# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_compound_1
#  CIF files read  : tp469_snmo_structure tp469_snmo_absorption

_audit_creation_date             2013-12-18T16:04:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C3.50 H19.70 F4 Fe4 N2 O14.43 P4'
_chemical_formula_weight         744.05

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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                   13.6808(4)
_cell_length_b                   12.6340(2)
_cell_length_c                   12.7830(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.983(4)
_cell_angle_gamma                90
_cell_volume                     1968.94(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9552
_cell_measurement_theta_min      1.6086
_cell_measurement_theta_max      28.1663

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.2309
_exptl_crystal_size_mid          0.0935
_exptl_crystal_size_min          0.052
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_method    flotation
_exptl_crystal_density_meas      2.50(3)
_exptl_crystal_F_000             1482
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 18 1 0.1049
-4 -17 5 0.1009
17 1 0 0.0227
-17 0 0 0.0229
-11 0 18 0.0485
7 0 -18 0.0378
-15 1 -4 0.0262

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.325
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_T_max  0.865

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      0.0291564
_diffrn_orient_matrix_ub_12      0.0019422
_diffrn_orient_matrix_ub_13      0.0621305
_diffrn_orient_matrix_ub_21      0.0501257
_diffrn_orient_matrix_ub_22      -0.0061583
_diffrn_orient_matrix_ub_23      -0.0031591
_diffrn_orient_matrix_ub_31      0.0045189
_diffrn_orient_matrix_ub_32      0.0557762
_diffrn_orient_matrix_ub_33      -0.0025185
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.016
_diffrn_reflns_number            13887
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             3726
_reflns_number_gt                3670
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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.

DFIX 1.30 0.05 H1 P1 H2 P2 H3 P3 H4 P4
DFIX 1.50 0.05 O1' P1 O2' P2 O3' P3
DFIX 51 (2.28682 Å) H1 O1 H1 O3_$6 H1 O18
DFIX 61 (2.27867 Å) H2 O7 H2 O13 H2 O9
DFIX 71 (2.29373 Å) H3 O6 H3 O10 H3 O14   
EADP O1' H1  O2' H2  O3' H3
Partial susbstitutions of the apical hydrogen atoms by oxygen ones were detected
in the P(1), P(2) and P(3) groups, deducing HPO3-HPO4 and HPO3-PO4 disorder
systems from electroneutrality considerations. In order to model correctly the
disorder system, P-H and P-O bonds were restrained to the ideal values (1.30(1)
Å and 1.50(1) Å, respectively). In order to maintain the geometry of the
(HPO3)2- groups, the three distances of the apical hydrogen atom to their
corresponding oxygen atoms forming the pseudotetrahedra base were refined as a
variable. Moreover, the disordered O and H atoms were forced to have equal
isotropic displacement parameters.

ISOR 0.005 0.01 O13 O9
ISOR 0.0025 0.005 O3
O(13), O(9) and O(3) were restrained to behave approximately isotropically
within a standard uncertainty.

DFIX 81 (1.51209 Å) C3 C4 C3 C4_$1 C4 C3_$1
DFIX 1.51 0.02 C1 C2
DFIX 1.49 0.02 N1 C1 N2 C2 N2 C3
In order to maintain the geometry of the organic template, the C-N and C-C bonds
were restrained.

DFIX 0.97 0.02 C3 H3A1 C3 H3A2 C3 H3B1 C3 H3B2
DFIX 1.57 0.02 H3A1 H3B1  H3A2 H3B2
DFIX  2.729 0.01 H3A1 H2C
DFIX  2.460 0.01 H3A1 H2D
DFIX  2.165 0.01 H3B1 H2D
DFIX  2.431 0.01 H3B1 H2C
DFIX  2.104 0.01 H3A2 H2D
DFIX  2.625 0.01 H3A2 H2C
DFIX  2.102 0.01 H3B2 H2C
DFIX  2.535 0.01 H3B2 H2D
DFIX -2.00  0.01 H2B_$1 H4B H2C H4A
Two systems of hydrogens (H3A1-H3B1 and H3A2-H3B2) were fixed geometrically
to its parent C(3) taking into account the symmetry disorder of the C(4) atom
with an occupation factor of 0.5.

DFIX 0.82 0.01 O16W H16B O17W H17A O17W H17B
DANG 1.35 0.02 H17A H17B
Hydrogen atoms related to the coordinated water molecules were first
located and placed in geometrically ideal positions and refined using the riding
mode.
;
_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)+(0.0577P)²+95.4386P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3726
_refine_ls_number_parameters     314
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0867
_refine_ls_wR_factor_ref         0.2069
_refine_ls_wR_factor_gt          0.2067
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.423
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.302

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Fe Fe 0.3463 0.8444 '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 0.006 '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'

