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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  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_dpmn

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 2,7-bis(2,2'-dipyridylmethyl)-1,8-naphthyridine  
;
_chemical_name_common            DPMN
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22 N6'
_chemical_formula_sum            'C30 H22 N6'
_chemical_formula_weight         466.54

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.072(2)
_cell_length_b                   12.076(3)
_cell_length_c                   12.881(3)
_cell_angle_alpha                69.775(4)
_cell_angle_beta                 84.874(4)
_cell_angle_gamma                79.297(4)
_cell_volume                     1157.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    131(2)
_cell_measurement_reflns_used    4230
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.44

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9584
_exptl_absorpt_correction_T_max  0.9878
_exptl_absorpt_process_details   TWINABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      131(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 SMART 1000 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4230
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.44
_reflns_number_total             4230
_reflns_number_gt                3529
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4230
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_restrained_S_all      1.243
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.40140(17) 0.71337(11) 0.88136(11) 0.0231(3) Uani 1 1 d . . .
N2 N 0.24275(16) 0.72251(11) 1.03658(11) 0.0252(3) Uani 1 1 d . . .
C7 C 0.29933(19) 0.65972(13) 0.96642(13) 0.0219(4) Uani 1 1 d . . .
N6 N 0.26218(19) 0.59140(14) 1.33462(12) 0.0367(4) Uani 1 1 d . . .
C4 C 0.1490(2) 0.50019(13) 1.07326(13) 0.0240(4) Uani 1 1 d . . .
H4 H 0.1153 0.4252 1.0858 0.029 Uiso 1 1 calc R . .
C1 C 0.4661(2) 0.65491(13) 0.81386(13) 0.0219(4) Uani 1 1 d . . .
C5 C 0.0951(2) 0.56196(14) 1.14288(13) 0.0256(4) Uani 1 1 d . . .
H5 H 0.0243 0.5306 1.2052 0.031 Uiso 1 1 calc R . .
C10 C 0.0851(2) 0.74608(14) 1.19745(14) 0.0278(4) Uani 1 1 d . . .
H10 H 0.1515 0.8132 1.1760 0.033 Uiso 1 1 calc R . .
C8 C 0.2556(2) 0.54746(13) 0.98169(13) 0.0225(4) Uani 1 1 d . . .
C9 C 0.5786(2) 0.71498(14) 0.71757(13) 0.0238(4) Uani 1 1 d . . .
H9 H 0.6351 0.6511 0.6873 0.029 Uiso 1 1 calc R . .
C3 C 0.3236(2) 0.48917(14) 0.90637(13) 0.0256(4) Uani 1 1 d . . .
H3 H 0.2957 0.4139 0.9133 0.031 Uiso 1 1 calc R . .
N4 N 0.86597(18) 0.74420(12) 0.69443(11) 0.0279(3) Uani 1 1 d . . .
C6 C 0.1456(2) 0.67386(14) 1.12186(14) 0.0246(4) Uani 1 1 d . . .
C2 C 0.4301(2) 0.54166(13) 0.82323(14) 0.0256(4) Uani 1 1 d . . .
H2 H 0.4793 0.5028 0.7724 0.031 Uiso 1 1 calc R . .
N5 N -0.21187(19) 0.72863(12) 1.20642(14) 0.0367(4) Uani 1 1 d . . .
N3 N 0.4505(2) 0.76835(14) 0.54119(13) 0.0407(4) Uani 1 1 d . . .
C17 C 0.7059(2) 0.82420(15) 0.82395(15) 0.0307(4) Uani 1 1 d . . .
H17 H 0.6005 0.8396 0.8599 0.037 Uiso 1 1 calc R . .
C26 C 0.1219(2) 0.67302(14) 1.31832(14) 0.0288(4) Uani 1 1 d . . .
C21 C -0.0987(2) 0.80262(14) 1.17728(14) 0.0277(4) Uani 1 1 d . . .
C27 C 0.0213(2) 0.69265(16) 1.40491(15) 0.0346(4) Uani 1 1 d . . .
H27 H -0.0777 0.7515 1.3909 0.042 Uiso 1 1 calc R . .
C20 C 1.0004(2) 0.78113(15) 0.71787(15) 0.0316(4) Uani 1 1 d . . .
H20 H 1.1040 0.7670 0.6797 0.038 Uiso 1 1 calc R . .
C16 C 0.7198(2) 0.76551(13) 0.74740(13) 0.0231(4) Uani 1 1 d . . .
C18 C 0.8465(2) 0.86002(15) 0.84751(15) 0.0344(4) Uani 1 1 d . . .
H18 H 0.8393 0.8995 0.9004 0.041 Uiso 1 1 calc R . .
C19 C 0.9971(2) 0.83794(14) 0.79355(15) 0.0314(4) Uani 1 1 d . . .
H19 H 1.0960 0.8614 0.8084 0.038 Uiso 1 1 calc R . .
C11 C 0.4681(2) 0.80539(14) 0.62610(13) 0.0261(4) Uani 1 1 d . . .
C25 C -0.3741(2) 0.77774(16) 1.18818(19) 0.0435(5) Uani 1 1 d . . .
H25 H -0.4560 0.7261 1.2085 0.052 Uiso 1 1 calc R . .
C22 C -0.1442(2) 0.92470(15) 1.12899(15) 0.0346(4) Uani 1 1 d . . .
H22 H -0.0604 0.9748 1.1087 0.042 Uiso 1 1 calc R . .
C15 C 0.3458(3) 0.84117(19) 0.46125(17) 0.0488(6) Uani 1 1 d . . .
H15 H 0.3319 0.8161 0.4008 0.059 Uiso 1 1 calc R . .
C28 C 0.0670(3) 0.62529(16) 1.51212(16) 0.0401(5) Uani 1 1 d . . .
H28 H 0.0000 0.6376 1.5729 0.048 Uiso 1 1 calc R . .
C29 C 0.2095(3) 0.54081(18) 1.52971(16) 0.0421(5) Uani 1 1 d . . .
H29 H 0.2437 0.4935 1.6027 0.050 Uiso 1 1 calc R . .
C12 C 0.3866(2) 0.91337(14) 0.63235(15) 0.0324(4) Uani 1 1 d . . .
H12 H 0.4032 0.9377 0.6928 0.039 Uiso 1 1 calc R . .
C23 C -0.3118(3) 0.97393(16) 1.11028(17) 0.0424(5) Uani 1 1 d . . .
H23 H -0.3454 1.0578 1.0766 0.051 Uiso 1 1 calc R . .
C30 C 0.3018(3) 0.52613(18) 1.43948(16) 0.0432(5) Uani 1 1 d . . .
H30 H 0.3996 0.4662 1.4520 0.052 Uiso 1 1 calc R . .
C14 C 0.2590(3) 0.94817(18) 0.46180(17) 0.0461(5) Uani 1 1 d . . .
H14 H 0.1853 0.9961 0.4036 0.055 Uiso 1 1 calc R . .
C24 C -0.4288(3) 0.89827(17) 1.14180(17) 0.0443(5) Uani 1 1 d . . .
H24 H -0.5456 0.9290 1.1316 0.053 Uiso 1 1 calc R . .
C13 C 0.2793(3) 0.98613(17) 0.54795(18) 0.0446(5) Uani 1 1 d . . .
H13 H 0.2206 1.0613 0.5499 0.053 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.317(2) . ?
N1 C7 1.358(2) . ?
N2 C6 1.318(2) . ?
N2 C7 1.368(2) . ?
C7 C8 1.408(2) . ?
N6 C26 1.335(2) . ?
N6 C30 1.340(2) . ?
C4 C5 1.350(2) . ?
C4 C8 1.412(2) . ?
C4 H4 0.9500 . ?
C1 C2 1.413(2) . ?
C1 C9 1.520(2) . ?
C5 C6 1.413(2) . ?
C5 H5 0.9500 . ?
C10 C6 1.514(2) . ?
C10 C21 1.518(2) . ?
C10 C26 1.525(3) . ?
C10 H10 1.0000 . ?
C8 C3 1.404(2) . ?
C9 C11 1.521(2) . ?
C9 C16 1.522(2) . ?
C9 H9 1.0000 . ?
C3 C2 1.362(2) . ?
C3 H3 0.9500 . ?
N4 C16 1.337(2) . ?
N4 C20 1.341(2) . ?
C2 H2 0.9500 . ?
N5 C21 1.336(2) . ?
N5 C25 1.339(2) . ?
N3 C15 1.342(3) . ?
N3 C11 1.344(2) . ?
C17 C18 1.379(2) . ?
C17 C16 1.386(2) . ?
C17 H17 0.9500 . ?
C26 C27 1.382(2) . ?
C21 C22 1.379(2) . ?
C27 C28 1.381(3) . ?
C27 H27 0.9500 . ?
C20 C19 1.369(3) . ?
C20 H20 0.9500 . ?
C18 C19 1.375(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C11 C12 1.372(2) . ?
C25 C24 1.370(3) . ?
C25 H25 0.9500 . ?
C22 C23 1.380(3) . ?
C22 H22 0.9500 . ?
C15 C14 1.353(3) . ?
C15 H15 0.9500 . ?
C28 C29 1.366(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(3) . ?
C29 H29 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9500 . ?
C30 H30 0.9500 . ?
C14 C13 1.371(3) . ?
C14 H14 0.9500 . ?
C24 H24 0.9500 . ?
C13 H13 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C7 117.94(13) . . ?
C6 N2 C7 117.79(14) . . ?
N1 C7 N2 115.08(13) . . ?
N1 C7 C8 122.51(15) . . ?
N2 C7 C8 122.41(14) . . ?
C26 N6 C30 117.41(17) . . ?
C5 C4 C8 119.74(15) . . ?
C5 C4 H4 120.1 . . ?
C8 C4 H4 120.1 . . ?
N1 C1 C2 123.40(15) . . ?
N1 C1 C9 118.27(13) . . ?
C2 C1 C9 118.26(14) . . ?
C4 C5 C6 119.10(15) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C6 C10 C21 110.33(14) . . ?
C6 C10 C26 111.87(13) . . ?
C21 C10 C26 113.77(14) . . ?
C6 C10 H10 106.8 . . ?
C21 C10 H10 106.8 . . ?
C26 C10 H10 106.8 . . ?
C3 C8 C7 117.89(14) . . ?
C3 C8 C4 124.53(14) . . ?
C7 C8 C4 117.57(15) . . ?
C1 C9 C11 108.86(13) . . ?
C1 C9 C16 115.52(14) . . ?
C11 C9 C16 113.61(12) . . ?
C1 C9 H9 106.0 . . ?
C11 C9 H9 106.0 . . ?
C16 C9 H9 106.0 . . ?
C2 C3 C8 119.36(15) . . ?
C2 C3 H3 120.3 . . ?
C8 C3 H3 120.3 . . ?
C16 N4 C20 117.90(15) . . ?
N2 C6 C5 123.38(15) . . ?
N2 C6 C10 116.27(14) . . ?
C5 C6 C10 120.33(15) . . ?
C3 C2 C1 118.84(15) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C21 N5 C25 117.30(15) . . ?
C15 N3 C11 117.12(18) . . ?
C18 C17 C16 119.36(17) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
N6 C26 C27 122.30(17) . . ?
N6 C26 C10 115.02(15) . . ?
C27 C26 C10 122.64(16) . . ?
N5 C21 C22 122.22(17) . . ?
N5 C21 C10 116.93(14) . . ?
C22 C21 C10 120.83(15) . . ?
C28 C27 C26 118.93(18) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
N4 C20 C19 123.88(17) . . ?
N4 C20 H20 118.1 . . ?
C19 C20 H20 118.1 . . ?
N4 C16 C17 121.60(15) . . ?
N4 C16 C9 113.07(14) . . ?
C17 C16 C9 125.29(15) . . ?
C19 C18 C17 119.24(17) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C20 C19 C18 118.01(17) . . ?
C20 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
N3 C11 C12 122.83(16) . . ?
N3 C11 C9 114.38(15) . . ?
C12 C11 C9 122.72(16) . . ?
N5 C25 C24 123.67(18) . . ?
N5 C25 H25 118.2 . . ?
C24 C25 H25 118.2 . . ?
C21 C22 C23 119.80(17) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
N3 C15 C14 123.8(2) . . ?
N3 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
C29 C28 C27 119.24(19) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C28 C29 C30 118.31(19) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C11 C12 C13 118.27(18) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 H12 120.9 . . ?
C24 C23 C22 118.11(17) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
N6 C30 C29 123.80(19) . . ?
N6 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C15 C14 C13 118.75(19) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C25 C24 C23 118.88(19) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C14 C13 C12 119.21(18) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.44
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.041
_database_code_depnum_ccdc_archive 'CCDC 959033'
#######################################################################
#
#                 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_dpfn

