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

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#                 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.
#
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#  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
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#  data retrieval see:
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data_1-150K



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C22.50 H30.50 Ag2 Fe N8.50 O3'

_chemical_formula_weight         739.64



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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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                   16.2400(7)

_cell_length_b                   13.6625(5)

_cell_length_c                   14.8867(7)

_cell_angle_alpha                90.00

_cell_angle_beta                 111.728(5)

_cell_angle_gamma                90.00

_cell_volume                     3068.4(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    150(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.42

_exptl_crystal_size_mid          0.32

_exptl_crystal_size_min          0.25

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.601

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1476

_exptl_absorpt_coefficient_mu    14.187

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.0660

_exptl_absorpt_correction_T_max  0.1256

_exptl_absorpt_process_details   ?



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      150(2)

_diffrn_radiation_wavelength     1.54178

_diffrn_radiation_type           CuK\a

_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'

_diffrn_radiation_monochromator  mirror

_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean 16.0855

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            4984

_diffrn_reflns_av_R_equivalents  0.0305

_diffrn_reflns_av_sigmaI/netI    0.0381

_diffrn_reflns_limit_h_min       -15

_diffrn_reflns_limit_h_max       18

_diffrn_reflns_limit_k_min       -15

_diffrn_reflns_limit_k_max       14

_diffrn_reflns_limit_l_min       -16

_diffrn_reflns_limit_l_max       16

_diffrn_reflns_theta_min         4.37

_diffrn_reflns_theta_max         61.00

_reflns_number_total             2307

_reflns_number_gt                2099

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_refine_special_details          
; 

 'SADI N4 C9 N4 C10 N4 C9' N4 C10'' is executed. Since the piperazine ring

 is disordered over two sites, relevant bonds are essentially equal.



 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)+(0.0532P)²+21.6292P] 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         2307

_refine_ls_number_parameters     198

_refine_ls_number_restraints     6

_refine_ls_R_factor_all          0.0484

_refine_ls_R_factor_gt           0.0448

_refine_ls_wR_factor_ref         0.1162

_refine_ls_wR_factor_gt          0.1139

_refine_ls_goodness_of_fit_ref   1.075

_refine_ls_restrained_S_all      1.125

_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








































Ag1 Ag 0.77183(3) 0.53318(4) 0.28586(3) 0.0489(2) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.2500 0.5000 0.0204(3) Uani 1 2 d S . .
N1 N 0.7597(3) 0.3642(3) 0.4282(3) 0.0287(10) Uani 1 1 d . . .
N2 N 0.7725(3) 0.6718(3) 0.1144(3) 0.0289(10) Uani 1 1 d . . .
N3 N 0.6198(3) 0.2746(3) 0.4624(3) 0.0267(10) Uani 1 1 d . . .
N4 N 0.3058(3) 0.2840(5) 0.4523(5) 0.066(2) Uani 1 1 d D . .
C1 C 0.7658(4) 0.4280(5) 0.3820(4) 0.0388(14) Uani 1 1 d . . .
C2 C 0.7793(4) 0.6242(5) 0.1805(4) 0.0406(15) Uani 1 1 d . . .
C3 C 0.5567(7) 0.2094(9) 0.4267(8) 0.029(3) Uani 0.469(8) 1 d P A 1
H3A H 0.5749 0.1452 0.4179 0.034 Uiso 0.469(8) 1 calc PR A 1
C4 C 0.4665(7) 0.2239(10) 0.4005(9) 0.033(3) Uani 0.469(8) 1 d P A 1
H4A H 0.4260 0.1720 0.3732 0.040 Uiso 0.469(8) 1 calc PR A 1
C5 C 0.5884(8) 0.3678(9) 0.4743(10) 0.038(3) Uani 0.469(8) 1 d P A 1
H5A H 0.6302 0.4188 0.5007 0.046 Uiso 0.469(8) 1 calc PR A 1
C6 C 0.4982(8) 0.3888(10) 0.4488(12) 0.046(4) Uani 0.469(8) 1 d P A 1
H6A H 0.4782 0.4529 0.4547 0.056 Uiso 0.469(8) 1 calc PR A 1
C3' C 0.5855(7) 0.2661(9) 0.5302(8) 0.039(3) Uani 0.531(8) 1 d P A 2
H3B H 0.6229 0.2487 0.5941 0.047 Uiso 0.531(8) 1 calc PR A 2
C4' C 0.4962(8) 0.2820(10) 0.5097(9) 0.046(3) Uani 0.531(8) 1 d P A 2
H4B H 0.4731 0.2746 0.5593 0.055 Uiso 0.531(8) 1 calc PR A 2
C5' C 0.5677(7) 0.2870(9) 0.3700(9) 0.040(3) Uani 0.531(8) 1 d P A 2
H5B H 0.5928 0.2848 0.3216 0.048 Uiso 0.531(8) 1 calc PR A 2
C6' C 0.4771(7) 0.3032(10) 0.3433(8) 0.042(3) Uani 0.531(8) 1 d P A 2
H6B H 0.4410 0.3100 0.2768 0.050 Uiso 0.531(8) 1 calc PR A 2
C7 C 0.4380(4) 0.3097(5) 0.4138(4) 0.0411(15) Uani 1 1 d . . .
C8 C 0.3411(4) 0.3311(6) 0.3885(5) 0.0467(17) Uani 1 1 d . A .
H8A H 0.3328 0.4027 0.3909 0.056 Uiso 1 1 calc R . .
H8B H 0.3077 0.3090 0.3215 0.056 Uiso 1 1 calc R . .
C9 C 0.2970(7) 0.1851(9) 0.4609(9) 0.041(4) Uani 0.508(13) 1 d PD . 1
H9A H 0.3544 0.1534 0.4705 0.050 Uiso 0.508(13) 1 calc PR . 1
H9B H 0.2528 0.1600 0.3996 0.050 Uiso 0.508(13) 1 calc PR . 1
C10 C 0.2313(8) 0.3440(10) 0.4573(10) 0.043(4) Uani 0.508(13) 1 d PD . 1
H10A H 0.1800 0.3376 0.3955 0.052 Uiso 0.508(13) 1 calc PR . 1
H10B H 0.2493 0.4137 0.4651 0.052 Uiso 0.508(13) 1 calc PR . 1
C9' C 0.3353(7) 0.2950(12) 0.5480(8) 0.047(4) Uani 0.492(13) 1 d PD . 2
H9C H 0.3223 0.3625 0.5631 0.057 Uiso 0.492(13) 1 calc PR . 2
H9D H 0.4005 0.2864 0.5748 0.057 Uiso 0.492(13) 1 calc PR . 2
C10' C 0.2063(7) 0.2775(14) 0.4034(10) 0.052(5) Uani 0.492(13) 1 d PD . 2
H10C H 0.1912 0.2577 0.3352 0.062 Uiso 0.492(13) 1 calc PR . 2
H10D H 0.1804 0.3431 0.4035 0.062 Uiso 0.492(13) 1 calc PR . 2






_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



















































Ag1 C2 2.040(6) . ?
Ag1 C1 2.055(6) . ?
Fe1 N2 1.928(5) 4_645 ?
Fe1 N2 1.928(5) 6_566 ?
Fe1 N1 1.930(5) 7_656 ?
Fe1 N1 1.930(5) . ?
Fe1 N3 2.005(4) 7_656 ?
Fe1 N3 2.005(4) . ?
N1 C1 1.139(8) . ?
N2 C2 1.150(8) . ?
N2 Fe1 1.928(5) 4_655 ?
N3 C3 1.313(13) . ?
N3 C3' 1.327(13) . ?
N3 C5' 1.331(12) . ?
N3 C5 1.408(13) . ?
N4 C9' 1.332(12) . ?
N4 C9 1.369(12) . ?
N4 C8 1.431(9) . ?
N4 C10 1.487(11) . ?
N4 C10' 1.510(11) . ?
C3 C4 1.383(16) . ?
C3 H3A 0.9500 . ?
C4 C7 1.303(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.400(17) . ?
C5 H5A 0.9500 . ?
C6 C7 1.421(16) . ?
C6 H6A 0.9500 . ?
C3' C4' 1.384(16) . ?
C3' H3B 0.9500 . ?
C4' C7 1.441(14) . ?
C4' H4B 0.9500 . ?
C5' C6' 1.392(16) . ?
C5' H5B 0.9500 . ?
C6' C7 1.416(14) . ?
C6' H6B 0.9500 . ?
C7 C8 1.504(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.505(18) 7_556 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C9 1.505(18) 7_556 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C9' C10' 1.525(19) 7_556 ?
C9' H9C 0.9900 . ?
C9' H9D 0.9900 . ?
C10' C9' 1.525(19) 7_556 ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag








































































