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 -0.1508(13) 0.4639(16) 0.1329(15) 0.057(5) Uiso 1 1 d D . .
H1A H -0.1094 0.5156 0.1929 0.068 Uiso 1 1 calc R . .
H1B H -0.1524 0.3983 0.1715 0.068 Uiso 1 1 calc R . .
C2 C -0.2673(11) 0.5038(12) 0.0587(12) 0.038(3) Uiso 1 1 d D . .
H2A H -0.2656 0.5668 0.0161 0.045 Uiso 1 1 calc R . .
H2B H -0.3096 0.4501 0.0018 0.045 Uiso 1 1 calc R . .
C3 C -0.4388(13) 0.5598(14) 0.0775(15) 0.056(5) Uiso 1 1 d D . .
H3A1 H -0.458(2) 0.597(2) 0.005(2) 0.067 Uiso 0.5 1 d PD A 1
H3B1 H -0.4550(15) 0.605(2) 0.129(3) 0.067 Uiso 0.5 1 d PD B 1
H3A2 H -0.4452(15) 0.6338(15) 0.092(6) 0.067 Uiso 0.5 1 d PD C 2
H3B2 H -0.4778(13) 0.519(2) 0.111(4) 0.067 Uiso 0.5 1 d PD D 2
C4 C -0.5043(11) 0.4565(13) 0.0531(17) 0.034(6) Uiso 0.5 1 d PD . -1
H4A H -0.4556 0.3977 0.0913 0.041 Uiso 0.5 1 calc PRD . -1
H4B H -0.5578 0.4611 0.0832 0.041 Uiso 0.5 1 calc PRD . -1
N1 N -0.0971(14) 0.4460(14) 0.0543(15) 0.063(4) Uiso 1 1 d D . .
H1C H -0.1447 0.4605 -0.0196 0.095 Uiso 1 1 calc R . .
H1D H -0.0759 0.3788 0.0596 0.095 Uiso 1 1 calc R . .
H1E H -0.0389 0.4882 0.0765 0.095 Uiso 1 1 calc R . .
N2 N -0.3202(10) 0.5286(13) 0.1343(13) 0.065(4) Uiso 1 1 d D . .
H2D H -0.2819 0.5815 0.1828 0.078 Uiso 1 1 calc RD . .
H2C H -0.3129 0.4715 0.1794 0.078 Uiso 1 1 calc RD . .
F1 F 0.1883(5) 0.0919(4) 0.1268(5) 0.0094(11) Uani 1 1 d . . .
F2 F 0.1671(5) 0.4012(5) 0.1371(5) 0.0121(12) Uani 1 1 d . . .
Fe1 Fe 0.17997(11) 0.24552(11) 0.12799(12) 0.0058(3) Uani 1 1 d . . .
Fe2 Fe 0.69209(11) 0.25117(11) 0.30927(12) 0.0057(3) Uani 1 1 d . . .
Fe3 Fe 0.26008(11) -0.00062(11) 0.04216(12) 0.0059(3) Uani 1 1 d . . .
Fe4 Fe 0.25529(11) 0.49893(11) 0.28870(12) 0.0075(3) Uani 1 1 d . . .
O1 O 0.2012(6) 0.2304(6) 0.2936(6) 0.0130(15) Uani 1 1 d D E .
O3 O 0.1629(6) 0.2620(5) -0.0321(6) 0.0083(14) Uani 1 1 d U . .
O5 O 0.3416(6) 0.2524(6) 0.1879(7) 0.0173(17) Uani 1 1 d . . .
O6 O 0.0199(6) 0.2378(6) 0.0728(7) 0.0152(16) Uani 1 1 d D G .
O7 O 0.3118(7) -0.2667(6) -0.1520(6) 0.0172(17) Uani 1 1 d D . .
O8 O 0.5353(7) 0.2272(8) 0.2403(10) 0.039(3) Uani 1 1 d . . .
O9 O 0.2976(6) -0.2609(6) 0.0339(7) 0.0133(15) Uani 1 1 d DU . .
O10 O -0.1459(6) 0.2299(7) -0.1213(7) 0.025(2) Uani 1 1 d D . .
F3 F 0.3260(5) -0.0973(5) 0.1924(5) 0.0157(13) Uani 1 1 d . . .
F4 F 0.2751(6) 0.5993(5) 0.1792(6) 0.0178(14) Uani 1 1 d . . .
O13 O 0.3234(5) -0.0905(5) -0.0563(6) 0.0061(13) Uani 1 1 d DU . .
O14 O -0.1165(6) 0.0897(6) 0.0360(6) 0.0107(14) Uani 1 1 d D . .
O15 O 0.4054(6) 0.0801(6) 0.1324(7) 0.0136(15) Uani 1 1 d . . .
O16W O 0.4090(6) 0.4326(6) 0.3265(7) 0.0176(16) Uani 1 1 d D . .
O17W O 0.0956(6) 0.5891(6) 0.2337(7) 0.0149(16) Uani 1 1 d D . .