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 2,7-bis(di-2-pyridylfluoromethyl)-1,8-naphthyridine
;
_chemical_name_common            DPFN
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H20 F2 N6'
_chemical_formula_sum            'C30 H20 F2 N6'
_chemical_formula_weight         502.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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                   8.7660(5)
_cell_length_b                   23.8721(16)
_cell_length_c                   11.4381(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.074(4)
_cell_angle_gamma                90.00
_cell_volume                     2380.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7403
_cell_measurement_theta_min      3.70
_cell_measurement_theta_max      67.98

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8441
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_monochromator  'HELIOS 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            11151
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         65.06
_reflns_number_total             3941
_reflns_number_gt                3494
_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.
;

_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)+(0.0557P)²+0.6088P] 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         3941
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 -0.09369(14) 0.31295(6) 0.51091(11) 0.0165(3) Uani 1 1 d . . .
C2 C -0.11949(15) 0.33409(6) 0.39429(11) 0.0187(3) Uani 1 1 d . . .
H2 H -0.0689 0.3670 0.3721 0.022 Uiso 1 1 calc R . .
C3 C -0.21861(15) 0.30596(6) 0.31493(11) 0.0179(3) Uani 1 1 d . . .
H3 H -0.2385 0.3191 0.2364 0.022 Uiso 1 1 calc R . .
C4 C -0.39939(15) 0.22569(6) 0.27794(11) 0.0188(3) Uani 1 1 d . . .
H4 H -0.4252 0.2362 0.1982 0.023 Uiso 1 1 calc R . .
C5 C -0.46614(15) 0.18015(6) 0.32320(11) 0.0191(3) Uani 1 1 d . . .
H5 H -0.5418 0.1591 0.2765 0.023 Uiso 1 1 calc R . .
C6 C -0.42037(14) 0.16475(6) 0.44159(11) 0.0164(3) Uani 1 1 d . . .
C7 C -0.25684(14) 0.23924(6) 0.46914(11) 0.0155(3) Uani 1 1 d . . .
C8 C -0.29134(15) 0.25703(6) 0.35126(11) 0.0167(3) Uani 1 1 d . . .
C9 C 0.01349(15) 0.34506(6) 0.60206(11) 0.0177(3) Uani 1 1 d . . .
C10 C -0.50049(15) 0.11555(6) 0.49433(11) 0.0177(3) Uani 1 1 d . . .
C11 C -0.06858(15) 0.39825(6) 0.63500(11) 0.0175(3) Uani 1 1 d . . .
C12 C -0.13082(17) 0.40272(6) 0.74159(12) 0.0236(3) Uani 1 1 d . . .
H12 H -0.1195 0.3733 0.7977 0.028 Uiso 1 1 calc R . .
C13 C -0.20960(17) 0.45120(7) 0.76380(13) 0.0283(3) Uani 1 1 d . . .
H13 H -0.2534 0.4556 0.8357 0.034 Uiso 1 1 calc R . .
C14 C -0.22360(16) 0.49306(6) 0.67987(13) 0.0265(3) Uani 1 1 d . . .
H14 H -0.2764 0.5268 0.6932 0.032 Uiso 1 1 calc R . .
C15 C -0.15894(15) 0.48461(6) 0.57596(12) 0.0215(3) Uani 1 1 d . . .
H15 H -0.1692 0.5134 0.5182 0.026 Uiso 1 1 calc R . .
C16 C 0.17238(15) 0.35573(6) 0.56284(11) 0.0187(3) Uani 1 1 d . . .
C17 C 0.23552(18) 0.31841(7) 0.48830(13) 0.0281(3) Uani 1 1 d . . .
H17 H 0.1771 0.2878 0.4548 0.034 Uiso 1 1 calc R . .
C18 C 0.38516(19) 0.32661(8) 0.46355(14) 0.0350(4) Uani 1 1 d . . .
H18 H 0.4308 0.3019 0.4123 0.042 Uiso 1 1 calc R . .
C19 C 0.46705(16) 0.37148(8) 0.51487(13) 0.0306(3) Uani 1 1 d . . .
H19 H 0.5700 0.3782 0.4998 0.037 Uiso 1 1 calc R . .
C20 C 0.39491(17) 0.40618(6) 0.58852(14) 0.0278(3) Uani 1 1 d . . .
H20 H 0.4512 0.4369 0.6238 0.033 Uiso 1 1 calc R . .
C21 C -0.64931(15) 0.13665(6) 0.53662(11) 0.0192(3) Uani 1 1 d . . .
C22 C -0.79108(17) 0.11554(7) 0.49204(13) 0.0279(3) Uani 1 1 d . . .
H22 H -0.7994 0.0875 0.4328 0.034 Uiso 1 1 calc R . .
C23 C -0.92066(17) 0.13680(8) 0.53699(14) 0.0340(4) Uani 1 1 d . . .
H23 H -1.0197 0.1232 0.5092 0.041 Uiso 1 1 calc R . .
C24 C -0.90386(18) 0.17790(7) 0.62235(13) 0.0312(4) Uani 1 1 d . . .
H24 H -0.9905 0.1927 0.6552 0.037 Uiso 1 1 calc R . .
C25 C -0.75786(18) 0.19699(7) 0.65879(12) 0.0270(3) Uani 1 1 d . . .
H25 H -0.7468 0.2259 0.7162 0.032 Uiso 1 1 calc R . .
C26 C -0.39681(15) 0.08410(5) 0.58780(11) 0.0172(3) Uani 1 1 d . . .
C27 C -0.43606(16) 0.07460(6) 0.70036(12) 0.0215(3) Uani 1 1 d . . .
H27 H -0.5286 0.0892 0.7244 0.026 Uiso 1 1 calc R . .
C28 C -0.33714(18) 0.04326(6) 0.77696(12) 0.0266(3) Uani 1 1 d . . .
H28 H -0.3610 0.0362 0.8547 0.032 Uiso 1 1 calc R . .
C29 C -0.20423(17) 0.02238(6) 0.73985(13) 0.0272(3) Uani 1 1 d . . .
H29 H -0.1352 0.0005 0.7906 0.033 Uiso 1 1 calc R . .
C30 C -0.17450(17) 0.03436(7) 0.62629(14) 0.0276(3) Uani 1 1 d . . .
H30 H -0.0826 0.0202 0.6003 0.033 Uiso 1 1 calc R . .
N1 N -0.15909(12) 0.26806(5) 0.54799(9) 0.0161(2) Uani 1 1 d . . .
N2 N -0.31975(12) 0.19247(5) 0.51264(9) 0.0162(2) Uani 1 1 d . . .
N3 N -0.08259(13) 0.43791(5) 0.55265(9) 0.0190(2) Uani 1 1 d . . .
N4 N 0.25002(14) 0.39897(5) 0.61308(10) 0.0228(3) Uani 1 1 d . . .
N5 N -0.63104(14) 0.17711(5) 0.61792(10) 0.0225(3) Uani 1 1 d . . .
N6 N -0.26735(14) 0.06472(5) 0.55082(10) 0.0232(3) Uani 1 1 d . . .
F1 F 0.03934(9) 0.31194(3) 0.70298(6) 0.02096(18) Uani 1 1 d . . .
F2 F -0.53950(9) 0.07681(3) 0.40356(7) 0.02260(19) 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 1.3070(18) . ?
C1 C2 1.4218(18) . ?
C1 C9 1.5329(17) . ?
C2 C3 1.3648(19) . ?
C2 H2 0.9500 . ?
C3 C8 1.414(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.363(2) . ?
C4 C8 1.4114(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.4195(18) . ?
C5 H5 0.9500 . ?
C6 N2 1.3133(17) . ?
C6 C10 1.5251(18) . ?
C7 N2 1.3624(18) . ?
C7 N1 1.3629(17) . ?
C7 C8 1.4154(18) . ?
C9 F1 1.3977(15) . ?
C9 C11 1.5262(19) . ?
C9 C16 1.5292(18) . ?
C10 F2 1.4054(15) . ?
C10 C21 1.5241(18) . ?
C10 C26 1.5255(18) . ?
C11 N3 1.3319(18) . ?
C11 C12 1.3915(19) . ?
C12 C13 1.385(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(2) . ?
C14 H14 0.9500 . ?
C15 N3 1.3416(19) . ?
C15 H15 0.9500 . ?
C16 N4 1.3329(19) . ?
C16 C17 1.388(2) . ?
C17 C18 1.385(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(2) . ?
C19 H19 0.9500 . ?
C20 N4 1.341(2) . ?
C20 H20 0.9500 . ?
C21 N5 1.3385(19) . ?
C21 C22 1.387(2) . ?
C22 C23 1.391(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(2) . ?
C24 H24 0.9500 . ?
C25 N5 1.338(2) . ?
C25 H25 0.9500 . ?
C26 N6 1.3352(19) . ?
C26 C27 1.3860(19) . ?
C27 C28 1.385(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.375(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.382(2) . ?
C29 H29 0.9500 . ?
C30 N6 1.336(2) . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.32(12) . . ?
N1 C1 C9 116.58(11) . . ?
C2 C1 C9 119.07(11) . . ?
C3 C2 C1 118.44(12) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C8 119.08(11) . . ?
C2 C3 H3 120.5 . . ?
C8 C3 H3 120.5 . . ?
C5 C4 C8 119.03(12) . . ?
C5 C4 H4 120.5 . . ?
C8 C4 H4 120.5 . . ?
C4 C5 C6 118.67(12) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
N2 C6 C5 124.28(12) . . ?
N2 C6 C10 116.78(11) . . ?
C5 C6 C10 118.77(11) . . ?
N2 C7 N1 114.99(11) . . ?
N2 C7 C8 122.67(12) . . ?
N1 C7 C8 122.34(12) . . ?
C4 C8 C3 123.94(11) . . ?
C4 C8 C7 117.99(12) . . ?
C3 C8 C7 118.05(12) . . ?
F1 C9 C11 107.83(10) . . ?
F1 C9 C16 105.27(10) . . ?
C11 C9 C16 113.68(11) . . ?
F1 C9 C1 108.24(10) . . ?
C11 C9 C1 108.23(10) . . ?
C16 C9 C1 113.30(10) . . ?
F2 C10 C21 107.60(10) . . ?
F2 C10 C6 107.50(10) . . ?
C21 C10 C6 108.45(11) . . ?
F2 C10 C26 105.91(10) . . ?
C21 C10 C26 114.00(10) . . ?
C6 C10 C26 113.02(10) . . ?
N3 C11 C12 123.35(13) . . ?
N3 C11 C9 115.30(11) . . ?
C12 C11 C9 121.26(12) . . ?
C13 C12 C11 118.31(13) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
C14 C13 C12 119.09(13) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 118.46(14) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.35(13) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
N4 C16 C17 122.91(13) . . ?
N4 C16 C9 116.23(12) . . ?
C17 C16 C9 120.53(13) . . ?
C18 C17 C16 118.86(15) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 118.84(15) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C20 C19 C18 118.17(14) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
N4 C20 C19 123.77(14) . . ?
N4 C20 H20 118.1 . . ?
C19 C20 H20 118.1 . . ?
N5 C21 C22 123.65(14) . . ?
N5 C21 C10 114.55(12) . . ?
C22 C21 C10 121.79(13) . . ?
C21 C22 C23 117.80(15) . . ?
C21 C22 H22 121.1 . . ?
C23 C22 H22 121.1 . . ?
C24 C23 C22 119.35(14) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 118.29(14) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
N5 C25 C24 123.75(15) . . ?
N5 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
N6 C26 C27 122.72(12) . . ?
N6 C26 C10 114.32(11) . . ?
C27 C26 C10 122.92(12) . . ?
C28 C27 C26 118.40(13) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C29 C28 C27 119.65(13) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 117.74(13) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
N6 C30 C29 123.88(14) . . ?
N6 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C1 N1 C7 117.76(11) . . ?
C6 N2 C7 117.28(11) . . ?
C11 N3 C15 117.44(11) . . ?
C16 N4 C20 117.44(13) . . ?
C25 N5 C21 117.13(13) . . ?
C26 N6 C30 117.61(12) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        65.06
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 959034'
#######################################################################
#
#                 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-OH)2(OH2)2(DPFN)][NO3]4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Co2(u-OH)2(OH2)2(DPFN)][NO3]4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H26 Co2 F2 N6 O4 4+, 4(N O3 1-)'
_chemical_formula_sum            'C30 H26 Co2 F2 N10 O16'
_chemical_formula_weight         938.47

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'
Co Co 0.3494 0.9721 '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                   26.800(2)
_cell_length_b                   10.8131(8)
_cell_length_c                   12.7351(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.8370(10)
_cell_angle_gamma                90.00
_cell_volume                     3532.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4881
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      25.31

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.590955
_exptl_absorpt_correction_T_max  0.745212
_exptl_absorpt_process_details   TWINABS

_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            3207
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         25.32
_reflns_number_total             3207
_reflns_number_gt                3100
_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 nitrate anion consisting of atoms N5 O6 O7 O8 was disordered over two sites due to the atom N5 being positioned on an inversion center.  Each atom of this anion was treated as having an occupancy factor of 0.5.

The nitrate anion consisting of atoms N6 O9 O10 O11 was disordered over two sites due to the close proximity of an inversion center.  Due to the nature of the disorder, atoms N6 and O11 were found to occupy symmetry-related positions.  For this reason, the atomic positions and anisotropic displacement factors for N6 and O11 were fixed to be equal to each other.  All of the atoms of this anion were refined with an occupancy factor of 0.5.