C2 Ag1 C1 173.2(3) . . ?
N2 Fe1 N2 180.000(1) 4_645 6_566 ?
N2 Fe1 N1 90.77(19) 4_645 7_656 ?
N2 Fe1 N1 89.23(19) 6_566 7_656 ?
N2 Fe1 N1 89.23(19) 4_645 . ?
N2 Fe1 N1 90.77(19) 6_566 . ?
N1 Fe1 N1 180.000(1) 7_656 . ?
N2 Fe1 N3 89.38(18) 4_645 7_656 ?
N2 Fe1 N3 90.62(18) 6_566 7_656 ?
N1 Fe1 N3 90.19(18) 7_656 7_656 ?
N1 Fe1 N3 89.81(18) . 7_656 ?
N2 Fe1 N3 90.62(18) 4_645 . ?
N2 Fe1 N3 89.38(18) 6_566 . ?
N1 Fe1 N3 89.81(18) 7_656 . ?
N1 Fe1 N3 90.19(18) . . ?
N3 Fe1 N3 180.0(3) 7_656 . ?
C1 N1 Fe1 176.0(5) . . ?
C2 N2 Fe1 175.0(5) . 4_655 ?
C3 N3 C3' 76.3(7) . . ?
C3 N3 C5' 64.3(8) . . ?
C3' N3 C5' 120.7(8) . . ?
C3 N3 C5 113.6(8) . . ?
C3' N3 C5 73.1(8) . . ?
C5' N3 C5 83.8(8) . . ?
C3 N3 Fe1 125.8(6) . . ?
C3' N3 Fe1 118.0(5) . . ?
C5' N3 Fe1 120.8(6) . . ?
C5 N3 Fe1 120.7(6) . . ?
C9' N4 C9 91.2(9) . . ?
C9' N4 C8 125.8(8) . . ?
C9 N4 C8 125.9(8) . . ?
C9' N4 C10 82.1(9) . . ?
C9 N4 C10 115.1(8) . . ?
C8 N4 C10 108.6(7) . . ?
C9' N4 C10' 114.8(9) . . ?
C9 N4 C10' 81.8(9) . . ?
C8 N4 C10' 109.1(7) . . ?
C10 N4 C10' 46.4(8) . . ?
N1 C1 Ag1 173.8(5) . . ?
N2 C2 Ag1 171.2(5) . . ?
N3 C3 C4 127.2(11) . . ?
N3 C3 H3A 116.4 . . ?
C4 C3 H3A 116.4 . . ?
C7 C4 C3 119.0(11) . . ?
C7 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C6 C5 N3 122.9(11) . . ?
C6 C5 H5A 118.6 . . ?
N3 C5 H5A 118.6 . . ?
C5 C6 C7 117.0(11) . . ?
C5 C6 H6A 121.5 . . ?
C7 C6 H6A 121.5 . . ?
N3 C3' C4' 121.3(10) . . ?
N3 C3' H3B 119.3 . . ?
C4' C3' H3B 119.3 . . ?
C3' C4' C7 120.6(11) . . ?
C3' C4' H4B 119.7 . . ?
C7 C4' H4B 119.7 . . ?
N3 C5' C6' 121.1(10) . . ?
N3 C5' H5B 119.5 . . ?
C6' C5' H5B 119.5 . . ?
C5' C6' C7 121.0(10) . . ?
C5' C6' H6B 119.5 . . ?
C7 C6' H6B 119.5 . . ?
C4 C7 C6' 63.2(8) . . ?
C4 C7 C6 120.3(8) . . ?
C6' C7 C6 83.3(9) . . ?
C4 C7 C4' 76.9(8) . . ?
C6' C7 C4' 114.0(8) . . ?
C6 C7 C4' 74.1(9) . . ?
C4 C7 C8 122.3(8) . . ?
C6' C7 C8 122.8(6) . . ?
C6 C7 C8 117.3(7) . . ?
C4' C7 C8 122.7(7) . . ?
N4 C8 C7 112.7(5) . . ?
N4 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N4 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N4 C9 C10 114.3(9) . 7_556 ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 7_556 . ?
N4 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 7_556 . ?
H9A C9 H9B 107.6 . . ?
N4 C10 C9 113.1(9) . 7_556 ?
N4 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 7_556 . ?
N4 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 7_556 . ?
H10A C10 H10B 107.8 . . ?
N4 C9' C10' 112.7(11) . 7_556 ?
N4 C9' H9C 109.0 . . ?
C10' C9' H9C 109.0 7_556 . ?
N4 C9' H9D 109.0 . . ?
C10' C9' H9D 109.0 7_556 . ?
H9C C9' H9D 107.8 . . ?
N4 C10' C9' 113.1(9) . 7_556 ?
N4 C10' H10C 109.0 . . ?
C9' C10' H10C 109.0 7_556 . ?
N4 C10' H10D 109.0 . . ?
C9' C10' H10D 109.0 7_556 . ?
H10C C10' H10D 107.8 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

























































































N2 Fe1 N1 C1 -16(7) 4_645 . . . ?
N2 Fe1 N1 C1 164(7) 6_566 . . . ?
N1 Fe1 N1 C1 -133(100) 7_656 . . . ?
N3 Fe1 N1 C1 74(7) 7_656 . . . ?
N3 Fe1 N1 C1 -106(7) . . . . ?
N2 Fe1 N3 C3 41.9(7) 4_645 . . . ?
N2 Fe1 N3 C3 -138.1(7) 6_566 . . . ?
N1 Fe1 N3 C3 -48.8(7) 7_656 . . . ?
N1 Fe1 N3 C3 131.2(7) . . . . ?
N3 Fe1 N3 C3 -145(100) 7_656 . . . ?
N2 Fe1 N3 C3' 134.9(7) 4_645 . . . ?
N2 Fe1 N3 C3' -45.1(7) 6_566 . . . ?
N1 Fe1 N3 C3' 44.2(7) 7_656 . . . ?
N1 Fe1 N3 C3' -135.8(7) . . . . ?
N3 Fe1 N3 C3' -52(100) 7_656 . . . ?
N2 Fe1 N3 C5' -36.9(7) 4_645 . . . ?
N2 Fe1 N3 C5' 143.1(7) 6_566 . . . ?
N1 Fe1 N3 C5' -127.7(7) 7_656 . . . ?
N1 Fe1 N3 C5' 52.3(7) . . . . ?
N3 Fe1 N3 C5' 136(100) 7_656 . . . ?
N2 Fe1 N3 C5 -138.9(7) 4_645 . . . ?
N2 Fe1 N3 C5 41.1(7) 6_566 . . . ?
N1 Fe1 N3 C5 130.3(7) 7_656 . . . ?
N1 Fe1 N3 C5 -49.7(7) . . . . ?
N3 Fe1 N3 C5 34(100) 7_656 . . . ?
Fe1 N1 C1 Ag1 25(11) . . . . ?
C2 Ag1 C1 N1 -26(6) . . . . ?
Fe1 N2 C2 Ag1 16(9) 4_655 . . . ?
C1 Ag1 C2 N2 75(5) . . . . ?
C3' N3 C3 C4 64.8(13) . . . . ?
C5' N3 C3 C4 -69.7(13) . . . . ?
C5 N3 C3 C4 0.5(16) . . . . ?
Fe1 N3 C3 C4 179.7(9) . . . . ?
N3 C3 C4 C7 -2.1(19) . . . . ?
C3 N3 C5 C6 -1.0(17) . . . . ?
C3' N3 C5 C6 -67.2(14) . . . . ?
C5' N3 C5 C6 57.5(14) . . . . ?
Fe1 N3 C5 C6 179.8(11) . . . . ?
N3 C5 C6 C7 3(2) . . . . ?
C3 N3 C3' C4' -56.6(12) . . . . ?
C5' N3 C3' C4' -8.2(17) . . . . ?
C5 N3 C3' C4' 63.7(13) . . . . ?
Fe1 N3 C3' C4' 179.9(9) . . . . ?
N3 C3' C4' C7 -0.8(19) . . . . ?
C3 N3 C5' C6' 61.5(12) . . . . ?
C3' N3 C5' C6' 7.8(16) . . . . ?
C5 N3 C5' C6' -58.4(12) . . . . ?
Fe1 N3 C5' C6' 179.4(9) . . . . ?
N3 C5' C6' C7 1.8(19) . . . . ?
C3 C4 C7 C6' 67.4(12) . . . . ?
C3 C4 C7 C6 4.0(17) . . . . ?
C3 C4 C7 C4' -58.5(12) . . . . ?
C3 C4 C7 C8 -179.2(9) . . . . ?
C5' C6' C7 C4 -69.7(13) . . . . ?
C5' C6' C7 C6 59.3(13) . . . . ?
C5' C6' C7 C4' -9.9(16) . . . . ?
C5' C6' C7 C8 177.5(10) . . . . ?
C5 C6 C7 C4 -4.4(18) . . . . ?
C5 C6 C7 C6' -57.9(13) . . . . ?
C5 C6 C7 C4' 59.5(13) . . . . ?
C5 C6 C7 C8 178.6(11) . . . . ?
C3' C4' C7 C4 61.8(13) . . . . ?
C3' C4' C7 C6' 9.5(16) . . . . ?
C3' C4' C7 C6 -65.4(13) . . . . ?
C3' C4' C7 C8 -178.0(10) . . . . ?
C9' N4 C8 C7 57.7(12) . . . . ?
C9 N4 C8 C7 -65.9(10) . . . . ?
C10 N4 C8 C7 151.3(8) . . . . ?
C10' N4 C8 C7 -159.5(9) . . . . ?
C4 C7 C8 N4 70.7(11) . . . . ?
C6' C7 C8 N4 147.5(9) . . . . ?
C6 C7 C8 N4 -112.3(10) . . . . ?
C4' C7 C8 N4 -24.4(12) . . . . ?
C9' N4 C9 C10 35.1(11) . . . 7_556 ?
C8 N4 C9 C10 172.5(7) . . . 7_556 ?
C10 N4 C9 C10 -46.7(14) . . . 7_556 ?
C10' N4 C9 C10 -79.9(11) . . . 7_556 ?
C9' N4 C10 C9 -41.4(12) . . . 7_556 ?
C9 N4 C10 C9 46.2(15) . . . 7_556 ?
C8 N4 C10 C9 -166.5(9) . . . 7_556 ?
C10' N4 C10 C9 94.5(14) . . . 7_556 ?
C9 N4 C9' C10' -33.0(12) . . . 7_556 ?
C8 N4 C9' C10' -170.6(8) . . . 7_556 ?
C10 N4 C9' C10' 82.2(12) . . . 7_556 ?
C10' N4 C9' C10' 48.5(18) . . . 7_556 ?
C9' N4 C10' C9' -48.7(19) . . . 7_556 ?
C9 N4 C10' C9' 38.8(13) . . . 7_556 ?
C8 N4 C10' C9' 164.1(11) . . . 7_556 ?
C10 N4 C10' C9' -98.1(15) . . . 7_556 ?