O18 O 0.2032(6) 0.4072(5) 0.3873(6) 0.0100(14) Uani 1 1 d D . .
P1 P 0.1529(2) 0.2957(2) 0.3584(2) 0.0071(5) Uani 1 1 d D . .
P2 P 0.3481(2) -0.2080(2) -0.0381(2) 0.0088(5) Uani 1 1 d D . .
P3 P -0.0644(2) 0.1626(2) -0.0189(2) 0.0112(5) Uani 1 1 d D . .
P4 P 0.4226(2) 0.1983(2) 0.1528(3) 0.0160(6) Uani 1 1 d D . .
O1' O 0.030(3) 0.306(5) 0.269(4) 0.032(18) Uiso 0.17(4) 1 d PD E 2
O2' O 0.468(4) -0.233(10) 0.023(10) 0.05(4) Uiso 0.10(5) 1 d PD F 2
O3' O -0.028(5) 0.105(5) -0.097(5) 0.03(2) Uiso 0.16(4) 1 d PD G 2
H1 H 0.048(4) 0.3080(13) 0.289(3) 0.032(18) Uiso 0.83(4) 1 d PD E 1
H2 H 0.454(4) -0.2185(13) 0.022(3) 0.05(4) Uiso 0.90(5) 1 d PD F 1
H3 H -0.010(2) 0.104(2) -0.060(2) 0.03(2) Uiso 0.84(4) 1 d PD G 1
H4 H 0.404(13) 0.234(12) 0.048(7) 0.039 Uiso 1 1 d D . .
H17B H 0.093(9) 0.601(7) 0.296(5) 0.01(3) Uiso 1 1 d D . .
H17A H 0.119(9) 0.641(5) 0.213(8) 0.01(3) Uiso 1 1 d D . .
H16B H 0.435(9) 0.414(9) 0.283(8) 0.008 Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.508(16) . ?
C1 C2 1.524(15) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N2 1.481(15) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 N2 1.499(15) . ?
C3 C4 1.50(2) 3_465 ?
C3 C4 1.53(2) . ?
C3 H3A1 0.969(18) . ?
C3 H3B1 0.970(19) . ?
C3 H3A2 0.96(2) . ?
C3 H3B2 0.97(2) . ?
C4 C3 1.50(2) 3_465 ?
C4 H3B2 1.03(5) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
N1 H1C 0.89 . ?
N1 H1D 0.89 . ?
N1 H1E 0.89 . ?
N2 H2D 0.9 . ?
N2 H2C 0.9 . ?
F1 Fe1 1.944(6) . ?
F1 Fe3 2.114(6) . ?
F2 Fe1 1.983(6) . ?
F2 Fe4 2.148(6) . ?
Fe1 O3 1.962(7) . ?
Fe1 O6 1.975(7) . ?
Fe1 O5 1.986(7) . ?
Fe1 O1 2.011(7) . ?
Fe2 F3 1.929(6) 2_655 ?
Fe2 O8 1.938(8) . ?
Fe2 O9 1.950(7) 2_655 ?
Fe2 F4 1.960(6) 2_645 ?
Fe2 O10 1.993(8) 4_666 ?
Fe2 O7 1.997(7) 3_655 ?
Fe3 O15 2.060(7) . ?
Fe3 O14 2.084(7) 3 ?
Fe3 F3 2.103(6) . ?
Fe3 O18 2.126(7) 4_565 ?
Fe3 O13 2.148(7) . ?
Fe4 F4 1.996(6) . ?
Fe4 O18 2.062(7) . ?
Fe4 O16W 2.105(7) . ?
Fe4 O13 2.111(7) 4_566 ?
Fe4 O17W 2.274(8) . ?
O1 P1 1.516(7) . ?
O3 P1 1.529(7) 4_565 ?
O5 P4 1.533(8) . ?
O6 P3 1.544(8) . ?
O7 P2 1.503(7) . ?
O7 Fe2 1.997(7) 3_655 ?
O8 P4 1.481(9) . ?
O9 P2 1.533(7) . ?
O9 Fe2 1.950(7) 2_645 ?
O10 P3 1.535(8) . ?
O10 Fe2 1.993(8) 4_465 ?
F3 Fe2 1.929(6) 2_645 ?
F4 Fe2 1.960(6) 2_655 ?
O13 P2 1.517(7) . ?
O13 Fe4 2.111(7) 4_565 ?
O14 P3 1.517(7) . ?
O14 Fe3 2.084(7) 3 ?
O15 P4 1.515(8) . ?
O16W H16B 0.819(10) . ?
O17W H17B 0.821(10) . ?
O17W H17A 0.820(10) . ?
O18 P1 1.539(7) . ?
O18 Fe3 2.126(7) 4_566 ?
P1 O3 1.529(7) 4_566 ?
P1 O1' 1.55(4) . ?
P1 H1 1.31(5) . ?
P2 O2' 1.50(5) . ?
P2 H2 1.31(5) . ?
P3 O3' 1.49(4) . ?
P3 H3 1.31(5) . ?
P4 H4 1.32(5) . ?
O1' H1 0.26(7) . ?
O2' H2 0.26(10) . ?
O3' H3 0.42(6) . ?