All of the hydrogen atoms were included at geometrically calculated positions and refined using a riding model except atoms H1A H2A H2B 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)+(0.0339P)²+4.6697P] 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         3207
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.003
_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 0.59082(7) -0.01682(18) -0.20828(16) 0.0160(4) Uani 1 1 d . . .
C2 C 0.59310(8) -0.14627(19) -0.20681(18) 0.0202(4) Uani 1 1 d . . .
H2 H 0.6256 -0.1882 -0.1914 0.024 Uiso 1 1 calc R . .
C3 C 0.54767(8) -0.21032(19) -0.2280(2) 0.0230(4) Uani 1 1 d . . .
H3 H 0.5481 -0.2982 -0.2279 0.028 Uiso 1 1 calc R . .
C4 C 0.5000 -0.1464(3) -0.2500 0.0194(6) Uani 1 2 d S . .
C5 C 0.5000 -0.0150(2) -0.2500 0.0146(5) Uani 1 2 d S . .
C6 C 0.64171(7) 0.05700(18) -0.18378(16) 0.0164(4) Uani 1 1 d . . .
C7 C 0.64248(8) 0.1399(2) -0.27866(17) 0.0163(4) Uani 1 1 d . . .
C8 C 0.68049(8) 0.1352(2) -0.33212(18) 0.0203(4) Uani 1 1 d . . .
H8 H 0.7080 0.0766 -0.3117 0.024 Uiso 1 1 calc R . .
C9 C 0.67730(9) 0.2188(2) -0.41679(19) 0.0244(5) Uani 1 1 d . . .
H9 H 0.7027 0.2178 -0.4556 0.029 Uiso 1 1 calc R . .
C10 C 0.63670(9) 0.3035(2) -0.44409(19) 0.0258(5) Uani 1 1 d . . .
H10 H 0.6339 0.3610 -0.5019 0.031 Uiso 1 1 calc R . .
C11 C 0.60053(8) 0.3031(2) -0.3862(2) 0.0219(4) Uani 1 1 d . . .
H11 H 0.5727 0.3611 -0.4048 0.026 Uiso 1 1 calc R . .
C12 C 0.64880(8) 0.1334(2) -0.08065(17) 0.0174(4) Uani 1 1 d . . .
C13 C 0.69215(9) 0.1239(2) 0.00933(18) 0.0231(5) Uani 1 1 d . . .
H13 H 0.7194 0.0674 0.0101 0.028 Uiso 1 1 calc R . .
C14 C 0.69472(9) 0.1997(2) 0.09888(19) 0.0278(5) Uani 1 1 d . . .
H14 H 0.7244 0.1972 0.1616 0.033 Uiso 1 1 calc R . .
C15 C 0.65379(10) 0.2787(2) 0.0961(2) 0.0290(6) Uani 1 1 d . . .
H15 H 0.6545 0.3290 0.1576 0.035 Uiso 1 1 calc R . .
C16 C 0.61168(9) 0.2836(2) 0.0022(2) 0.0233(5) Uani 1 1 d . . .
H16 H 0.5837 0.3383 0.0000 0.028 Uiso 1 1 calc R . .
N1 N 0.54665(6) 0.04857(15) -0.22841(13) 0.0137(3) Uani 1 1 d . . .
N2 N 0.60358(7) 0.22272(16) -0.30407(15) 0.0157(4) Uani 1 1 d . . .
N3 N 0.60960(7) 0.21281(18) -0.08544(15) 0.0172(4) Uani 1 1 d . . .
O1 O 0.50205(7) 0.24653(13) -0.15159(12) 0.0155(3) Uani 1 1 d . . .
O2 O 0.55762(6) 0.40332(13) -0.21557(15) 0.0233(3) Uani 1 1 d . . .
F1 F 0.68251(4) -0.02599(11) -0.16640(10) 0.0216(3) Uani 1 1 d . . .
Co1 Co 0.554201(9) 0.22713(2) -0.22111(2) 0.01306(9) Uani 1 1 d . . .
H1A H 0.5025(13) 0.201(3) -0.109(2) 0.027(8) Uiso 1 1 d . . .
H2A H 0.5838(12) 0.441(3) -0.212(3) 0.042(8) Uiso 1 1 d . . .
H2B H 0.5420(16) 0.431(4) -0.167(3) 0.072(13) Uiso 1 1 d . . .
N4 N 0.67918(6) 0.47988(16) 0.34989(15) 0.0209(4) Uani 1 1 d . . .
O3 O 0.63264(5) 0.43984(14) 0.31201(14) 0.0257(4) Uani 1 1 d . . .
O4 O 0.68729(6) 0.59262(15) 0.34972(18) 0.0387(4) Uani 1 1 d . . .
O5 O 0.71440(6) 0.40460(17) 0.38588(19) 0.0420(5) Uani 1 1 d . . .
N5 N 0.5000 0.0000 0.0000 0.0423(8) Uani 1 2 d S . .
O6 O 0.4874(3) 0.1091(5) 0.0037(4) 0.0647(17) Uani 0.50 1 d P . .
O7 O 0.5254(2) 0.0886(6) 0.0132(4) 0.0558(14) Uani 0.50 1 d P . .
O8 O 0.55246(16) -0.0140(4) 0.0170(3) 0.0479(10) Uani 0.50 1 d P . .
N6 N 0.49829(13) 0.4774(2) 0.0439(2) 0.0604(7) Uani 0.50 1 d P . .
O9 O 0.54199(16) 0.4217(4) 0.1023(3) 0.0422(10) Uani 0.50 1 d P . .
O10 O 0.46235(14) 0.4772(4) 0.0556(4) 0.0479(13) Uani 0.50 1 d P . .
O11 O 0.49829(13) 0.4774(2) 0.0439(2) 0.0604(7) Uani 0.50 1 d P . .


_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(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.532(3) . ?
C2 C3 1.358(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.408(2) . ?
C3 H3 0.9500 . ?
C4 C3 1.408(2) 2_654 ?
C4 C5 1.421(4) . ?
C5 N1 1.383(2) . ?
C5 N1 1.383(2) 2_654 ?
C6 F1 1.382(2) . ?
C6 C7 1.510(3) . ?
C6 C12 1.516(3) . ?
C7 N2 1.341(3) . ?
C7 C8 1.380(3) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 H10 0.9500 . ?
C11 N2 1.344(3) . ?
C11 H11 0.9500 . ?
C12 N3 1.345(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.390(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 N3 1.341(3) . ?
C16 H16 0.9500 . ?
N1 Co1 1.9408(16) . ?
N2 Co1 1.9182(19) . ?
N3 Co1 1.9306(19) . ?
O1 Co1 1.8703(16) . ?
O1 Co1 1.8787(17) 2_654 ?
O1 H1A 0.73(3) . ?
O2 Co1 1.9077(14) . ?
O2 H2A 0.80(3) . ?
O2 H2B 0.89(4) . ?
Co1 O1 1.8787(17) 2_654 ?
Co1 Co1 2.7826(5) 2_654 ?
N4 O5 1.230(2) . ?
N4 O4 1.238(2) . ?
N4 O3 1.276(2) . ?
N5 O7 1.159(5) . ?
N5 O7 1.159(5) 5_655 ?
N5 O6 1.232(5) 5_655 ?
N5 O6 1.232(5) . ?
N5 O8 1.367(4) . ?
N5 O8 1.367(4) 5_655 ?
N6 O10 1.016(4) . ?
N6 O11 1.248(5) 5_665 ?
N6 O9 1.336(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 124.28(18) . . ?
N1 C1 C6 116.71(17) . . ?
C2 C1 C6 119.01(17) . . ?
C3 C2 C1 118.28(18) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.91(19) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C3 121.1(3) 2_654 . ?
C3 C4 C5 119.43(13) 2_654 . ?
C3 C4 C5 119.43(13) . . ?
N1 C5 N1 120.4(2) . 2_654 ?
N1 C5 C4 119.80(11) . . ?
N1 C5 C4 119.80(11) 2_654 . ?
F1 C6 C7 108.68(16) . . ?
F1 C6 C12 108.68(16) . . ?
C7 C6 C12 110.03(16) . . ?
F1 C6 C1 108.10(16) . . ?
C7 C6 C1 111.35(16) . . ?
C12 C6 C1 109.93(16) . . ?
N2 C7 C8 122.6(2) . . ?
N2 C7 C6 113.57(18) . . ?
C8 C7 C6 123.78(19) . . ?
C7 C8 C9 118.1(2) . . ?
C7 C8 H8 121.0 . . ?
C9 C8 H8 121.0 . . ?
C10 C9 C8 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
N2 C11 C10 121.7(2) . . ?
N2 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
N3 C12 C13 123.0(2) . . ?
N3 C12 C6 114.11(18) . . ?
C13 C12 C6 122.9(2) . . ?
C12 C13 C14 117.9(2) . . ?
C12 C13 H13 121.1 . . ?
C14 C13 H13 121.1 . . ?
C15 C14 C13 119.5(2) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 119.2(2) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
N3 C16 C15 121.5(2) . . ?
N3 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C1 N1 C5 118.31(17) . . ?
C1 N1 Co1 116.25(12) . . ?
C5 N1 Co1 125.42(13) . . ?
C7 N2 C11 119.17(19) . . ?
C7 N2 Co1 119.73(15) . . ?
C11 N2 Co1 121.08(15) . . ?
C16 N3 C12 118.88(19) . . ?
C16 N3 Co1 122.34(16) . . ?
C12 N3 Co1 118.69(15) . . ?
Co1 O1 Co1 95.85(7) . 2_654 ?
Co1 O1 H1A 115(3) . . ?
Co1 O1 H1A 114(3) 2_654 . ?
Co1 O2 H2A 123(2) . . ?
Co1 O2 H2B 109(3) . . ?
H2A O2 H2B 112(4) . . ?
O1 Co1 O1 82.71(7) . 2_654 ?
O1 Co1 O2 84.55(7) . . ?
O1 Co1 O2 86.46(7) 2_654 . ?
O1 Co1 N2 173.14(7) . . ?
O1 Co1 N2 92.10(7) 2_654 . ?
O2 Co1 N2 90.68(8) . . ?
O1 Co1 N3 94.11(7) . . ?
O1 Co1 N3 176.49(7) 2_654 . ?
O2 Co1 N3 91.76(8) . . ?
N2 Co1 N3 90.95(7) . . ?
O1 Co1 N1 93.00(6) . . ?
O1 Co1 N1 91.33(6) 2_654 . ?
O2 Co1 N1 176.89(6) . . ?
N2 Co1 N1 91.59(7) . . ?
N3 Co1 N1 90.32(7) . . ?
O1 Co1 Co1 42.19(5) . 2_654 ?
O1 Co1 Co1 41.96(5) 2_654 2_654 ?
O2 Co1 Co1 92.58(5) . 2_654 ?
N2 Co1 Co1 133.49(6) . 2_654 ?
N3 Co1 Co1 135.23(6) . 2_654 ?
N1 Co1 Co1 84.32(4) . 2_654 ?
O5 N4 O4 122.40(18) . . ?
O5 N4 O3 118.49(18) . . ?
O4 N4 O3 119.11(17) . . ?
O7 N5 O6 129.9(3) . 5_655 ?
O7 N5 O6 129.9(3) 5_655 . ?
O7 N5 O8 117.8(4) 5_655 . ?
O6 N5 O8 112.3(4) . . ?
O7 N5 O8 117.8(4) . 5_655 ?
O6 N5 O8 112.3(4) 5_655 5_655 ?
O7 O8 O6 102.8(4) . 5_655 ?
O10 N6 O11 116.8(5) . 5_665 ?
O10 N6 N6 116.8(5) . 5_665 ?
O10 N6 O9 129.2(4) . . ?
O11 N6 O9 113.3(5) 5_665 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 959035'
#######################################################################
#
#                 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(OH)2(DPFN))2(k2,k2-PO4)][NO3]5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[(Co2(OH)2(DPFN))2(k2,k2-PO4)][NO3]5'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C60 H44 Co4 F4 N12 O8 P 5+, 5(N O3 1-), C2 H3 N, 7(H2 O)'
_chemical_formula_sum            'C62 H61 Co4 F4 N18 O30 P'
_chemical_formula_weight         1880.96