_diffrn_measured_fraction_theta_max 0.985

_diffrn_reflns_theta_full        61.00

_diffrn_measured_fraction_theta_full 0.985

_refine_diff_density_max         1.420

_refine_diff_density_min         -1.378

_refine_diff_density_rms         0.111





# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.500 0.000 0.014 399 102 ' '
2 1.000 0.500 0.188 399 102 ' '

_platon_squeeze_details          
;

;



# start Validation Reply Form



_vrf_CHEMW03_fe                  
;

PROBLEM: ALERT: The ratio of given/expected molecular weight as

RESPONSE: This is caused by the given molecular weight being increased 

from the atom count to account for half a disordered dimethyl formamide molecule, half a disordered

ethanol molecule and 2 disordered water molecules omitted by SQUEEZE.

;



_vrf_THETM01_fe                  
;

PROBLEM: ALERT: The value of sine(theta_max)/wavelength is less than 0.575

RESPONSE: The crystal diffracted poorly at higher resolution and therefore 

the data were cut at sin(theta_max)/wavelength = 0.5617 and theta = 60.0 deg.

;
_database_code_depnum_ccdc_archive 'CCDC 987371'
#######################################################################
#
#                 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_1-225K





_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C22.50 H30.50 Ag2 Fe N8.50 O3'

_chemical_formula_weight         739.64



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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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                   16.3171(9)

_cell_length_b                   13.8577(5)

_cell_length_c                   14.8466(9)

_cell_angle_alpha                90.00

_cell_angle_beta                 111.744(6)

_cell_angle_gamma                90.00

_cell_volume                     3118.2(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    225(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.42

_exptl_crystal_size_mid          0.32

_exptl_crystal_size_min          0.25

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.576

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1476

_exptl_absorpt_coefficient_mu    13.960

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.0673

_exptl_absorpt_correction_T_max  0.1280

_exptl_absorpt_process_details   ?



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      225(2)

_diffrn_radiation_wavelength     1.54178

_diffrn_radiation_type           CuK\a

_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'

_diffrn_radiation_monochromator  mirror

_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean 16.0855

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            4578

_diffrn_reflns_av_R_equivalents  0.0414

_diffrn_reflns_av_sigmaI/netI    0.0521

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       18

_diffrn_reflns_limit_k_min       -15

_diffrn_reflns_limit_k_max       10

_diffrn_reflns_limit_l_min       -16

_diffrn_reflns_limit_l_max       14

_diffrn_reflns_theta_min         4.32

_diffrn_reflns_theta_max         60.98

_reflns_number_total             2339

_reflns_number_gt                2035

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_refine_special_details          
; 

 'SADI N4 C9 N4 C10 N4 C9' N4 C10'' is executed. Since the piperazine ring

 is disordered over two sites, relevant bonds are essentially equal.



 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)+(0.0772P)²+14.4928P] 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         2339

_refine_ls_number_parameters     198

_refine_ls_number_restraints     6

_refine_ls_R_factor_all          0.0586

_refine_ls_R_factor_gt           0.0528

_refine_ls_wR_factor_ref         0.1476

_refine_ls_wR_factor_gt          0.1419

_refine_ls_goodness_of_fit_ref   1.071

_refine_ls_restrained_S_all      1.095

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group








































Ag1 Ag 0.76993(4) 0.52997(4) 0.28356(4) 0.0633(3) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.2500 0.5000 0.0271(3) Uani 1 2 d S . .
N1 N 0.7589(4) 0.3627(4) 0.4260(4) 0.0412(12) Uani 1 1 d . . .
N2 N 0.7706(4) 0.6708(4) 0.1140(4) 0.0397(12) Uani 1 1 d . . .
N3 N 0.6187(3) 0.2731(4) 0.4604(3) 0.0371(12) Uani 1 1 d . . .
N4 N 0.3054(4) 0.2827(6) 0.4522(6) 0.078(2) Uani 1 1 d D . .
C1 C 0.7651(5) 0.4246(5) 0.3799(5) 0.0499(17) Uani 1 1 d . . .
C2 C 0.7751(5) 0.6218(5) 0.1775(5) 0.0537(18) Uani 1 1 d . . .
C3 C 0.5569(9) 0.2074(10) 0.4284(10) 0.045(3) Uani 0.491(9) 1 d P A 1
H3A H 0.5758 0.1443 0.4228 0.054 Uiso 0.491(9) 1 calc PR A 1
C4 C 0.4670(10) 0.2205(11) 0.4020(11) 0.053(4) Uani 0.491(9) 1 d P A 1
H4A H 0.4278 0.1687 0.3775 0.063 Uiso 0.491(9) 1 calc PR A 1
C5 C 0.5842(9) 0.3642(10) 0.4647(13) 0.057(4) Uani 0.491(9) 1 d P A 1
H5A H 0.6240 0.4161 0.4845 0.069 Uiso 0.491(9) 1 calc PR A 1
C6 C 0.4954(11) 0.3840(12) 0.4419(15) 0.070(5) Uani 0.491(9) 1 d P A 1
H6A H 0.4753 0.4467 0.4466 0.084 Uiso 0.491(9) 1 calc PR A 1
C3' C 0.5832(9) 0.2637(11) 0.5273(9) 0.051(4) Uani 0.509(9) 1 d P A 2
H3B H 0.6199 0.2451 0.5903 0.061 Uiso 0.509(9) 1 calc PR A 2
C4' C 0.4975(10) 0.2795(13) 0.5091(10) 0.060(4) Uani 0.509(9) 1 d P A 2
H4B H 0.4760 0.2736 0.5594 0.072 Uiso 0.509(9) 1 calc PR A 2
C5' C 0.5660(9) 0.2816(10) 0.3696(10) 0.047(3) Uani 0.509(9) 1 d P A 2
H5B H 0.5897 0.2772 0.3209 0.056 Uiso 0.509(9) 1 calc PR A 2
C6' C 0.4763(9) 0.2969(12) 0.3437(10) 0.053(4) Uani 0.509(9) 1 d P A 2
H6B H 0.4407 0.3013 0.2776 0.064 Uiso 0.509(9) 1 calc PR A 2
C7 C 0.4372(5) 0.3058(6) 0.4116(5) 0.0544(18) Uani 1 1 d . . .
C8 C 0.3409(5) 0.3253(8) 0.3874(6) 0.067(2) Uani 1 1 d . A .
H8A H 0.3320 0.3953 0.3868 0.081 Uiso 1 1 calc R . .
H8B H 0.3079 0.3013 0.3218 0.081 Uiso 1 1 calc R . .
C9 C 0.2977(8) 0.1851(10) 0.4621(11) 0.057(5) Uani 0.534(17) 1 d PD . 1
H9A H 0.3553 0.1548 0.4752 0.069 Uiso 0.534(17) 1 calc PR . 1
H9B H 0.2564 0.1589 0.4008 0.069 Uiso 0.534(17) 1 calc PR . 1
C10 C 0.2335(9) 0.3408(12) 0.4589(13) 0.061(4) Uani 0.534(17) 1 d PD . 1
H10A H 0.1833 0.3362 0.3971 0.073 Uiso 0.534(17) 1 calc PR . 1
H10B H 0.2524 0.4084 0.4675 0.073 Uiso 0.534(17) 1 calc PR . 1
C9' C 0.3345(10) 0.2931(15) 0.5490(10) 0.066(6) Uani 0.466(17) 1 d PD . 2
H9C H 0.3210 0.3583 0.5650 0.079 Uiso 0.466(17) 1 calc PR . 2
H9D H 0.3987 0.2845 0.5767 0.079 Uiso 0.466(17) 1 calc PR . 2
C10' C 0.2086(8) 0.280(2) 0.4075(13) 0.077(8) Uani 0.466(17) 1 d PD . 2
H10C H 0.1915 0.2660 0.3382 0.093 Uiso 0.466(17) 1 calc PR . 2
H10D H 0.1857 0.3442 0.4132 0.093 Uiso 0.466(17) 1 calc PR . 2