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 108.8(13) . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 110.2(12) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 113.8(15) . 3_465 ?
N2 C3 C4 106.2(10) . . ?
C4 C3 C4 72.4(18) 3_465 . ?
N2 C3 H3A1 111.0(18) . . ?
C4 C3 H3A1 39(2) 3_465 . ?
C4 C3 H3A1 110(2) . . ?
N2 C3 H3B1 110.9(15) . . ?
C4 C3 H3B1 132.2(19) 3_465 . ?
C4 C3 H3B1 110(2) . . ?
H3A1 C3 H3B1 108(2) . . ?
N2 C3 H3A2 109.5(15) . . ?
C4 C3 H3A2 107(4) 3_465 . ?
C4 C3 H3A2 140(2) . . ?
H3A1 C3 H3A2 72(5) . . ?
H3B1 C3 H3A2 40(4) . . ?
N2 C3 H3B2 109.6(14) . . ?
C4 C3 H3B2 108(3) 3_465 . ?
C4 C3 H3B2 41(3) . . ?
H3A1 C3 H3B2 136(3) . . ?
H3B1 C3 H3B2 71(3) . . ?
H3A2 C3 H3B2 108(3) . . ?
C3 C4 C3 107.6(18) 3_465 . ?
C3 C4 H3B2 138(2) 3_465 . ?
C3 C4 H3B2 38.7(17) . . ?
C3 C4 H4A 110.2 3_465 . ?
C3 C4 H4A 110.2 . . ?
H3B2 C4 H4A 106.7 . . ?
C3 C4 H4B 110.2 3_465 . ?
C3 C4 H4B 110.2 . . ?
H3B2 C4 H4B 75.6 . . ?
H4A C4 H4B 108.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C2 N2 C3 118.8(14) . . ?
C2 N2 H2D 107.6 . . ?
C3 N2 H2D 107.6 . . ?
C2 N2 H2C 107.6 . . ?
C3 N2 H2C 107.6 . . ?
H2D N2 H2C 107.1 . . ?
Fe1 F1 Fe3 126.8(3) . . ?
Fe1 F2 Fe4 126.5(3) . . ?
F1 Fe1 O3 94.5(3) . . ?
F1 Fe1 O6 90.4(3) . . ?
O3 Fe1 O6 92.6(3) . . ?
F1 Fe1 F2 176.0(2) . . ?
O3 Fe1 F2 89.1(3) . . ?
O6 Fe1 F2 87.5(3) . . ?
F1 Fe1 O5 89.3(3) . . ?
O3 Fe1 O5 89.0(3) . . ?
O6 Fe1 O5 178.4(3) . . ?
F2 Fe1 O5 92.7(3) . . ?
F1 Fe1 O1 86.1(3) . . ?
O3 Fe1 O1 178.5(3) . . ?
O6 Fe1 O1 88.8(3) . . ?
F2 Fe1 O1 90.4(3) . . ?
O5 Fe1 O1 89.7(3) . . ?
F3 Fe2 O8 92.3(4) 2_655 . ?
F3 Fe2 O9 92.2(3) 2_655 2_655 ?
O8 Fe2 O9 90.3(4) . 2_655 ?
F3 Fe2 F4 174.7(3) 2_655 2_645 ?
O8 Fe2 F4 92.9(4) . 2_645 ?
O9 Fe2 F4 86.5(3) 2_655 2_645 ?
F3 Fe2 O10 89.8(3) 2_655 4_666 ?
O8 Fe2 O10 177.8(4) . 4_666 ?
O9 Fe2 O10 90.2(3) 2_655 4_666 ?
F4 Fe2 O10 85.0(3) 2_645 4_666 ?
F3 Fe2 O7 86.9(3) 2_655 3_655 ?
O8 Fe2 O7 92.2(4) . 3_655 ?
O9 Fe2 O7 177.4(3) 2_655 3_655 ?
F4 Fe2 O7 94.1(3) 2_645 3_655 ?
O10 Fe2 O7 87.3(4) 4_666 3_655 ?
O15 Fe3 O14 175.1(3) . 3 ?
O15 Fe3 F3 82.6(3) . . ?
O14 Fe3 F3 92.5(3) 3 . ?
O15 Fe3 F1 89.6(3) . . ?
O14 Fe3 F1 89.3(3) 3 . ?
F3 Fe3 F1 87.7(2) . . ?
O15 Fe3 O18 95.7(3) . 4_565 ?
O14 Fe3 O18 89.2(3) 3 4_565 ?
F3 Fe3 O18 175.6(3) . 4_565 ?
F1 Fe3 O18 96.4(2) . 4_565 ?
O15 Fe3 O13 92.7(3) . . ?
O14 Fe3 O13 88.7(3) 3 . ?
F3 Fe3 O13 96.2(3) . . ?
F1 Fe3 O13 175.7(2) . . ?
O18 Fe3 O13 79.8(3) 4_565 . ?
F4 Fe4 O18 168.5(3) . . ?
F4 Fe4 O16W 88.5(3) . . ?
O18 Fe4 O16W 102.8(3) . . ?
F4 Fe4 O13 99.6(3) . 4_566 ?
O18 Fe4 O13 82.1(3) . 4_566 ?
O16W Fe4 O13 91.9(3) . 4_566 ?
F4 Fe4 F2 86.1(2) . . ?
O18 Fe4 F2 91.2(3) . . ?
O16W Fe4 F2 94.1(3) . . ?
O13 Fe4 F2 171.8(2) 4_566 . ?
F4 Fe4 O17W 83.2(3) . . ?
O18 Fe4 O17W 85.5(3) . . ?
O16W Fe4 O17W 171.7(3) . . ?
O13 Fe4 O17W 88.2(3) 4_566 . ?
F2 Fe4 O17W 86.7(3) . . ?
P1 O1 Fe1 129.3(4) . . ?
P1 O3 Fe1 145.4(4) 4_565 . ?
P4 O5 Fe1 133.9(5) . . ?
P3 O6 Fe1 128.8(4) . . ?
P2 O7 Fe2 140.6(5) . 3_655 ?
P4 O8 Fe2 160.0(7) . . ?
P2 O9 Fe2 137.8(5) . 2_645 ?
P3 O10 Fe2 132.6(5) . 4_465 ?
Fe2 F3 Fe3 124.5(3) 2_645 . ?
Fe2 F4 Fe4 132.0(3) 2_655 . ?
P2 O13 Fe4 130.8(4) . 4_565 ?
P2 O13 Fe3 123.3(4) . . ?
Fe4 O13 Fe3 97.8(3) 4_565 . ?
P3 O14 Fe3 130.1(4) . 3 ?
P4 O15 Fe3 128.3(4) . . ?
Fe4 O16W H16B 131(8) . . ?
Fe4 O17W H17B 104(8) . . ?
Fe4 O17W H17A 93(8) . . ?
H17B O17W H17A 111(3) . . ?
P1 O18 Fe4 127.5(4) . . ?
P1 O18 Fe3 131.9(4) . 4_566 ?
Fe4 O18 Fe3 100.1(3) . 4_566 ?
O1 P1 O3 111.2(4) . 4_566 ?
O1 P1 O18 111.7(4) . . ?
O3 P1 O18 111.8(4) 4_566 . ?
O1 P1 O1' 104(2) . . ?
O3 P1 O1' 109(2) 4_566 . ?
O18 P1 O1' 108(2) . . ?
O1 P1 H1 107.9(7) . . ?
O3 P1 H1 107.2(7) 4_566 . ?
O18 P1 H1 106.7(7) . . ?
O1' P1 H1 4(2) . . ?
O2' P2 O7 102(5) . . ?
O2' P2 O13 113(5) . . ?
O7 P2 O13 112.4(4) . . ?
O2' P2 O9 106(5) . . ?
O7 P2 O9 109.0(4) . . ?
O13 P2 O9 112.9(4) . . ?
O2' P2 H2 7(5) . . ?
O7 P2 H2 108.2(7) . . ?
O13 P2 H2 107.5(7) . . ?
O9 P2 H2 106.5(7) . . ?
O3' P3 O14 112(2) . . ?
O3' P3 O10 92(3) . . ?
O14 P3 O10 114.8(4) . . ?
O3' P3 O6 117(2) . . ?
O14 P3 O6 111.6(4) . . ?
O10 P3 O6 108.1(5) . . ?
O3' P3 H3 16(3) . . ?
O14 P3 H3 108.2(7) . . ?
O10 P3 H3 107.1(7) . . ?
O6 P3 H3 106.7(7) . . ?
O8 P4 O15 113.6(5) . . ?
O8 P4 O5 108.2(5) . . ?
O15 P4 O5 114.4(4) . . ?
O8 P4 H4 109(7) . . ?
O15 P4 H4 103(7) . . ?
O5 P4 H4 108(7) . . ?
P1 O1' H1 19(10) . . ?
P2 O2' H2 38(10) . . ?
P3 O3' H3 57(9) . . ?
_database_code_depnum_ccdc_archive 'CCDC 978254'
#######################################################################
#
#                 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_compound_2
#  CIF files read  : tp944_snmo_structure tp944_snmo_absorption