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'
P P 0.1023 0.0942 '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'
F F 0.0171 0.0103 '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)/m

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

_cell_length_a                   16.5997(17)
_cell_length_b                   12.8750(14)
_cell_length_c                   18.2563(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.203(2)
_cell_angle_gamma                90.00
_cell_volume                     3612.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      26.41

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1900
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5796
_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            50251
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         25.35
_reflns_number_total             6842
_reflns_number_gt                5416
_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          
;
 The nitrate anion consisting of atoms N8 O7 O8 O9 is located on an inversion center and disordered over two symmetry related sites.
 For this reason, O7 O8 O9 have been modeled with structural occupancy factors of 0.5.

 The nitrate anion consisting of atoms N9 O10 O11 O12 O13 is located on a mirror plane through atoms N9 O10 O11 and is disordered
 over two symmetry related sites of consisting of N9 O11 O12 O13_2 and N9 O10 O13 O12_2. Atoms O12 and O13 are modeled with structure
 occupancy factors of 0.5 and the structure occupancy factors of atoms O10 and O11 are refined against each other to a total 
 occupancy of 1.

 The nitrate anion consisting of atoms N10 O14 O15 O16 O17 is located on a mirror plane N10 O14 O15 and is disordered over three sites,
 two of which are symmetry related. The two symmetry related sites consist of N10 O14 O16 O17_2 and N10 O14 O16_2 O17 and are modeled
 with a total occupancy of the nitrate anion of 0.375 for each site. The third position of the nitrate anion consists of atoms N10 O15 
 O17 O17_2 and is modeled with an occupancy of 0.25 for the nitrate anion. Due to disorder, the N10 O15 bond distance is 
 restrained to a chemically appropriate value.

 The nitrate anion consisting of atoms N11 N12 O18 O19 O20 O21 O22 is disordered over two sites of N11 O18 O19 O20 and N12 O18 O21 O22. 
 Each site is modeled as 0.5 occupancy of the nitrate anion. Due to disorder, N11 is restrained isotropically, anisotropic parameters
 for N11 N12 O18 O19 O20 O21 O22 are restrained to be similar, and N11 O18 O19 O20 are restrained to be coplanar. The bonds between N11 O18,
 N11 O19, N12 O21, and N12 O22 are restrained to chemically appropriate values.

 The water solvate molecule sites O26 and O28 were found to have partial occupancy modeled as 0.5 occupancy.

 Hydrogen atoms were modeled at geometrically calculated positions with a constrained riding model except for water solvate hydrogen
 atoms and hydroxo ligand hydrogen atoms which were located from the electron difference map. Water solvate hydrogens were restrained
 to chemically appropriate bond lengths and angles and isotropic parameters were fixed at 1.5 times the isotropic parameter of the 
 parent oxygen atoms. Hydrogen atoms for water solvate molecules O25, O26, O27, and O28 could not be located. Hydrogen atoms of hydroxyl 
 ligands were restrained to bond lengths of chemically appropriate values.