_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



















































Ag1 C2 2.050(7) . ?
Ag1 C1 2.066(7) . ?
Fe1 N2 1.939(5) 4_645 ?
Fe1 N2 1.939(5) 6_566 ?
Fe1 N1 1.946(5) 7_656 ?
Fe1 N1 1.946(6) . ?
Fe1 N3 2.027(5) 7_656 ?
Fe1 N3 2.027(5) . ?
N1 C1 1.124(9) . ?
N2 C2 1.143(9) . ?
N2 Fe1 1.939(5) 4_655 ?
N3 C5' 1.308(14) . ?
N3 C3 1.310(15) . ?
N3 C3' 1.327(14) . ?
N3 C5 1.393(14) . ?
N4 C9' 1.345(14) . ?
N4 C9 1.372(13) . ?
N4 C8 1.422(11) . ?
N4 C10 1.458(13) . ?
N4 C10' 1.470(14) . ?
C3 C4 1.38(2) . ?
C3 H3A 0.9400 . ?
C4 C7 1.306(17) . ?
C4 H4A 0.9400 . ?
C5 C6 1.39(2) . ?
C5 H5A 0.9400 . ?
C6 C7 1.40(2) . ?
C6 H6A 0.9400 . ?
C3' C4' 1.34(2) . ?
C3' H3B 0.9400 . ?
C4' C7 1.463(16) . ?
C4' H4B 0.9400 . ?
C5' C6' 1.39(2) . ?
C5' H5B 0.9400 . ?
C6' C7 1.384(16) . ?
C6' H6B 0.9400 . ?
C7 C8 1.500(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.48(2) 7_556 ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C9 1.48(2) 7_556 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C9' C10' 1.51(3) 7_556 ?
C9' H9C 0.9800 . ?
C9' H9D 0.9800 . ?
C10' C9' 1.51(3) 7_556 ?
C10' H10C 0.9800 . ?
C10' H10D 0.9800 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag








































































































C2 Ag1 C1 173.4(3) . . ?
N2 Fe1 N2 180.000(1) 4_645 6_566 ?
N2 Fe1 N1 90.8(2) 4_645 7_656 ?
N2 Fe1 N1 89.2(2) 6_566 7_656 ?
N2 Fe1 N1 89.2(2) 4_645 . ?
N2 Fe1 N1 90.8(2) 6_566 . ?
N1 Fe1 N1 180.000(1) 7_656 . ?
N2 Fe1 N3 89.2(2) 4_645 7_656 ?
N2 Fe1 N3 90.8(2) 6_566 7_656 ?
N1 Fe1 N3 90.1(2) 7_656 7_656 ?
N1 Fe1 N3 89.9(2) . 7_656 ?
N2 Fe1 N3 90.8(2) 4_645 . ?
N2 Fe1 N3 89.2(2) 6_566 . ?
N1 Fe1 N3 89.9(2) 7_656 . ?
N1 Fe1 N3 90.1(2) . . ?
N3 Fe1 N3 180.0(3) 7_656 . ?
C1 N1 Fe1 176.3(6) . . ?
C2 N2 Fe1 174.0(6) . 4_655 ?
C5' N3 C3 64.3(9) . . ?
C5' N3 C3' 118.6(9) . . ?
C3 N3 C3' 73.3(9) . . ?
C5' N3 C5 81.0(10) . . ?
C3 N3 C5 112.2(9) . . ?
C3' N3 C5 76.1(10) . . ?
C5' N3 Fe1 122.2(7) . . ?
C3 N3 Fe1 125.7(7) . . ?
C3' N3 Fe1 118.3(7) . . ?
C5 N3 Fe1 122.1(7) . . ?
C9' N4 C9 90.0(12) . . ?
C9' N4 C8 127.4(11) . . ?
C9 N4 C8 124.0(10) . . ?
C9' N4 C10 80.9(11) . . ?
C9 N4 C10 115.4(10) . . ?
C8 N4 C10 111.0(9) . . ?
C9' N4 C10' 112.3(12) . . ?
C9 N4 C10' 84.2(13) . . ?
C8 N4 C10' 110.1(8) . . ?
C10 N4 C10' 44.5(11) . . ?
N1 C1 Ag1 174.4(6) . . ?
N2 C2 Ag1 174.0(7) . . ?
N3 C3 C4 127.1(12) . . ?
N3 C3 H3A 116.4 . . ?
C4 C3 H3A 116.4 . . ?
C7 C4 C3 119.1(13) . . ?
C7 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C6 C5 N3 124.8(13) . . ?
C6 C5 H5A 117.6 . . ?
N3 C5 H5A 117.6 . . ?
C5 C6 C7 116.6(13) . . ?
C5 C6 H6A 121.7 . . ?
C7 C6 H6A 121.7 . . ?
N3 C3' C4' 123.0(12) . . ?
N3 C3' H3B 118.5 . . ?
C4' C3' H3B 118.5 . . ?
C3' C4' C7 120.6(12) . . ?
C3' C4' H4B 119.7 . . ?
C7 C4' H4B 119.7 . . ?
N3 C5' C6' 121.5(12) . . ?
N3 C5' H5B 119.2 . . ?
C6' C5' H5B 119.2 . . ?
C7 C6' C5' 122.4(11) . . ?
C7 C6' H6B 118.8 . . ?
C5' C6' H6B 118.8 . . ?
C4 C7 C6' 63.2(10) . . ?
C4 C7 C6 120.0(11) . . ?
C6' C7 C6 82.1(11) . . ?
C4 C7 C4' 75.0(10) . . ?
C6' C7 C4' 112.0(9) . . ?
C6 C7 C4' 75.4(11) . . ?
C4 C7 C8 122.4(10) . . ?
C6' C7 C8 124.4(8) . . ?
C6 C7 C8 117.6(9) . . ?
C4' C7 C8 122.9(8) . . ?
N4 C8 C7 114.6(6) . . ?
N4 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
N4 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
N4 C9 C10 113.3(11) . 7_556 ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 7_556 . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 7_556 . ?
H9A C9 H9B 107.7 . . ?
N4 C10 C9 116.2(12) . 7_556 ?
N4 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 7_556 . ?
N4 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 7_556 . ?
H10A C10 H10B 107.4 . . ?
N4 C9' C10' 110.5(15) . 7_556 ?
N4 C9' H9C 109.5 . . ?
C10' C9' H9C 109.5 7_556 . ?
N4 C9' H9D 109.5 . . ?
C10' C9' H9D 109.5 7_556 . ?
H9C C9' H9D 108.1 . . ?
N4 C10' C9' 114.6(12) . 7_556 ?
N4 C10' H10C 108.6 . . ?
C9' C10' H10C 108.6 7_556 . ?
N4 C10' H10D 108.6 . . ?
C9' C10' H10D 108.6 7_556 . ?
H10C C10' H10D 107.6 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

























































