_audit_creation_date             2013-12-18T15:19:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C3.5 H20 Co1.29 F4 Fe2.71 N2 O14.38 P4'
_chemical_formula_weight         747.53

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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                   13.6823(4)
_cell_length_b                   12.6063(3)
_cell_length_c                   12.7535(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.988(4)
_cell_angle_gamma                90
_cell_volume                     1960.21(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10293
_cell_measurement_theta_min      1.6121
_cell_measurement_theta_max      28.3262

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.2236
_exptl_crystal_size_mid          0.0657
_exptl_crystal_size_min          0.0607
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_density_method    flotation
_exptl_crystal_density_meas      2.51(3)
_exptl_crystal_F_000             1480
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
18 -1 -2 0.0263
14 0 -17 0.0279
-19 0 10 0.0394
-13 0 -6 0.0295
0 -18 -1 0.1181
0 -18 1 0.1208
-7 0 18 0.0378
13 0 6 0.0361
7 0 -18 0.0279
0 18 1 0.1017
-18 0 1 0.0279

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.499
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_T_max  0.839

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      0.0092907
_diffrn_orient_matrix_ub_12      -0.0042054
_diffrn_orient_matrix_ub_13      0.0592737
_diffrn_orient_matrix_ub_21      -0.0574424
_diffrn_orient_matrix_ub_22      -0.0010818
_diffrn_orient_matrix_ub_23      -0.0191922
_diffrn_orient_matrix_ub_31      0.0004347
_diffrn_orient_matrix_ub_32      -0.0560894
_diffrn_orient_matrix_ub_33      -0.0040296
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_number            13695
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             3700
_reflns_number_gt                3537
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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.

DFIX 1.30 0.05 H1 P1 H2 P2 H3 P3 H4 P4
DFIX 1.50 0.05 O1' P1  O2' P2  O3' P3
DFIX 51 (2.29122 Å)  H1 O1 H1 O3_$6 H1 O18
DFIX 61 (2.29110 Å)  H2 O7 H2 O13 H2 O9
DFIX 71 (2.30295 Å)  H3 O6 H3 O10 H3 O14
EADP O1' H1  O2' H2  O3' H3
Partial susbstitutions of the apical hydrogen atoms by oxygen ones were detected
in the P(1), P(2) and P(3) groups, deducing HPO3-HPO4 disorder systems from
electroneutrality considerations. In order to model correctly the disorder
system, P-H and P-O bonds were restrained to the ideal values (1.30(1) Å and
1.50(1) Å, respectively). In order to maintain the geometry of the (HPO3)2-
groups, the three distances of the apical hydrogen atom to their corresponding
oxygen atoms forming the pseudotetrahedra base were refined as a variable.
Moreover, the disordered O and H atoms were forced to have equal isotropic
displacement parameters.

EADP CO3 Fe3
EXYZ CO3 Fe3
ISOR 0.005 0.01 O13
Co(3) and Fe(3) were forced to possess the same coordinates and anisotropic
displacement parameters. O(13) was restrained to behave approximately
isotropically within a standard uncertainty.

DFIX 91 (1.52799 Å)  C3 C4 C3 C4_$1 C4 C3_$1
DFIX 1.51 0.02 C1 C2
DFIX 1.49 0.02 N1 C1 N2 C2 N2 C3
In order to maintain the geometry of the organic template, the C-N and C-C bonds
were restrained.

DFIX 0.97 0.02 C3 H3A1 C3 H3A2 C3 H3B1 C3 H3B2
DFIX 1.57 0.02 H3A1 H3B1  H3A2 H3B2
DFIX  2.706 0.01 H3A1 H2C
DFIX  2.440 0.01 H3A1 H2D
DFIX  2.134 0.01 H3B1 H2D
DFIX  2.407 0.01 H3B1 H2C
DFIX  2.068 0.01 H3A2 H2D
DFIX  2.614 0.01 H3A2 H2C
DFIX  2.064 0.01 H3B2 H2C
DFIX  2.461 0.01 H3B2 H2D
DFIX -2.00  0.01 H2B_$1 H4B H2C H4A
Two systems of hydrogens (H3A1-H3B1 and H3A2-H3B2) were fixed geometrically
to its parent C(3) taking into account the symmetry disorder of the C(4) atom
with an occupation factor of 0.5.

DFIX 0.82 0.01 O17W H17A O17W H17B O16W H16A O16W H16B
DANG 1.35 0.02 H17A H17B H16A H16B
Hydrogen atoms related to the coordinated water molecules were first
located and placed in geometrically ideal positions and refined using the riding
mode.
;
_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)+(0.0072P)²+62.0640P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3700
_refine_ls_number_parameters     317
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1391
_refine_ls_wR_factor_gt          0.1384
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.08
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.218

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
Fe Fe 0.3463 0.8444 '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 0.006 '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'