 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)+(0.1385P)²+12.1359P] 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         6842
_refine_ls_number_parameters     691
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0739
_refine_ls_wR_factor_ref         0.2403
_refine_ls_wR_factor_gt          0.2159
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.008
_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 -0.1336(4) 0.2500 0.3870(5) 0.0429(17) Uani 1 2 d S . .
C2 C -0.1832(5) 0.2500 0.4348(5) 0.052(2) Uani 1 2 d S . .
H2 H -0.2449 0.2500 0.4114 0.062 Uiso 1 2 calc SR . .
C3 C -0.1425(6) 0.2500 0.5136(6) 0.056(2) Uani 1 2 d S . .
H3 H -0.1749 0.2500 0.5468 0.067 Uiso 1 2 calc SR . .
C4 C -0.0037(6) 0.2500 0.6308(5) 0.057(2) Uani 1 2 d S . .
H4 H -0.0347 0.2500 0.6652 0.069 Uiso 1 2 calc SR . .
C5 C 0.0848(6) 0.2500 0.6608(5) 0.0503(19) Uani 1 2 d S . .
H5 H 0.1167 0.2500 0.7163 0.060 Uiso 1 2 calc SR . .
C6 C 0.1280(5) 0.2500 0.6078(5) 0.0422(16) Uani 1 2 d S . .
C7 C -0.0032(5) 0.2500 0.4971(5) 0.0416(16) Uani 1 2 d S . .
C8 C -0.0496(5) 0.2500 0.5471(5) 0.0506(19) Uani 1 2 d S . .
C9 C -0.1772(4) 0.2500 0.2970(5) 0.0473(18) Uani 1 2 d S . .
C10 C 0.2271(5) 0.2500 0.6387(4) 0.0419(16) Uani 1 2 d S . .
C11 C -0.1533(3) 0.3484(4) 0.2649(3) 0.0428(12) Uani 1 1 d . . .
C12 C -0.2126(4) 0.4229(5) 0.2230(3) 0.0511(14) Uani 1 1 d . . .
H12 H -0.2728 0.4149 0.2123 0.061 Uiso 1 1 calc R . .
C13 C -0.1821(4) 0.5087(5) 0.1973(4) 0.0555(15) Uani 1 1 d . . .
H13 H -0.2215 0.5614 0.1688 0.067 Uiso 1 1 calc R . .
C14 C -0.0945(4) 0.5192(4) 0.2125(3) 0.0475(13) Uani 1 1 d . . .
H14 H -0.0734 0.5784 0.1943 0.057 Uiso 1 1 calc R . .
C15 C -0.0382(3) 0.4422(4) 0.2546(3) 0.0426(12) Uani 1 1 d . . .
H15 H 0.0224 0.4500 0.2667 0.051 Uiso 1 1 calc R . .
C16 C 0.2590(3) 0.3473(4) 0.6112(3) 0.0418(12) Uani 1 1 d . . .
C17 C 0.3110(4) 0.4212(5) 0.6624(4) 0.0543(14) Uani 1 1 d . . .
H17 H 0.3296 0.4139 0.7181 0.065 Uiso 1 1 calc R . .
C18 C 0.3348(4) 0.5064(5) 0.6288(4) 0.0651(18) Uani 1 1 d . . .
H18 H 0.3705 0.5587 0.6621 0.078 Uiso 1 1 calc R . .
C19 C 0.3077(4) 0.5164(5) 0.5487(4) 0.0576(15) Uani 1 1 d . . .
H19 H 0.3236 0.5755 0.5260 0.069 Uiso 1 1 calc R . .
C20 C 0.2568(3) 0.4389(4) 0.5015(4) 0.0493(13) Uani 1 1 d . . .
H20 H 0.2384 0.4445 0.4456 0.059 Uiso 1 1 calc R . .
C21 C 0.3263(4) 0.4310(10) 0.0933(5) 0.093(3) Uani 1 1 d . . .
C22 C 0.3581(5) 0.4335(14) 0.0319(6) 0.127(6) Uani 1 1 d . . .
H22 H 0.3692 0.4985 0.0129 0.152 Uiso 1 1 calc R . .
C23 C 0.3728(6) 0.3457(15) 0.0000(6) 0.136(6) Uani 1 1 d . . .
H23 H 0.3928 0.3466 -0.0424 0.163 Uiso 1 1 calc R . .
C24 C 0.3572(6) 0.2500 0.0325(7) 0.108(6) Uani 1 2 d S . .
C25 C 0.3243(5) 0.2500 0.0917(6) 0.082(4) Uani 1 2 d S . .
C26 C 0.3076(5) 0.5295(9) 0.1288(5) 0.092(3) Uani 1 1 d . . .
C27 C 0.2097(5) 0.5371(7) 0.1110(4) 0.076(2) Uani 1 1 d . . .
C28 C 0.1581(6) 0.6108(7) 0.0636(5) 0.090(3) Uani 1 1 d . . .
H28 H 0.1802 0.6607 0.0377 0.109 Uiso 1 1 calc R . .
C29 C 0.0707(6) 0.6104(6) 0.0545(5) 0.083(2) Uani 1 1 d . . .
H29 H 0.0327 0.6623 0.0231 0.100 Uiso 1 1 calc R . .
C30 C 0.0395(5) 0.5368(5) 0.0899(4) 0.0622(16) Uani 1 1 d . . .
H30 H -0.0196 0.5379 0.0849 0.075 Uiso 1 1 calc R . .
C31 C 0.0954(4) 0.4600(5) 0.1335(4) 0.0528(14) Uani 1 1 d . . .
H31 H 0.0740 0.4066 0.1572 0.063 Uiso 1 1 calc R . .
C32 C 0.3581(5) 0.5332(9) 0.2186(5) 0.101(3) Uani 1 1 d . . .
C33 C 0.4198(7) 0.6075(11) 0.2557(6) 0.135(5) Uani 1 1 d . . .
H33 H 0.4334 0.6607 0.2262 0.162 Uiso 1 1 calc R . .
C34 C 0.4611(7) 0.6026(11) 0.3368(6) 0.135(5) Uani 1 1 d . . .
H34 H 0.5042 0.6526 0.3637 0.162 Uiso 1 1 calc R . .
C35 C 0.4407(6) 0.5271(10) 0.3783(6) 0.119(4) Uani 1 1 d . . .
H35 H 0.4679 0.5245 0.4343 0.143 Uiso 1 1 calc R . .
C36 C 0.3799(5) 0.4543(8) 0.3375(5) 0.089(3) Uani 1 1 d . . .
H36 H 0.3663 0.3998 0.3661 0.106 Uiso 1 1 calc R . .
N1 N -0.0459(3) 0.2500 0.4160(4) 0.0350(12) Uani 1 2 d S . .