N2 Fe1 N1 C1 -21(9) 4_645 . . . ?
N2 Fe1 N1 C1 159(9) 6_566 . . . ?
N1 Fe1 N1 C1 -142(100) 7_656 . . . ?
N3 Fe1 N1 C1 68(9) 7_656 . . . ?
N3 Fe1 N1 C1 -112(9) . . . . ?
N2 Fe1 N3 C5' -35.2(8) 4_645 . . . ?
N2 Fe1 N3 C5' 144.8(8) 6_566 . . . ?
N1 Fe1 N3 C5' -126.0(8) 7_656 . . . ?
N1 Fe1 N3 C5' 54.0(8) . . . . ?
N3 Fe1 N3 C5' 68(100) 7_656 . . . ?
N2 Fe1 N3 C3 44.5(9) 4_645 . . . ?
N2 Fe1 N3 C3 -135.5(9) 6_566 . . . ?
N1 Fe1 N3 C3 -46.3(9) 7_656 . . . ?
N1 Fe1 N3 C3 133.7(9) . . . . ?
N3 Fe1 N3 C3 148(100) 7_656 . . . ?
N2 Fe1 N3 C3' 133.7(9) 4_645 . . . ?
N2 Fe1 N3 C3' -46.3(9) 6_566 . . . ?
N1 Fe1 N3 C3' 42.9(9) 7_656 . . . ?
N1 Fe1 N3 C3' -137.1(9) . . . . ?
N3 Fe1 N3 C3' -123(100) 7_656 . . . ?
N2 Fe1 N3 C5 -135.4(10) 4_645 . . . ?
N2 Fe1 N3 C5 44.6(10) 6_566 . . . ?
N1 Fe1 N3 C5 133.8(10) 7_656 . . . ?
N1 Fe1 N3 C5 -46.2(10) . . . . ?
N3 Fe1 N3 C5 -32(100) 7_656 . . . ?
Fe1 N1 C1 Ag1 40(15) . . . . ?
C2 Ag1 C1 N1 -31(8) . . . . ?
Fe1 N2 C2 Ag1 2(12) 4_655 . . . ?
C1 Ag1 C2 N2 74(8) . . . . ?
C5' N3 C3 C4 -68.4(16) . . . . ?
C3' N3 C3 C4 65.9(16) . . . . ?
C5 N3 C3 C4 -1.0(19) . . . . ?
Fe1 N3 C3 C4 179.1(11) . . . . ?
N3 C3 C4 C7 -2(2) . . . . ?
C5' N3 C5 C6 59.9(19) . . . . ?
C3 N3 C5 C6 3(2) . . . . ?
C3' N3 C5 C6 -62.7(18) . . . . ?
Fe1 N3 C5 C6 -177.6(14) . . . . ?
N3 C5 C6 C7 -1(3) . . . . ?
C5' N3 C3' C4' -12(2) . . . . ?
C3 N3 C3' C4' -59.5(16) . . . . ?
C5 N3 C3' C4' 59.2(17) . . . . ?
Fe1 N3 C3' C4' 178.5(13) . . . . ?
N3 C3' C4' C7 2(2) . . . . ?
C3 N3 C5' C6' 62.2(14) . . . . ?
C3' N3 C5' C6' 10.8(19) . . . . ?
C5 N3 C5' C6' -57.9(15) . . . . ?
Fe1 N3 C5' C6' 179.6(10) . . . . ?
N3 C5' C6' C7 1(2) . . . . ?
C3 C4 C7 C6' 66.3(14) . . . . ?
C3 C4 C7 C6 4(2) . . . . ?
C3 C4 C7 C4' -58.5(14) . . . . ?
C3 C4 C7 C8 -178.2(11) . . . . ?
C5' C6' C7 C4 -69.5(16) . . . . ?
C5' C6' C7 C6 59.9(16) . . . . ?
C5' C6' C7 C4' -11(2) . . . . ?
C5' C6' C7 C8 178.1(12) . . . . ?
C5 C6 C7 C4 -3(2) . . . . ?
C5 C6 C7 C6' -55.6(17) . . . . ?
C5 C6 C7 C4' 59.7(17) . . . . ?
C5 C6 C7 C8 179.5(13) . . . . ?
C3' C4' C7 C4 61.5(17) . . . . ?
C3' C4' C7 C6' 9(2) . . . . ?
C3' C4' C7 C6 -65.7(17) . . . . ?
C3' C4' C7 C8 -179.4(13) . . . . ?
C9' N4 C8 C7 55.0(15) . . . . ?
C9 N4 C8 C7 -66.1(13) . . . . ?
C10 N4 C8 C7 149.6(10) . . . . ?
C10' N4 C8 C7 -162.7(14) . . . . ?
C4 C7 C8 N4 69.9(13) . . . . ?
C6' C7 C8 N4 147.6(11) . . . . ?
C6 C7 C8 N4 -112.5(13) . . . . ?
C4' C7 C8 N4 -22.6(15) . . . . ?
C9' N4 C9 C10 37.3(13) . . . 7_556 ?
C8 N4 C9 C10 174.5(9) . . . 7_556 ?
C10 N4 C9 C10 -42.6(18) . . . 7_556 ?
C10' N4 C9 C10 -75.1(15) . . . 7_556 ?
C9' N4 C10 C9 -41.8(15) . . . 7_556 ?
C9 N4 C10 C9 43.8(19) . . . 7_556 ?
C8 N4 C10 C9 -168.5(12) . . . 7_556 ?
C10' N4 C10 C9 93.7(18) . . . 7_556 ?
C9 N4 C9' C10' -33.1(14) . . . 7_556 ?
C8 N4 C9' C10' -167.8(11) . . . 7_556 ?
C10 N4 C9' C10' 82.7(15) . . . 7_556 ?
C10' N4 C9' C10' 51(2) . . . 7_556 ?
C9' N4 C10' C9' -53(3) . . . 7_556 ?
C9 N4 C10' C9' 34.8(19) . . . 7_556 ?
C8 N4 C10' C9' 158.9(16) . . . 7_556 ?
C10 N4 C10' C9' -101(2) . . . 7_556 ?



_diffrn_measured_fraction_theta_max 0.981

_diffrn_reflns_theta_full        60.98

_diffrn_measured_fraction_theta_full 0.981

_refine_diff_density_max         1.880

_refine_diff_density_min         -0.957

_refine_diff_density_rms         0.112



# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.500 0.000 0.014 399 102 ' '
2 1.000 0.500 0.188 399 102 ' '

_platon_squeeze_details          
;

;



# start Validation Reply Form



_vrf_CHEMW03_fe                  
;

PROBLEM: ALERT: The ratio of given/expected molecular weight as

RESPONSE: This is caused by the given molecular weight being increased 

from the atom count to account for half a disordered dimethyl formamide molecule, half a disordered

ethanol molecule and 2 disordered water molecules omitted by SQUEEZE.

;



_vrf_THETM01_fe                  
;

PROBLEM: ALERT: The value of sine(theta_max)/wavelength is less than 0.575

RESPONSE: The crystal diffracted poorly at higher resolution and therefore 

the data were cut at sin(theta_max)/wavelength = 0.5617 and theta = 60.0 deg.

;
_database_code_depnum_ccdc_archive 'CCDC 987372'
#######################################################################
#
#                 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_1-300K



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C22.50 H30.50 Ag2 Fe N8.50 O3'

_chemical_formula_weight         739.64



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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 '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                   16.622(2)

_cell_length_b                   13.9014(10)

_cell_length_c                   15.434(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 112.586(17)

_cell_angle_gamma                90.00

_cell_volume                     3292.7(7)

_cell_formula_units_Z            4

_cell_measurement_temperature    300(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.42

_exptl_crystal_size_mid          0.32

_exptl_crystal_size_min          0.25

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.492

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1476

_exptl_absorpt_coefficient_mu    13.220

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.0720

_exptl_absorpt_correction_T_max  0.1367

_exptl_absorpt_process_details   ?



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      300(2)

_diffrn_radiation_wavelength     1.54178

_diffrn_radiation_type           CuK\a

_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'

_diffrn_radiation_monochromator  mirror

_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean 16.0855

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            4870

_diffrn_reflns_av_R_equivalents  0.0369

_diffrn_reflns_av_sigmaI/netI    0.0438

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       17

_diffrn_reflns_limit_k_min       -9

_diffrn_reflns_limit_k_max       15

_diffrn_reflns_limit_l_min       -15

_diffrn_reflns_limit_l_max       17

_diffrn_reflns_theta_min         4.29

_diffrn_reflns_theta_max         60.99

_reflns_number_total             2463

_reflns_number_gt                1877

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_refine_special_details          
; 

 'SADI N4 C9 N4 C10 N4 C9' N4 C10'

DELU 0.01 0.01 N4 C9

DELU 0.01 0.01 C9' C10'' is executed. Since the piperazine ring

 is disordered over two sites, these restraints are needed to comply with

 their chemical nature.



 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)+(0.0825P)²+14.1386P] 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         2463