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 -0.1512(11) 0.4639(13) 0.1316(12) 0.057(4) Uiso 1 1 d D . .
H1A H -0.1086 0.5144 0.1927 0.068 Uiso 1 1 calc R . .
H1B H -0.1537 0.3976 0.169 0.068 Uiso 1 1 calc R . .
C2 C -0.2654(8) 0.5053(10) 0.0605(10) 0.038(3) Uiso 1 1 d D . .
H2A H -0.2625 0.57 0.0208 0.045 Uiso 1 1 calc R . .
H2B H -0.308 0.4536 0.0009 0.045 Uiso 1 1 calc R . .
C3 C -0.4361(11) 0.5606(11) 0.0804(12) 0.056(4) Uiso 1 1 d D . .
H3A1 H -0.455(2) 0.601(3) 0.009(2) 0.068 Uiso 0.5 1 d PD A 1
H3B1 H -0.4513(14) 0.604(2) 0.134(3) 0.068 Uiso 0.5 1 d PD B 1
H3A2 H -0.4390(17) 0.6358(16) 0.092(5) 0.068 Uiso 0.5 1 d PD C 2
H3B2 H -0.4730(11) 0.524(3) 0.119(4) 0.068 Uiso 0.5 1 d PD D 2
C4 C -0.5051(8) 0.4558(10) 0.0510(13) 0.028(4) Uiso 0.5 1 d PD . -1
H4A H -0.4571 0.396 0.0881 0.033 Uiso 0.5 1 calc PRD . -1
H4B H -0.5582 0.4601 0.0817 0.033 Uiso 0.5 1 calc PRD . -1
N1 N -0.0985(6) 0.4463(9) 0.0528(7) 0.059(3) Uiso 1 1 d D . .
H1C H -0.1466 0.4602 -0.0213 0.088 Uiso 1 1 calc R . .
H1D H -0.0765 0.3792 0.0585 0.088 Uiso 1 1 calc R . .
H1E H -0.0409 0.4892 0.0743 0.088 Uiso 1 1 calc R . .
N2 N -0.3203(7) 0.5275(8) 0.1351(8) 0.065(3) Uiso 1 1 d RD . .
H2C H -0.3147 0.4685 0.1772 0.077 Uiso 1 1 calc RD . .
H2D H -0.2812 0.5783 0.1866 0.077 Uiso 1 1 calc RD . .
F1 F 0.1894(4) 0.0912(3) 0.1258(4) 0.0103(9) Uani 1 1 d . . .
F2 F 0.1670(4) 0.4020(3) 0.1389(4) 0.0104(9) Uani 1 1 d . . .
Fe1 Fe 0.18006(9) 0.24542(8) 0.12798(9) 0.0058(2) Uani 1 1 d . . .
Fe2 Fe 0.69238(9) 0.25105(8) 0.30898(9) 0.0059(2) Uani 1 1 d . . .
Co3 Co 0.26061(8) -0.00069(8) 0.04243(9) 0.0052(4) Uani 0.32(12) 1 d P . 1
Fe3 Fe 0.26061(8) -0.00069(8) 0.04243(9) 0.0052(4) Uani 0.68(12) 1 d P . 2
Co4 Co 0.25234(9) 0.49943(8) 0.28919(9) 0.0085(2) Uani 1 1 d . . .
O1 O 0.2030(5) 0.2306(4) 0.2937(5) 0.0115(11) Uani 1 1 d D . .
O3 O 0.1593(5) 0.2642(4) -0.0351(5) 0.0131(12) Uani 1 1 d . . .
O5 O 0.3417(5) 0.2529(5) 0.1869(5) 0.0155(12) Uani 1 1 d . . .
O6 O 0.0195(4) 0.2373(5) 0.0731(5) 0.0127(12) Uani 1 1 d D . .
O7 O 0.3125(6) -0.2679(5) -0.1522(5) 0.0192(14) Uani 1 1 d D . .
O8 O 0.5360(5) 0.2264(6) 0.2414(7) 0.0334(19) Uani 1 1 d . . .
O9 O 0.2940(6) -0.2627(5) 0.0308(5) 0.0187(13) Uani 1 1 d D . .
O10 O -0.1452(5) 0.2292(5) -0.1222(6) 0.0221(15) Uani 1 1 d D . .
F3 F 0.3249(4) -0.0971(4) 0.1906(4) 0.0158(10) Uani 1 1 d . . .
F4 F 0.2757(4) 0.5996(4) 0.1816(4) 0.0153(10) Uani 1 1 d . . .
O13 O 0.3210(4) -0.0906(4) -0.0567(5) 0.0065(10) Uani 1 1 d DU . .
O14 O -0.1180(4) 0.0896(4) 0.0355(5) 0.0100(11) Uani 1 1 d D . .
O15 O 0.4057(5) 0.0804(4) 0.1330(5) 0.0131(12) Uani 1 1 d . . .
O16W O 0.4040(5) 0.4312(5) 0.3285(6) 0.0175(13) Uani 1 1 d D . .
O17W O 0.0971(5) 0.5879(5) 0.2361(5) 0.0128(12) Uani 1 1 d D . .
O18 O 0.2033(4) 0.4061(4) 0.3889(5) 0.0096(11) Uani 1 1 d D . .
P1 P 0.15311(16) 0.29538(15) 0.35831(17) 0.0071(4) Uani 1 1 d D . .
P2 P 0.34674(17) -0.20851(15) -0.03787(17) 0.0088(4) Uani 1 1 d D . .
P3 P -0.06439(16) 0.16221(16) -0.01901(17) 0.0091(4) Uani 1 1 d D . .
P4 P 0.42255(17) 0.19829(17) 0.15185(19) 0.0124(4) Uani 1 1 d D . .
O1' O 0.027(3) 0.306(3) 0.267(3) 0.021(13) Uiso 0.15(3) 1 d PD . 1
O2' O 0.469(4) -0.225(6) 0.025(6) 0.02(2) Uiso 0.08(3) 1 d PD . 1
O3' O -0.025(4) 0.103(4) -0.096(4) 0.030(17) Uiso 0.15(3) 1 d PD . 1
H1 H 0.048(4) 0.3080(13) 0.285(3) 0.021(13) Uiso 0.85(3) 1 d PD . 2
H2 H 0.454(4) -0.2183(12) 0.025(3) 0.02(2) Uiso 0.92(3) 1 d PD . 2