N2 N 0.0879(4) 0.2500 0.5294(4) 0.0374(13) Uani 1 2 d S . .
N3 N -0.0674(3) 0.3563(3) 0.2788(2) 0.0361(9) Uani 1 1 d . . .
N4 N 0.2326(3) 0.3557(3) 0.5324(3) 0.0372(9) Uani 1 1 d . . .
N5 N 0.3096(3) 0.3424(6) 0.1228(3) 0.0683(18) Uani 1 1 d . . .
N6 N 0.1793(3) 0.4601(4) 0.1428(3) 0.0546(13) Uani 1 1 d . . .
N7 N 0.3393(4) 0.4578(5) 0.2592(3) 0.0726(18) Uani 1 1 d . . .
O1 O 0.0889(2) 0.3499(3) 0.39998(19) 0.0338(7) Uani 1 1 d D . .
O2 O 0.0748(3) 0.2500 0.2738(3) 0.0382(11) Uani 1 2 d S . .
O3 O 0.2214(3) 0.2500 0.3987(3) 0.0413(11) Uani 1 2 d S . .
O4 O 0.1781(3) 0.2500 0.1473(3) 0.0444(12) Uani 1 2 d SD . .
O5 O 0.3320(3) 0.2500 0.2602(3) 0.0583(16) Uani 1 2 d SD . .
O6 O 0.2065(2) 0.3516(3) 0.2784(2) 0.0466(9) Uani 1 1 d . . .
P4 P 0.17772(11) 0.2500 0.30693(11) 0.0382(4) Uani 1 2 d S . .
F1 F -0.2663(3) 0.2500 0.2775(3) 0.0559(12) Uani 1 2 d S . .
F2 F 0.2580(3) 0.2500 0.7202(3) 0.0527(11) Uani 1 2 d S . .
F3 F 0.3301(4) 0.6150(6) 0.0959(3) 0.128(2) Uani 1 1 d . . .
Co1 Co 0.00965(5) 0.2500 0.33994(6) 0.0337(3) Uani 1 2 d S . .
Co2 Co 0.15992(6) 0.2500 0.46730(6) 0.0344(3) Uani 1 2 d S . .
Co3 Co 0.25775(4) 0.35404(7) 0.20145(5) 0.0532(3) Uani 1 1 d D . .
H1A H 0.060(5) 0.398(5) 0.415(5) 0.10(3) Uiso 1 1 d D . .
H4A H 0.133(4) 0.2500 0.100(3) 0.07(3) Uiso 1 2 d SD . .
H5A H 0.3906(6) 0.2500 0.282(8) 0.19(8) Uiso 1 2 d SD . .
N8 N 0.0000 0.5000 0.5000 0.0517(17) Uani 1 2 d S . .
O7 O -0.0690(8) 0.5018(8) 0.4426(7) 0.073(3) Uani 0.50 1 d P . 1
O9 O 0.0699(8) 0.5007(10) 0.4845(10) 0.103(5) Uani 0.50 1 d P . 1
O8 O -0.0095(11) 0.4880(10) 0.4318(8) 0.099(4) Uani 0.50 1 d P . 2
N9 N 0.8701(4) 0.7500 0.0574(5) 0.0568(19) Uani 1 2 d S . .
O10 O 0.903(3) 0.7500 0.125(2) 0.056(9) Uani 0.60(16) 2 d SP A 1
O12 O 0.8501(7) 0.6477(8) 0.0332(8) 0.062(3) Uani 0.50 1 d P A 1
O11 O 0.872(10) 0.7500 0.133(3) 0.085(18) Uani 0.40(16) 2 d SP A 2
O13 O 0.8685(7) 0.6910(9) 0.0111(7) 0.060(3) Uani 0.50 1 d P . 2
N10 N 0.5721(9) 0.2500 0.4526(11) 0.107(4) Uani 1 2 d SD . .
O14 O 0.6079(5) 0.2500 0.4006(6) 0.058(2) Uani 0.75 2 d SP B .
O15 O 0.642(4) 0.2500 0.510(4) 0.18(4) Uani 0.25 2 d SPD B 1
O17 O 0.5165(11) 0.3121(11) 0.4417(16) 0.182(9) Uani 0.63 1 d P . 1
O16 O 0.588(3) 0.302(2) 0.5223(15) 0.157(12) Uani 0.38 1 d P . 2
O18 O 0.5193(8) 0.4908(14) 0.1839(6) 0.203(5) Uani 1 1 d DU . .
N11 N 0.5549(15) 0.518(3) 0.1397(15) 0.184(10) Uani 0.50 1 d PDU C 1
O19 O 0.577(3) 0.609(4) 0.145(2) 0.279(18) Uani 0.50 1 d PDU C 1
O20 O 0.5645(14) 0.455(2) 0.0864(16) 0.207(10) Uani 0.50 1 d PDU C 1
N12 N 0.5613(8) 0.4794(14) 0.1519(12) 0.104(7) Uani 0.50 1 d PDU C 2
O21 O 0.6029(11) 0.545(2) 0.1374(10) 0.157(10) Uani 0.50 1 d PDU C 2
O22 O 0.5655(9) 0.3884(17) 0.1643(11) 0.129(6) Uani 0.50 1 d PDU C 2
C37 C 0.6960(7) 0.2500 0.0541(6) 0.070(3) Uani 1 2 d S . .
C38 C 0.6028(7) 0.2500 0.0303(11) 0.115(5) Uani 1 2 d S . .
H38A H 0.5875 0.2237 0.0737 0.172 Uiso 0.50 1 calc PR . .
H38B H 0.5768 0.2054 -0.0162 0.172 Uiso 0.50 1 calc PR . .
H38C H 0.5807 0.3210 0.0171 0.172 Uiso 0.50 1 calc PR . .
N13 N 0.7691(5) 0.2500 0.0749(5) 0.067(2) Uani 1 2 d S . .
O23 O 0.9593(3) 0.2500 0.1101(3) 0.0516(14) Uani 1 2 d SD . .
H23A H 0.999(4) 0.2500 0.160(2) 0.077 Uiso 1 2 d SD . .
H23B H 0.906(3) 0.2500 0.113(5) 0.077 Uiso 1 2 d SD . .
O24 O 0.3988(5) 0.2500 0.5128(5) 0.104(3) Uani 1 2 d SD . .
H24A H 0.439(7) 0.2500 0.490(8) 0.155 Uiso 1 2 d SD . .
H24B H 0.346(4) 0.2500 0.473(6) 0.155 Uiso 1 2 d SD . .
O25 O 0.1765(7) 0.5753(8) 0.3115(6) 0.162(4) Uani 1 1 d . . .
O26 O 0.9147(10) 0.2500 0.7716(9) 0.076(4) Uani 0.50 2 d SP . .
O27 O 0.5263(10) 0.7500 0.1767(16) 0.237(12) Uani 1 2 d S . .
O28 O 0.7276(14) 0.2500 0.6139(13) 0.124(8) Uani 0.50 2 d SP D 2
O29 O 0.4895(5) 0.2500 0.2449(7) 0.124(4) Uani 1 2 d SD . .
H29A H 0.524(10) 0.2500 0.217(9) 0.186 Uiso 1 2 d SD . .
H29B H 0.524(10) 0.2500 0.297(3) 0.186 Uiso 1 2 d SD . .


