?
N5 Cu2 Cu1 137.35(4) . . ?
N6 Cu2 Cu1 130.42(4) . . ?
O1 Cu2 Cu1 45.06(3) . . ?
O3 Cu2 Cu1 104.58(3) . . ?
N2 Cu2 Cu1 83.49(3) . . ?
O11 N9 O10 119.96(10) . . ?
O11 N9 O10 119.96(10) . 2 ?
O10 N9 O10 120.1(2) . 2 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.049

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    Hygroscopic
_database_code_depnum_ccdc_archive 'CCDC 1022465'