H3 H -0.010(2) 0.102(2) -0.059(2) 0.030(17) Uiso 0.85(3) 1 d PD . 2
H17B H 0.099(9) 0.596(6) 0.301(4) 0.02(3) Uiso 1 1 d D . .
H17A H 0.091(8) 0.645(3) 0.203(7) 0.02(3) Uiso 1 1 d D . .
H4 H 0.408(8) 0.233(8) 0.049(5) 0.021 Uiso 1 1 d D . .
H16A H 0.458(7) 0.464(9) 0.334(11) 0.05(4) Uiso 1 1 d D . .
H16B H 0.375(11) 0.398(12) 0.267(8) 0.09(6) Uiso 1 1 d D . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.496(13) . ?
C1 C2 1.500(13) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 N2 1.481(11) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 N2 1.473(13) . ?
C3 C4 1.508(16) 3_465 ?
C3 C4 1.567(16) . ?
C3 H3A1 0.967(18) . ?
C3 H3B1 0.971(19) . ?
C3 H3A2 0.96(2) . ?
C3 H3B2 0.97(2) . ?
C4 C3 1.508(16) 3_465 ?
C4 H3B2 1.16(5) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
N1 H1C 0.89 . ?
N1 H1D 0.89 . ?
N1 H1E 0.89 . ?
N2 H2C 0.9 . ?
N2 H2D 0.9 . ?
F1 Fe1 1.949(4) . ?
F1 Co3 2.089(5) . ?
F2 Fe1 1.992(5) . ?
F2 Co4 2.125(4) . ?
Fe1 O3 1.981(6) . ?
Fe1 O6 1.983(6) . ?
Fe1 O5 1.989(6) . ?
Fe1 O1 2.000(5) . ?
Fe2 F3 1.929(5) 2_655 ?
Fe2 O8 1.935(6) . ?
Fe2 F4 1.950(5) 2_645 ?
Fe2 O9 1.974(6) 2_655 ?
Fe2 O7 1.982(6) 3_655 ?
Fe2 O10 2.000(6) 4_666 ?
Co3 O15 2.059(6) . ?
Co3 O14 2.072(5) 3 ?
Co3 F3 2.077(5) . ?
Co3 O18 2.116(5) 4_565 ?
Co3 O13 2.125(5) . ?
Co4 F4 1.995(5) . ?
Co4 O18 2.056(5) . ?
Co4 O16W 2.086(6) . ?
Co4 O13 2.095(5) 4_566 ?
Co4 O17W 2.215(6) . ?
O1 P1 1.523(6) . ?
O3 P1 1.522(5) 4_565 ?
O5 P4 1.532(6) . ?
O6 P3 1.540(6) . ?
O7 P2 1.512(6) . ?
O7 Fe2 1.982(6) 3_655 ?
O8 P4 1.493(7) . ?
O9 P2 1.526(6) . ?
O9 Fe2 1.974(6) 2_645 ?
O10 P3 1.532(6) . ?
O10 Fe2 2.000(6) 4_465 ?
F3 Fe2 1.929(5) 2_645 ?
F4 Fe2 1.950(5) 2_655 ?
O13 P2 1.521(5) . ?
O13 Co4 2.095(5) 4_565 ?
O14 P3 1.524(6) . ?
O14 Fe3 2.072(5) 3 ?
O14 Co3 2.072(5) 3 ?
O15 P4 1.506(6) . ?
O16W H16A 0.820(10) . ?
O16W H16B 0.820(10) . ?
O17W H17B 0.820(10) . ?
O17W H17A 0.820(10) . ?
O18 P1 1.526(6) . ?
O18 Fe3 2.116(5) 4_566 ?
O18 Co3 2.116(5) 4_566 ?
P1 O3 1.522(5) 4_566 ?
P1 O1' 1.59(3) . ?
P1 H1 1.32(5) . ?
P2 O2' 1.50(4) . ?
P2 H2 1.32(5) . ?
P3 O3' 1.51(4) . ?
P3 H3 1.32(5) . ?
P4 H4 1.31(5) . ?
O1' H1 0.27(6) . ?
O2' H2 0.22(7) . ?
O3' H3 0.41(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 109.5(10) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 111.7(9) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 C4 113.8(11) . 3_465 ?
N2 C3 C4 106.0(8) . . ?
C4 C3 C4 70.1(13) 3_465 . ?
N2 C3 H3A1 111.2(18) . . ?
C4 C3 H3A1 41(2) 3_465 . ?
C4 C3 H3A1 110(2) . . ?
N2 C3 H3B1 110.8(14) . . ?
C4 C3 H3B1 133.1(17) 3_465 . ?
C4 C3 H3B1 110(2) . . ?
H3A1 C3 H3B1 108(2) . . ?
N2 C3 H3A2 108.4(16) . . ?
C4 C3 H3A2 106(3) 3_465 . ?
C4 C3 H3A2 143(2) . . ?
H3A1 C3 H3A2 68(5) . . ?
H3B1 C3 H3A2 45(4) . . ?
N2 C3 H3B2 108.6(13) . . ?
C4 C3 H3B2 111(3) 3_465 . ?
C4 C3 H3B2 47(3) . . ?
H3A1 C3 H3B2 139(3) . . ?
H3B1 C3 H3B2 65(3) . . ?
H3A2 C3 H3B2 109(3) . . ?
C3 C4 C3 109.9(13) 3_465 . ?
C3 C4 H3B2 140.1(18) 3_465 . ?
C3 C4 H3B2 38.2(12) . . ?
C3 C4 H4A 109.7 3_465 . ?
C3 C4 H4A 109.7 . . ?
H3B2 C4 H4A 105.4 . . ?
C3 C4 H4B 109.7 3_465 . ?
C3 C4 H4B 109.7 . . ?
H3B2 C4 H4B 75.7 . . ?
H4A C4 H4B 108.2 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C3 N2 C2 119.9(9) . . ?
C3 N2 H2C 107.3 . . ?
C2 N2 H2C 107.3 . . ?
C3 N2 H2D 107.3 . . ?
C2 N2 H2D 107.3 . . ?
H2C N2 H2D 106.9 . . ?
Fe1 F1 Co3 127.5(2) . . ?
Fe1 F2 Co4 127.3(2) . . ?
F1 Fe1 O3 94.8(2) . . ?
F1 Fe1 O6 90.8(2) . . ?
O3 Fe1 O6 91.6(2) . . ?