_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 1.348(9) . ?
C1 C2 1.408(11) . ?
C1 C9 1.525(12) . ?
C2 C3 1.339(13) . ?
C2 H2 0.9500 . ?
C3 C8 1.427(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.361(12) . ?
C4 C8 1.426(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.404(11) . ?
C5 H5 0.9500 . ?
C6 N2 1.330(10) . ?
C6 C10 1.525(10) . ?
C7 N1 1.380(10) . ?
C7 C8 1.399(11) . ?
C7 N2 1.401(9) . ?
C9 F1 1.385(8) . ?
C9 C11 1.510(7) . ?
C9 C11 1.510(7) 4_565 ?
C10 F2 1.378(9) . ?
C10 C16 1.517(7) 4_565 ?
C10 C16 1.517(7) . ?
C11 N3 1.354(6) . ?
C11 C12 1.380(8) . ?
C12 C13 1.369(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(8) . ?
C14 H14 0.9500 . ?
C15 N3 1.347(7) . ?
C15 H15 0.9500 . ?
C16 N4 1.340(7) . ?
C16 C17 1.384(8) . ?
C17 C18 1.384(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.364(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(8) . ?
C19 H19 0.9500 . ?
C20 N4 1.341(7) . ?
C20 H20 0.9500 . ?
C21 N5 1.335(11) . ?
C21 C22 1.408(13) . ?
C21 C26 1.508(15) . ?
C22 C23 1.34(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.432(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(16) . ?
C24 C23 1.432(16) 4_565 ?
C25 N5 1.380(8) . ?
C25 N5 1.380(8) 4_565 ?
C26 F3 1.372(9) . ?
C26 C32 1.535(12) . ?
C26 C27 1.536(11) . ?
C27 N6 1.339(8) . ?
C27 C28 1.350(12) . ?
C28 C29 1.395(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.356(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(9) . ?
C30 H30 0.9500 . ?
C31 N6 1.338(8) . ?
C31 H31 0.9500 . ?
C32 N7 1.327(10) . ?
C32 C33 1.378(12) . ?
C33 C34 1.378(14) . ?
C33 H33 0.9500 . ?
C34 C35 1.351(15) . ?
C34 H34 0.9500 . ?
C35 C36 1.373(12) . ?
C35 H35 0.9500 . ?
C36 N7 1.332(10) . ?
C36 H36 0.9500 . ?
N1 Co1 1.935(6) . ?
N2 Co2 1.933(6) . ?
N3 Co1 1.918(4) . ?
N4 Co2 1.907(4) . ?
N5 Co3 1.938(5) . ?
N6 Co3 1.912(5) . ?
N7 Co3 1.910(6) . ?
O1 Co2 1.860(3) . ?
O1 Co1 1.870(3) . ?
O1 H1A 0.89(2) . ?
O2 P4 1.582(5) . ?
O2 Co1 1.901(5) . ?
O3 P4 1.554(5) . ?
O3 Co2 1.891(5) . ?
O4 Co3 1.880(3) . ?
O4 Co3 1.880(3) 4_565 ?
O4 H4A 0.90(2) . ?
O5 Co3 1.861(4) 4_565 ?
O5 Co3 1.861(4) . ?
O5 H5A 0.901(5) . ?
O6 P4 1.548(4) . ?
O6 Co3 1.899(4) . ?
P4 O6 1.548(4) 4_565 ?
Co1 O1 1.870(3) 4_565 ?
Co1 N3 1.918(4) 4_565 ?
Co1 Co2 2.6917(13) . ?
Co2 O1 1.860(3) 4_565 ?
Co2 N4 1.907(4) 4_565 ?
Co3 Co3 2.6791(19) 4_565 ?
N8 O8 1.204(13) 3_566 ?
N8 O8 1.204(13) . ?
N8 O7 1.226(12) . ?
N8 O7 1.226(12) 3_566 ?
N8 O9 1.294(11) 3_566 ?
N8 O9 1.294(11) . ?
O7 O9 1.337(19) 3_566 ?
O9 O7 1.337(19) 3_566 ?
N9 O13 1.129(11) 4_575 ?
N9 O13 1.129(11) . ?
N9 O10 1.14(4) . ?
N9 O11 1.37(5) . ?
N9 O12 1.389(10) . ?
N9 O12 1.389(10) 4_575 ?
O13 O13 1.52(2) 4_575 ?
N10 O17 1.180(15) 4_565 ?
N10 O17 1.180(15) . ?
N10 O15 1.23(2) . ?
N10 O14 1.296(16) . ?
N10 O16 1.37(3) . ?
N10 O16 1.37(3) 4_565 ?
O17 O17 1.60(3) 4_565 ?
O16 O16 1.35(6) 4_565 ?
O18 N12 1.08(2) . ?
O18 N11 1.219(19) . ?
O18 O22 1.63(2) . ?
N11 O19 1.22(2) . ?
N11 O20 1.32(4) . ?
N12 O21 1.183(19) . ?
N12 O22 1.190(17) . ?
C37 N13 1.127(12) . ?
C37 C38 1.440(15) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O23 H23A 0.90(2) . ?
O23 H23B 0.90(2) . ?
O24 H24A 0.91(2) . ?
O24 H24B 0.90(2) . ?
O29 H29A 0.90(2) . ?
O29 H29B 0.90(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
N1 C1 C2 123.7(7) . . ?
N1 C1 C9 115.1(6) . . ?
C2 C1 C9 121.2(6) . . ?
C3 C2 C1 119.4(7) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C8 119.0(8) . . ?
C2 C3 H3 120.5 . . ?
C8 C3 H3 120.5 . . ?
C5 C4 C8 119.3(8) . . ?
C5 C4 H4 120.3 . . ?
C8 C4 H4 120.3 . . ?
C4 C5 C6 118.5(8) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
N2 C6 C5 124.3(7) . . ?
N2 C6 C10 115.4(7) . . ?
C5 C6 C10 120.3(7) . . ?
N1 C7 C8 121.0(7) . . ?
N1 C7 N2 119.1(7) . . ?
C8 C7 N2 119.9(7) . . ?
C7 C8 C4 119.7(7) . . ?
C7 C8 C3 119.5(8) . . ?
C4 C8 C3 120.8(8) . . ?
F1 C9 C11 108.2(4) . . ?
F1 C9 C11 108.2(4) . 4_565 ?
C11 C9 C11 114.0(6) . 4_565 ?
F1 C9 C1 107.6(6) . . ?
C11 C9 C1 109.3(4) . . ?
C11 C9 C1 109.3(4) 4_565 . ?
F2 C10 C16 108.9(4) . 4_565 ?
F2 C10 C16 108.9(4) . . ?
C16 C10 C16 111.3(6) 4_565 . ?
F2 C10 C6 108.0(6) . . ?
C16 C10 C6 109.9(4) 4_565 . ?
C16 C10 C6 109.9(4) . . ?
N3 C11 C12 122.1(5) . . ?
N3 C11 C9 113.7(5) . . ?
C12 C11 C9 124.1(5) . . ?
C13 C12 C11 118.2(5) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C15 118.8(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
N3 C15 C14 121.3(5) . . ?
N3 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
N4 C16 C17 122.5(5) . . ?
N4 C16 C10 114.1(5) . . ?
C17 C16 C10 123.4(6) . . ?
C18 C17 C16 117.1(6) . . ?
C18 C17 H17 121.5 . . ?
C16 C17 H17 121.5 . . ?
C19 C18 C17 121.1(6) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 118.5(6) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
N4 C20 C19 121.6(6) . . ?
N4 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
N5 C21 C22 122.6(12) . . ?
N5 C21 C26 115.9(7) . . ?
C22 C21 C26 121.5(11) . . ?
C23 C22 C21 120.9(13) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 117.1(9) . . ?
C22 C23 H23 121.4 . . ?
C24 C23 H23 121.4 . . ?
C25 C24 C23 120.7(8) . . ?
C25 C24 C23 120.7(8) . 4_565 ?
C23 C24 C23 118.6(15) . 4_565 ?
N5 C25 N5 119.1(9) . 4_565 ?
N5 C25 C24 120.4(4) . . ?