_refine_ls_number_parameters     198

_refine_ls_number_restraints     7

_refine_ls_R_factor_all          0.0828

_refine_ls_R_factor_gt           0.0682

_refine_ls_wR_factor_ref         0.1961

_refine_ls_wR_factor_gt          0.1835

_refine_ls_goodness_of_fit_ref   1.138

_refine_ls_restrained_S_all      1.145

_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








































Ag1 Ag 0.77045(6) 0.53595(7) 0.28739(6) 0.1246(5) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.2500 0.5000 0.0555(5) Uani 1 2 d S . .
N1 N 0.7597(5) 0.3760(5) 0.4278(6) 0.084(2) Uani 1 1 d . . .
N2 N 0.7769(5) 0.6711(6) 0.1262(6) 0.089(2) Uani 1 1 d . . .
N3 N 0.6101(5) 0.2771(5) 0.4608(5) 0.0721(17) Uani 1 1 d . . .
N4 N 0.3034(6) 0.2847(8) 0.4542(7) 0.110(3) Uani 1 1 d DU . .
C1 C 0.7646(7) 0.4345(8) 0.3811(7) 0.097(3) Uani 1 1 d . . .
C2 C 0.7778(7) 0.6259(8) 0.1847(8) 0.103(3) Uani 1 1 d . . .
C3 C 0.5470(13) 0.2178(16) 0.4277(15) 0.090(6) Uani 0.487(13) 1 d P A 1
H3A H 0.5619 0.1563 0.4155 0.108 Uiso 0.487(13) 1 calc PR A 1
C4 C 0.4629(13) 0.232(2) 0.408(2) 0.116(9) Uani 0.487(13) 1 d P A 1
H4A H 0.4253 0.1800 0.3877 0.139 Uiso 0.487(13) 1 calc PR A 1
C5 C 0.5787(15) 0.3695(16) 0.471(2) 0.119(9) Uani 0.487(13) 1 d P A 1
H5A H 0.6182 0.4199 0.4922 0.143 Uiso 0.487(13) 1 calc PR A 1
C6 C 0.4916(16) 0.3874(17) 0.449(2) 0.123(10) Uani 0.487(13) 1 d P A 1
H6A H 0.4726 0.4486 0.4565 0.148 Uiso 0.487(13) 1 calc PR A 1
C3' C 0.5789(12) 0.2662(16) 0.5248(13) 0.093(6) Uani 0.513(13) 1 d P A 2
H3B H 0.6157 0.2463 0.5844 0.112 Uiso 0.513(13) 1 calc PR A 2
C4' C 0.4923(14) 0.283(2) 0.5069(14) 0.114(8) Uani 0.513(13) 1 d P A 2
H4B H 0.4727 0.2771 0.5555 0.137 Uiso 0.513(13) 1 calc PR A 2
C5' C 0.5550(12) 0.2835(15) 0.3715(12) 0.081(5) Uani 0.513(13) 1 d P A 2
H5B H 0.5759 0.2756 0.3240 0.097 Uiso 0.513(13) 1 calc PR A 2
C6' C 0.4680(11) 0.3017(17) 0.3484(13) 0.090(6) Uani 0.513(13) 1 d P A 2
H6B H 0.4319 0.3084 0.2855 0.108 Uiso 0.513(13) 1 calc PR A 2
C7 C 0.4319(6) 0.3106(9) 0.4161(7) 0.094(3) Uani 1 1 d . . .
C8 C 0.3380(7) 0.3337(10) 0.3945(8) 0.111(4) Uani 1 1 d . A .
H8A H 0.3322 0.4025 0.4008 0.133 Uiso 1 1 calc R . .
H8B H 0.3038 0.3166 0.3298 0.133 Uiso 1 1 calc R . .
C9 C 0.2952(13) 0.1847(12) 0.4635(17) 0.100(7) Uani 0.50(2) 1 d PDU . 1
H9A H 0.3509 0.1544 0.4743 0.120 Uiso 0.50(2) 1 calc PR . 1
H9B H 0.2531 0.1596 0.4050 0.120 Uiso 0.50(2) 1 calc PR . 1
C10 C 0.2320(16) 0.341(2) 0.461(2) 0.108(9) Uani 0.50(2) 1 d PD . 1
H10A H 0.2494 0.4086 0.4681 0.130 Uiso 0.50(2) 1 calc PR . 1
H10B H 0.1821 0.3356 0.4018 0.130 Uiso 0.50(2) 1 calc PR . 1
C9' C 0.3345(15) 0.285(2) 0.5522(13) 0.129(11) Uani 0.50(2) 1 d PD . 2
H9C H 0.3234 0.3476 0.5735 0.155 Uiso 0.50(2) 1 calc PR . 2
H9D H 0.3969 0.2747 0.5778 0.155 Uiso 0.50(2) 1 calc PR . 2
C10' C 0.2076(10) 0.289(3) 0.413(2) 0.126(14) Uani 0.50(2) 1 d PD . 2
H10C H 0.1895 0.3519 0.4274 0.151 Uiso 0.50(2) 1 calc PR . 2
H10D H 0.1877 0.2839 0.3457 0.151 Uiso 0.50(2) 1 calc PR . 2






_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



















































Ag1 C1 2.048(9) . ?
Ag1 C2 2.060(10) . ?
Fe1 N1 2.115(7) 7_656 ?
Fe1 N1 2.115(7) . ?
Fe1 N2 2.128(8) 6_566 ?
Fe1 N2 2.128(8) 4_645 ?
Fe1 N3 2.198(7) . ?
Fe1 N3 2.198(7) 7_656 ?
N1 C1 1.111(11) . ?
N2 C2 1.094(11) . ?
N2 Fe1 2.128(8) 4_655 ?
N3 C3 1.28(2) . ?
N3 C3' 1.29(2) . ?
N3 C5' 1.332(18) . ?
N3 C5 1.42(2) . ?
N4 C9' 1.397(17) . ?
N4 C9 1.409(16) . ?
N4 C8 1.433(14) . ?
N4 C10 1.460(16) . ?
N4 C10' 1.472(15) . ?
C3 C4 1.33(3) . ?
C3 H3A 0.9300 . ?
C4 C7 1.23(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.38(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.41(3) . ?
C6 H6A 0.9300 . ?
C3' C4' 1.38(3) . ?
C3' H3B 0.9300 . ?
C4' C7 1.43(2) . ?
C4' H4B 0.9300 . ?
C5' C6' 1.37(2) . ?
C5' H5B 0.9300 . ?
C6' C7 1.40(2) . ?
C6' H6B 0.9300 . ?
C7 C8 1.501(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.45(3) 7_556 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C9 1.45(3) 7_556 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9' C10' 1.46(4) 7_556 ?
C9' H9C 0.9700 . ?
C9' H9D 0.9700 . ?
C10' C9' 1.46(4) 7_556 ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag








































































































C1 Ag1 C2 173.9(5) . . ?
N1 Fe1 N1 180.000(1) 7_656 . ?
N1 Fe1 N2 88.6(3) 7_656 6_566 ?
N1 Fe1 N2 91.4(3) . 6_566 ?
N1 Fe1 N2 91.4(3) 7_656 4_645 ?
N1 Fe1 N2 88.6(3) . 4_645 ?
N2 Fe1 N2 180.000(1) 6_566 4_645 ?
N1 Fe1 N3 90.0(3) 7_656 . ?
N1 Fe1 N3 90.0(3) . . ?
N2 Fe1 N3 89.5(3) 6_566 . ?
N2 Fe1 N3 90.5(3) 4_645 . ?
N1 Fe1 N3 90.0(3) 7_656 7_656 ?
N1 Fe1 N3 90.0(3) . 7_656 ?
N2 Fe1 N3 90.5(3) 6_566 7_656 ?
N2 Fe1 N3 89.5(3) 4_645 7_656 ?
N3 Fe1 N3 180.0(4) . 7_656 ?
C1 N1 Fe1 171.1(9) . . ?
C2 N2 Fe1 169.1(8) . 4_655 ?
C3 N3 C3' 73.7(14) . . ?
C3 N3 C5' 59.8(13) . . ?
C3' N3 C5' 118.8(12) . . ?
C3 N3 C5 110.3(14) . . ?
C3' N3 C5 75.6(15) . . ?
C5' N3 C5 85.1(16) . . ?
C3 N3 Fe1 128.3(10) . . ?
C3' N3 Fe1 117.6(9) . . ?
C5' N3 Fe1 122.0(9) . . ?
C5 N3 Fe1 121.4(11) . . ?
C9' N4 C9 84.6(17) . . ?
C9' N4 C8 128.4(17) . . ?
C9 N4 C8 127.8(14) . . ?
C9' N4 C10 84.0(16) . . ?
C9 N4 C10 114.5(16) . . ?
C8 N4 C10 108.9(15) . . ?
C9' N4 C10' 110.6(18) . . ?
C9 N4 C10' 88(2) . . ?
C8 N4 C10' 109.8(12) . . ?
C10 N4 C10' 39.7(17) . . ?
N1 C1 Ag1 176.1(10) . . ?
N2 C2 Ag1 175.4(10) . . ?
N3 C3 C4 129(2) . . ?
N3 C3 H3A 115.6 . . ?
C4 C3 H3A 115.6 . . ?
C7 C4 C3 124(2) . . ?
C7 C4 H4A 118.2 . . ?
C3 C4 H4A 118.2 . . ?
C6 C5 N3 122(2) . . ?
C6 C5 H5A 118.8 . . ?
N3 C5 H5A 118.8 . . ?
C5 C6 C7 118.5(19) . . ?
C5 C6 H6A 120.7 . . ?
C7 C6 H6A 120.7 . . ?
N3 C3' C4' 121.5(17) . . ?
N3 C3' H3B 119.2 . . ?
C4' C3' H3B 119.2 . . ?
C3' C4' C7 122.0(18) . . ?
C3' C4' H4B 119.0 . . ?
C7 C4' H4B 119.0 . . ?
N3 C5' C6' 121.2(15) . . ?
N3 C5' H5B 119.4 . . ?
C6' C5' H5B 119.4 . . ?
C5' C6' C7 122.4(14) . . ?
C5' C6' H6B 118.8 . . ?
C7 C6' H6B 118.8 . . ?
C4 C7 C6' 62.1(16) . . ?
C4 C7 C6 116.2(15) . . ?
C6' C7 C6 83.9(16) . . ?
C4 C7 C4' 72.4(17) . . ?
C6' C7 C4' 111.6(13) . . ?
C6 C7 C4' 73.3(17) . . ?
C4 C7 C8 127.3(15) . . ?
C6' C7 C8 124.2(10) . . ?
C6 C7 C8 116.4(14) . . ?
C4' C7 C8 123.7(12) . . ?
N4 C8 C7 113.3(9) . . ?
N4 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
N4 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N4 C9 C10 113.6(16) . 7_556 ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 7_556 . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 7_556 . ?
H9A C9 H9B 107.7 . . ?
C9 C10 N4 116(2) 7_556 . ?
C9 C10 H10A 108.4 7_556 . ?
N4 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 7_556 . ?
N4 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
N4 C9' C10' 111(2) . 7_556 ?
N4 C9' H9C 109.4 . . ?
C10' C9' H9C 109.4 7_556 . ?
N4 C9' H9D 109.4 . . ?
C10' C9' H9D 109.4 7_556 . ?
H9C C9' H9D 108.0 . . ?
C9' C10' N4 113.7(19) 7_556 . ?
C9' C10' H10C 108.8 7_556 . ?
N4 C10' H10C 108.8 . . ?
C9' C10' H10D 108.8 7_556 . ?
N4 C10' H10D 108.8 . . ?
H10C C10' H10D 107.7 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

























































