F1 Fe1 O5 89.1(2) . . ?
O3 Fe1 O5 89.8(3) . . ?
O6 Fe1 O5 178.6(2) . . ?
F1 Fe1 F2 175.97(19) . . ?
O3 Fe1 F2 88.9(2) . . ?
O6 Fe1 F2 87.4(2) . . ?
O5 Fe1 F2 92.7(2) . . ?
F1 Fe1 O1 86.7(2) . . ?
O3 Fe1 O1 178.4(2) . . ?
O6 Fe1 O1 89.1(2) . . ?
O5 Fe1 O1 89.5(2) . . ?
F2 Fe1 O1 89.7(2) . . ?
F3 Fe2 O8 92.8(3) 2_655 . ?
F3 Fe2 F4 174.7(2) 2_655 2_645 ?
O8 Fe2 F4 92.4(3) . 2_645 ?
F3 Fe2 O9 92.2(2) 2_655 2_655 ?
O8 Fe2 O9 90.7(3) . 2_655 ?
F4 Fe2 O9 86.4(2) 2_645 2_655 ?
F3 Fe2 O7 87.0(2) 2_655 3_655 ?
O8 Fe2 O7 92.5(3) . 3_655 ?
F4 Fe2 O7 94.1(2) 2_645 3_655 ?
O9 Fe2 O7 176.7(3) 2_655 3_655 ?
F3 Fe2 O10 89.3(2) 2_655 4_666 ?
O8 Fe2 O10 177.9(3) . 4_666 ?
F4 Fe2 O10 85.5(2) 2_645 4_666 ?
O9 Fe2 O10 89.6(3) 2_655 4_666 ?
O7 Fe2 O10 87.2(3) 3_655 4_666 ?
O15 Co3 O14 175.1(2) . 3 ?
O15 Co3 F3 83.0(2) . . ?
O14 Co3 F3 92.2(2) 3 . ?
O15 Co3 F1 89.6(2) . . ?
O14 Co3 F1 89.4(2) 3 . ?
F3 Co3 F1 87.95(19) . . ?
O15 Co3 O18 95.6(2) . 4_565 ?
O14 Co3 O18 89.3(2) 3 4_565 ?
F3 Co3 O18 176.2(2) . 4_565 ?
F1 Co3 O18 95.51(19) . 4_565 ?
O15 Co3 O13 93.6(2) . . ?
O14 Co3 O13 87.8(2) 3 . ?
F3 Co3 O13 96.4(2) . . ?
F1 Co3 O13 174.95(19) . . ?
O18 Co3 O13 80.2(2) 4_565 . ?
F4 Co4 O18 170.8(2) . . ?
F4 Co4 O16W 88.5(2) . . ?
O18 Co4 O16W 100.6(2) . . ?
F4 Co4 O13 98.9(2) . 4_566 ?
O18 Co4 O13 82.4(2) . 4_566 ?
O16W Co4 O13 91.5(2) . 4_566 ?
F4 Co4 F2 86.52(18) . . ?
O18 Co4 F2 91.56(19) . . ?
O16W Co4 F2 93.3(2) . . ?
O13 Co4 F2 172.82(19) 4_566 . ?
F4 Co4 O17W 84.4(2) . . ?
O18 Co4 O17W 86.6(2) . . ?
O16W Co4 O17W 172.8(2) . . ?
O13 Co4 O17W 88.3(2) 4_566 . ?
F2 Co4 O17W 87.5(2) . . ?
P1 O1 Fe1 128.8(3) . . ?
P1 O3 Fe1 143.3(4) 4_565 . ?
P4 O5 Fe1 134.0(4) . . ?
P3 O6 Fe1 128.6(3) . . ?
P2 O7 Fe2 140.6(4) . 3_655 ?
P4 O8 Fe2 159.1(5) . . ?
P2 O9 Fe2 135.1(4) . 2_645 ?
P3 O10 Fe2 132.1(4) . 4_465 ?
Fe2 F3 Co3 125.6(2) 2_645 . ?
Fe2 F4 Co4 132.7(2) 2_655 . ?
P2 O13 Co4 131.1(3) . 4_565 ?
P2 O13 Co3 123.5(3) . . ?
Co4 O13 Co3 97.8(2) 4_565 . ?
P3 O14 Fe3 130.5(3) . 3 ?
P3 O14 Co3 130.5(3) . 3 ?
Fe3 O14 Co3 0.00(10) 3 3 ?
P4 O15 Co3 128.2(3) . . ?
Co4 O16W H16A 124(10) . . ?
Co4 O16W H16B 90(10) . . ?
H16A O16W H16B 111(3) . . ?
Co4 O17W H17B 100(7) . . ?
Co4 O17W H17A 118(7) . . ?
H17B O17W H17A 111(3) . . ?
P1 O18 Co4 126.9(3) . . ?
P1 O18 Fe3 133.4(3) . 4_566 ?
Co4 O18 Fe3 99.3(2) . 4_566 ?
P1 O18 Co3 133.4(3) . 4_566 ?
Co4 O18 Co3 99.3(2) . 4_566 ?
Fe3 O18 Co3 0.00(6) 4_566 4_566 ?
O3 P1 O1 111.2(3) 4_566 . ?
O3 P1 O18 112.8(3) 4_566 . ?
O1 P1 O18 111.6(3) . . ?
O3 P1 O1' 107.3(15) 4_566 . ?
O1 P1 O1' 104.8(15) . . ?
O18 P1 O1' 108.7(16) . . ?
O3 P1 H1 107.1(7) 4_566 . ?
O1 P1 H1 107.0(7) . . ?
O18 P1 H1 106.9(6) . . ?
O1' P1 H1 2.3(17) . . ?
O2' P2 O7 103(3) . . ?
O2' P2 O13 110(3) . . ?
O7 P2 O13 112.5(3) . . ?
O2' P2 O9 109(3) . . ?
O7 P2 O9 108.1(3) . . ?
O13 P2 O9 113.1(3) . . ?
O2' P2 H2 5(3) . . ?
O7 P2 H2 108.0(7) . . ?
O13 P2 H2 107.5(7) . . ?
O9 P2 H2 107.2(7) . . ?
O3' P3 O14 112.7(19) . . ?
O3' P3 O10 92.8(19) . . ?
O14 P3 O10 114.4(3) . . ?
O3' P3 O6 115.8(19) . . ?
O14 P3 O6 111.6(3) . . ?
O10 P3 O6 108.3(4) . . ?
O3' P3 H3 15(2) . . ?
O14 P3 H3 107.9(6) . . ?
O10 P3 H3 107.4(7) . . ?
O6 P3 H3 107.0(7) . . ?
O8 P4 O15 112.8(4) . . ?
O8 P4 O5 107.9(4) . . ?
O15 P4 O5 114.3(3) . . ?
O8 P4 H4 109(4) . . ?
O15 P4 H4 103(5) . . ?
O5 P4 H4 110(4) . . ?
P1 O1' H1 11(9) . . ?
P2 O2' H2 30(10) . . ?
P3 O3' H3 55(8) . . ?

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 978255'