N5 C25 C24 120.4(4) 4_565 . ?
F3 C26 C21 110.6(8) . . ?
F3 C26 C32 108.3(7) . . ?
C21 C26 C32 111.6(9) . . ?
F3 C26 C27 107.3(8) . . ?
C21 C26 C27 109.6(7) . . ?
C32 C26 C27 109.4(7) . . ?
N6 C27 C28 123.1(7) . . ?
N6 C27 C26 113.7(7) . . ?
C28 C27 C26 123.0(7) . . ?
C27 C28 C29 116.9(7) . . ?
C27 C28 H28 121.6 . . ?
C29 C28 H28 121.6 . . ?
C30 C29 C28 120.9(7) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 118.7(7) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
N6 C31 C30 120.8(6) . . ?
N6 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
N7 C32 C33 121.4(8) . . ?
N7 C32 C26 115.1(6) . . ?
C33 C32 C26 123.5(8) . . ?
C34 C33 C32 118.2(9) . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C35 C34 C33 120.5(9) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 118.4(9) . . ?
C34 C35 H35 120.8 . . ?
C36 C35 H35 120.8 . . ?
N7 C36 C35 121.9(9) . . ?
N7 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C1 N1 C7 117.5(6) . . ?
C1 N1 Co1 117.1(5) . . ?
C7 N1 Co1 125.4(5) . . ?
C6 N2 C7 118.3(7) . . ?
C6 N2 Co2 117.5(5) . . ?
C7 N2 Co2 124.2(5) . . ?
C15 N3 C11 119.0(4) . . ?
C15 N3 Co1 122.2(3) . . ?
C11 N3 Co1 118.6(3) . . ?
C16 N4 C20 119.2(5) . . ?
C16 N4 Co2 119.0(3) . . ?
C20 N4 Co2 121.8(4) . . ?
C21 N5 C25 118.3(7) . . ?
C21 N5 Co3 116.8(7) . . ?
C25 N5 Co3 124.7(6) . . ?
C31 N6 C27 119.3(6) . . ?
C31 N6 Co3 121.8(4) . . ?
C27 N6 Co3 118.9(5) . . ?
C32 N7 C36 119.6(7) . . ?
C32 N7 Co3 118.1(5) . . ?
C36 N7 Co3 122.3(5) . . ?
Co2 O1 Co1 92.37(15) . . ?
Co2 O1 H1A 124(6) . . ?
Co1 O1 H1A 108(6) . . ?
P4 O2 Co1 123.2(3) . . ?
P4 O3 Co2 124.4(3) . . ?
Co3 O4 Co3 90.9(2) . 4_565 ?
Co3 O4 H4A 131.9(19) . . ?
Co3 O4 H4A 131.9(19) 4_565 . ?
Co3 O5 Co3 92.1(2) 4_565 . ?
Co3 O5 H5A 128(4) 4_565 . ?
Co3 O5 H5A 128(4) . . ?
P4 O6 Co3 123.0(2) . . ?
O6 P4 O6 115.3(3) 4_565 . ?
O6 P4 O3 106.54(18) 4_565 . ?
O6 P4 O3 106.54(18) . . ?
O6 P4 O2 107.28(18) 4_565 . ?
O6 P4 O2 107.28(18) . . ?
O3 P4 O2 114.1(3) . . ?
O1 Co1 O1 86.9(2) . 4_565 ?
O1 Co1 O2 85.93(15) . . ?
O1 Co1 O2 85.93(15) 4_565 . ?
O1 Co1 N3 177.48(16) . 4_565 ?
O1 Co1 N3 90.97(16) 4_565 4_565 ?
O2 Co1 N3 92.56(16) . 4_565 ?
O1 Co1 N3 90.97(16) . . ?
O1 Co1 N3 177.48(16) 4_565 . ?
O2 Co1 N3 92.56(16) . . ?
N3 Co1 N3 91.1(2) 4_565 . ?
O1 Co1 N1 90.02(16) . . ?
O1 Co1 N1 90.02(16) 4_565 . ?
O2 Co1 N1 174.4(2) . . ?
N3 Co1 N1 91.34(17) 4_565 . ?
N3 Co1 N1 91.34(17) . . ?
O1 Co1 Co2 43.67(10) . . ?
O1 Co1 Co2 43.67(10) 4_565 . ?
O2 Co1 Co2 89.13(15) . . ?
N3 Co1 Co2 134.38(12) 4_565 . ?
N3 Co1 Co2 134.38(12) . . ?
N1 Co1 Co2 85.29(17) . . ?
O1 Co2 O1 87.5(2) 4_565 . ?
O1 Co2 O3 85.88(15) 4_565 . ?
O1 Co2 O3 85.88(15) . . ?
O1 Co2 N4 177.54(17) 4_565 . ?
O1 Co2 N4 90.69(16) . . ?
O3 Co2 N4 92.31(17) . . ?
O1 Co2 N4 90.69(16) 4_565 4_565 ?
O1 Co2 N4 177.54(17) . 4_565 ?
O3 Co2 N4 92.31(16) . 4_565 ?
N4 Co2 N4 91.0(2) . 4_565 ?
O1 Co2 N2 90.57(16) 4_565 . ?
O1 Co2 N2 90.57(16) . . ?
O3 Co2 N2 175.1(2) . . ?
N4 Co2 N2 91.14(18) . . ?
N4 Co2 N2 91.14(18) 4_565 . ?
O1 Co2 Co1 43.97(10) 4_565 . ?
O1 Co2 Co1 43.97(10) . . ?
O3 Co2 Co1 89.07(15) . . ?
N4 Co2 Co1 134.43(12) . . ?
N4 Co2 Co1 134.43(12) 4_565 . ?
N2 Co2 Co1 86.00(17) . . ?
O5 Co3 O4 88.36(16) . . ?
O5 Co3 O6 86.9(2) . . ?
O4 Co3 O6 87.4(2) . . ?
O5 Co3 N7 90.5(2) . . ?
O4 Co3 N7 178.4(2) . . ?
O6 Co3 N7 91.5(2) . . ?
O5 Co3 N6 178.3(2) . . ?
O4 Co3 N6 91.11(18) . . ?
O6 Co3 N6 91.47(19) . . ?
N7 Co3 N6 90.0(2) . . ?
O5 Co3 N5 89.4(3) . . ?
O4 Co3 N5 88.6(2) . . ?
O6 Co3 N5 174.6(3) . . ?
N7 Co3 N5 92.4(3) . . ?
N6 Co3 N5 92.3(2) . . ?
O5 Co3 Co3 43.97(12) . 4_565 ?
O4 Co3 Co3 44.55(11) . 4_565 ?
O6 Co3 Co3 89.04(12) . 4_565 ?
N7 Co3 Co3 134.4(2) . 4_565 ?
N6 Co3 Co3 135.60(14) . 4_565 ?
N5 Co3 Co3 85.6(2) . 4_565 ?
O8 N8 O8 180.000(3) 3_566 . ?
O8 N8 O7 126.6(8) 3_566 . ?
O8 N8 O7 53.4(7) . . ?
O8 N8 O7 53.4(8) 3_566 3_566 ?
O8 N8 O7 126.6(7) . 3_566 ?
O7 N8 O7 180.000(4) . 3_566 ?
O8 N8 O9 63.5(10) 3_566 3_566 ?
O8 N8 O9 116.5(10) . 3_566 ?
O7 N8 O9 64.0(9) . 3_566 ?
O7 N8 O9 116.0(9) 3_566 3_566 ?
O8 N8 O9 116.5(10) 3_566 . ?
O8 N8 O9 63.5(10) . . ?
O7 N8 O9 116.0(9) . . ?
O7 N8 O9 64.0(9) 3_566 . ?
O9 N8 O9 180.0(14) 3_566 . ?
N8 O7 O9 60.5(7) . 3_566 ?
N8 O9 O7 55.6(7) . 3_566 ?
O13 N9 O10 132.3(13) 4_575 . ?
O13 N9 O10 132.3(13) . . ?
O13 N9 O11 137.7(8) 4_575 . ?
O13 N9 O11 137.7(8) . . ?
O13 N9 O12 117.7(12) 4_575 . ?
O10 N9 O12 107.5(8) . . ?
O11 N9 O12 103.3(17) . . ?
O13 N9 O12 117.7(12) . 4_575 ?
O10 N9 O12 107.5(8) . 4_575 ?
O11 N9 O12 103.3(17) . 4_575 ?
O12 N9 O12 143.0(12) . 4_575 ?
O17 N10 O17 85.3(18) 4_565 . ?
O17 N10 O15 125(3) 4_565 . ?
O17 N10 O15 125(3) . . ?
O17 N10 O14 114.9(16) 4_565 . ?
O17 N10 O14 114.9(16) . . ?
O17 N10 O16 110.9(18) 4_565 . ?
O17 N10 O16 72.0(18) . . ?
O14 N10 O16 134.0(16) . . ?
O17 N10 O16 110.9(18) . 4_565 ?
O14 N10 O16 134.0(16) . 4_565 ?
O18 N11 O19 115(4) . . ?
O18 N11 O20 122(4) . . ?
O19 N11 O20 122(3) . . ?
O18 N12 O21 125.2(16) . . ?
O18 N12 O22 92(2) . . ?
O21 N12 O22 138.4(16) . . ?
N13 C37 C38 178.1(13) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H23A O23 H23B 107(5) . . ?
H24A O24 H24B 106(5) . . ?
H29A O29 H29B 108(5) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.117
_database_code_depnum_ccdc_archive 'CCDC 959036'