N1 Fe1 N1 C1 172(100) 7_656 . . . ?
N2 Fe1 N1 C1 169(5) 6_566 . . . ?
N2 Fe1 N1 C1 -11(5) 4_645 . . . ?
N3 Fe1 N1 C1 -101(5) . . . . ?
N3 Fe1 N1 C1 79(5) 7_656 . . . ?
N1 Fe1 N3 C3 -46.4(15) 7_656 . . . ?
N1 Fe1 N3 C3 133.6(15) . . . . ?
N2 Fe1 N3 C3 -135.0(15) 6_566 . . . ?
N2 Fe1 N3 C3 45.0(15) 4_645 . . . ?
N3 Fe1 N3 C3 166(100) 7_656 . . . ?
N1 Fe1 N3 C3' 44.2(12) 7_656 . . . ?
N1 Fe1 N3 C3' -135.8(12) . . . . ?
N2 Fe1 N3 C3' -44.4(12) 6_566 . . . ?
N2 Fe1 N3 C3' 135.6(12) 4_645 . . . ?
N3 Fe1 N3 C3' -103(100) 7_656 . . . ?
N1 Fe1 N3 C5' -121.2(12) 7_656 . . . ?
N1 Fe1 N3 C5' 58.8(12) . . . . ?
N2 Fe1 N3 C5' 150.2(12) 6_566 . . . ?
N2 Fe1 N3 C5' -29.8(12) 4_645 . . . ?
N3 Fe1 N3 C5' 92(100) 7_656 . . . ?
N1 Fe1 N3 C5 133.6(15) 7_656 . . . ?
N1 Fe1 N3 C5 -46.4(15) . . . . ?
N2 Fe1 N3 C5 44.9(15) 6_566 . . . ?
N2 Fe1 N3 C5 -135.1(15) 4_645 . . . ?
N3 Fe1 N3 C5 -14(100) 7_656 . . . ?
Fe1 N1 C1 Ag1 19(19) . . . . ?
C2 Ag1 C1 N1 -27(17) . . . . ?
Fe1 N2 C2 Ag1 14(20) 4_655 . . . ?
C1 Ag1 C2 N2 64(17) . . . . ?
C3' N3 C3 C4 64(3) . . . . ?
C5' N3 C3 C4 -75(3) . . . . ?
C5 N3 C3 C4 -4(3) . . . . ?
Fe1 N3 C3 C4 176(2) . . . . ?
N3 C3 C4 C7 4(5) . . . . ?
C3 N3 C5 C6 2(3) . . . . ?
C3' N3 C5 C6 -64(3) . . . . ?
C5' N3 C5 C6 57(3) . . . . ?
Fe1 N3 C5 C6 -178(2) . . . . ?
N3 C5 C6 C7 0(4) . . . . ?
C3 N3 C3' C4' -56(2) . . . . ?
C5' N3 C3' C4' -15(3) . . . . ?
C5 N3 C3' C4' 61(2) . . . . ?
Fe1 N3 C3' C4' 178.7(18) . . . . ?
N3 C3' C4' C7 2(4) . . . . ?
C3 N3 C5' C6' 62(2) . . . . ?
C3' N3 C5' C6' 16(3) . . . . ?
C5 N3 C5' C6' -55(2) . . . . ?
Fe1 N3 C5' C6' -179.1(15) . . . . ?
N3 C5' C6' C7 -3(3) . . . . ?
C3 C4 C7 C6' 66(3) . . . . ?
C3 C4 C7 C6 -1(4) . . . . ?
C3 C4 C7 C4' -62(3) . . . . ?
C3 C4 C7 C8 179(2) . . . . ?
C5' C6' C7 C4 -64(2) . . . . ?
C5' C6' C7 C6 60(2) . . . . ?
C5' C6' C7 C4' -9(3) . . . . ?
C5' C6' C7 C8 177.8(17) . . . . ?
C5 C6 C7 C4 0(4) . . . . ?
C5 C6 C7 C6' -55(3) . . . . ?
C5 C6 C7 C4' 60(3) . . . . ?
C5 C6 C7 C8 180(2) . . . . ?
C3' C4' C7 C4 59(3) . . . . ?
C3' C4' C7 C6' 10(3) . . . . ?
C3' C4' C7 C6 -67(3) . . . . ?
C3' C4' C7 C8 -177.5(19) . . . . ?
C9' N4 C8 C7 56(2) . . . . ?
C9 N4 C8 C7 -61.7(19) . . . . ?
C10 N4 C8 C7 153.2(16) . . . . ?
C10' N4 C8 C7 -165(2) . . . . ?
C4 C7 C8 N4 65(2) . . . . ?
C6' C7 C8 N4 143.6(17) . . . . ?
C6 C7 C8 N4 -115.2(18) . . . . ?
C4' C7 C8 N4 -28(2) . . . . ?
C9' N4 C9 C10 36.7(19) . . . 7_556 ?
C8 N4 C9 C10 172.3(15) . . . 7_556 ?
C10 N4 C9 C10 -44(3) . . . 7_556 ?
C10' N4 C9 C10 -74(3) . . . 7_556 ?
C9' N4 C10 C9 -36(2) . . . 7_556 ?
C9 N4 C10 C9 45(3) . . . 7_556 ?
C8 N4 C10 C9 -164.7(18) . . . 7_556 ?
C10' N4 C10 C9 97(3) . . . 7_556 ?
C9 N4 C9' C10' -33(2) . . . 7_556 ?
C8 N4 C9' C10' -167.9(17) . . . 7_556 ?
C10 N4 C9' C10' 83(3) . . . 7_556 ?
C10' N4 C9' C10' 53(4) . . . 7_556 ?
C9' N4 C10' C9' -54(4) . . . 7_556 ?
C9 N4 C10' C9' 29(3) . . . 7_556 ?
C8 N4 C10' C9' 159(2) . . . 7_556 ?
C10 N4 C10' C9' -105(4) . . . 7_556 ?



_diffrn_measured_fraction_theta_max 0.975

_diffrn_reflns_theta_full        60.99

_diffrn_measured_fraction_theta_full 0.975

_refine_diff_density_max         1.559

_refine_diff_density_min         -1.124

_refine_diff_density_rms         0.094



# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.500 0.000 0.014 399 102 ' '
2 1.000 0.500 0.188 399 102 ' '

_platon_squeeze_details          
;

;





# start Validation Reply Form



_vrf_CHEMW03_fe                  
;

PROBLEM: ALERT: The ratio of given/expected molecular weight as

RESPONSE: This is caused by the given molecular weight being increased 

from the atom count to account for half a disordered dimethyl formamide molecule, half a disordered

ethanol molecule and 2 disordered water molecules omitted by SQUEEZE.

;



_vrf_THETM01_fe                  
;

PROBLEM: ALERT: The value of sine(theta_max)/wavelength is less than 0.575

RESPONSE: The crystal diffracted poorly at higher resolution and therefore 

the data were cut at sin(theta_max)/wavelength = 0.5617 and theta = 60.0 deg.

;
_database_code_depnum_ccdc_archive 'CCDC 987373'
#######################################################################
#
#                 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_2-100K



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C24 H32 Au2 Fe N9 O2.50'

_chemical_formula_weight         936.37



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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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                   16.4515(8)

_cell_length_b                   14.2025(7)

_cell_length_c                   14.2637(7)

_cell_angle_alpha                90.00

_cell_angle_beta                 112.0840(10)

_cell_angle_gamma                90.00

_cell_volume                     3088.2(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    100(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       block

_exptl_crystal_colour            red

_exptl_crystal_size_max          0.12

_exptl_crystal_size_mid          0.11

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    2.014

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1772

_exptl_absorpt_coefficient_mu    9.979

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.3806

_exptl_absorpt_correction_T_max  0.4352

_exptl_absorpt_process_details   ?



_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  ?

_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            9928

_diffrn_reflns_av_R_equivalents  0.0424

_diffrn_reflns_av_sigmaI/netI    0.0487

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       21

_diffrn_reflns_limit_k_min       -18

_diffrn_reflns_limit_k_max       18

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       18

_diffrn_reflns_theta_min         3.08

_diffrn_reflns_theta_max         27.48

_reflns_number_total             3504

_reflns_number_gt                2951

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_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)+(0.0341P)²+39.9910P] 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         3504

_refine_ls_number_parameters     198

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0520

_refine_ls_R_factor_gt           0.0434

_refine_ls_wR_factor_ref         0.1023

_refine_ls_wR_factor_gt          0.0971

_refine_ls_goodness_of_fit_ref   1.102

_refine_ls_restrained_S_all      1.102

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group








































Au1 Au 0.73146(2) 0.48067(2) 0.723633(19) 0.03668(12) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.7500 0.5000 0.0226(3) Uani 1 2 d S . .
N1 N 0.7456(4) 0.6430(4) 0.5825(4) 0.0309(13) Uani 1 1 d . . .
N2 N 0.7315(4) 0.3332(4) 0.8868(4) 0.0271(12) Uani 1 1 d . . .
N3 N 0.6201(4) 0.7659(4) 0.4588(4) 0.0280(12) Uani 1 1 d . . .
N4 N 0.3081(5) 0.7742(6) 0.4521(6) 0.058(2) Uani 1 1 d . . .
C1 C 0.7407(5) 0.5800(5) 0.6315(5) 0.0334(16) Uani 1 1 d . . .
C2 C 0.7272(5) 0.3866(5) 0.8233(5) 0.0332(16) Uani 1 1 d . . .
C3 C 0.5597(9) 0.6994(9) 0.4361(10) 0.028(3) Uani 0.507(9) 1 d P A 1
H3A H 0.5797 0.6364 0.4379 0.034 Uiso 0.507(9) 1 calc PR A 1
C4 C 0.4710(9) 0.7114(10) 0.4101(10) 0.031(3) Uani 0.507(9) 1 d P A 1
H4A H 0.4335 0.6579 0.3938 0.037 Uiso 0.507(9) 1 calc PR A 1
C5 C 0.5830(10) 0.8590(8) 0.4490(10) 0.028(3) Uani 0.507(9) 1 d P A 1
H5A H 0.6214 0.9114 0.4604 0.033 Uiso 0.507(9) 1 calc PR A 1
C6 C 0.4940(10) 0.8764(10) 0.4237(10) 0.033(3) Uani 0.507(9) 1 d P A 1
H6A H 0.4707 0.9383 0.4173 0.039 Uiso 0.507(9) 1 calc PR A 1
C3' C 0.5872(11) 0.7545(11) 0.5314(10) 0.034(4) Uani 0.493(9) 1 d P A 2
H3B H 0.6254 0.7383 0.5981 0.041 Uiso 0.493(9) 1 calc PR A 2
C4' C 0.4986(9) 0.7661(11) 0.5102(10) 0.033(4) Uani 0.493(9) 1 d P A 2
H4B H 0.4763 0.7573 0.5622 0.040 Uiso 0.493(9) 1 calc PR A 2
C5' C 0.5684(9) 0.7727(9) 0.3655(9) 0.026(3) Uani 0.493(9) 1 d P A 2
H5B H 0.5928 0.7695 0.3148 0.031 Uiso 0.493(9) 1 calc PR A 2
C6' C 0.4787(10) 0.7846(10) 0.3359(11) 0.034(3) Uani 0.493(9) 1 d P A 2
H6B H 0.4433 0.7877 0.2659 0.041 Uiso 0.493(9) 1 calc PR A 2
C7 C 0.4385(5) 0.7922(6) 0.4075(5) 0.0379(18) Uani 1 1 d . . .
C8 C 0.3418(5) 0.8103(6) 0.3791(6) 0.0415(18) Uani 1 1 d . A .
H8A H 0.3311 0.8790 0.3719 0.050 Uiso 1 1 calc R . .
H8B H 0.3091 0.7810 0.3126 0.050 Uiso 1 1 calc R . .
C9 C 0.2049(10) 0.7569(12) 0.3926(10) 0.035(4) Uani 0.482(13) 1 d P . 1
H9A H 0.1735 0.8179 0.3772 0.042 Uiso 0.482(13) 1 calc PR . 1
H9B H 0.1946 0.7238 0.3280 0.042 Uiso 0.482(13) 1 calc PR . 1
C10 C 0.3289(9) 0.8025(11) 0.5408(11) 0.031(4) Uani 0.482(13) 1 d P . 1
H10A H 0.3067 0.8676 0.5390 0.037 Uiso 0.482(13) 1 calc PR . 1
H10B H 0.3937 0.8051 0.5728 0.037 Uiso 0.482(13) 1 calc PR . 1
C9' C 0.3040(10) 0.6856(11) 0.4760(11) 0.042(4) Uani 0.518(13) 1 d P . 2
H9C H 0.3633 0.6580 0.4953 0.050 Uiso 0.518(13) 1 calc PR . 2
H9D H 0.2650 0.6521 0.4148 0.050 Uiso 0.518(13) 1 calc PR . 2
C10' C 0.2284(10) 0.8336(11) 0.4394(10) 0.039(4) Uani 0.518(13) 1 d P . 2
H10C H 0.1812 0.8193 0.3735 0.047 Uiso 0.518(13) 1 calc PR . 2
H10D H 0.2435 0.9011 0.4398 0.047 Uiso 0.518(13) 1 calc PR . 2






_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



















































Au1 C2 1.971(7) . ?
Au1 C1 1.972(6) . ?
Fe1 N2 1.930(5) 4_656 ?
Fe1 N2 1.930(5) 6_565 ?
Fe1 N1 1.940(6) . ?
Fe1 N1 1.940(6) 7_666 ?
Fe1 N3 2.005(6) 7_666 ?
Fe1 N3 2.005(6) . ?
N1 C1 1.157(9) . ?
N2 C2 1.164(9) . ?
N2 Fe1 1.930(5) 4_646 ?
N3 C5' 1.285(13) . ?
N3 C3 1.320(14) . ?
N3 C3' 1.347(15) . ?
N3 C5 1.441(13) . ?
N4 C10 1.247(16) . ?
N4 C9' 1.311(18) . ?
N4 C8 1.445(10) . ?
N4 C10' 1.512(15) . ?
N4 C9 1.606(17) . ?
C3 C4 1.375(19) . ?
C3 H3A 0.9500 . ?
C4 C7 1.261(16) . ?
C4 H4A 0.9500 . ?
C5 C6 1.39(2) . ?
C5 H5A 0.9500 . ?
C6 C7 1.468(17) . ?
C6 H6A 0.9500 . ?
C3' C4' 1.38(2) . ?
C3' H3B 0.9500 . ?
C4' C7 1.474(15) . ?
C4' H4B 0.9500 . ?
C5' C6' 1.39(2) . ?
C5' H5B 0.9500 . ?
C6' C7 1.413(17) . ?
C6' H6B 0.9500 . ?
C7 C8 1.510(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.52(2) 7_566 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C9 1.52(2) 7_566 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C9' C10' 1.51(2) 7_566 ?
C9' H9C 0.9900 . ?
C9' H9D 0.9900 . ?
C10' C9' 1.51(2) 7_566 ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag








































































































C2 Au1 C1 176.2(3) . . ?
N2 Fe1 N2 180.000(1) 4_656 6_565 ?
N2 Fe1 N1 90.1(2) 4_656 . ?
N2 Fe1 N1 89.9(2) 6_565 . ?
N2 Fe1 N1 89.9(2) 4_656 7_666 ?
N2 Fe1 N1 90.1(2) 6_565 7_666 ?
N1 Fe1 N1 180.000(1) . 7_666 ?
N2 Fe1 N3 90.5(2) 4_656 7_666 ?
N2 Fe1 N3 89.5(2) 6_565 7_666 ?
N1 Fe1 N3 90.7(2) . 7_666 ?
N1 Fe1 N3 89.3(2) 7_666 7_666 ?
N2 Fe1 N3 89.5(2) 4_656 . ?
N2 Fe1 N3 90.5(2) 6_565 . ?
N1 Fe1 N3 89.3(2) . . ?
N1 Fe1 N3 90.7(2) 7_666 . ?
N3 Fe1 N3 180.000(1) 7_666 . ?
C1 N1 Fe1 178.1(7) . . ?
C2 N2 Fe1 174.2(6) . 4_646 ?
C5' N3 C3 69.9(8) . . ?
C5' N3 C3' 120.3(10) . . ?
C3 N3 C3' 67.7(9) . . ?
C5' N3 C5 74.9(8) . . ?
C3 N3 C5 112.3(9) . . ?
C3' N3 C5 84.7(9) . . ?
C5' N3 Fe1 121.9(7) . . ?
C3 N3 Fe1 127.8(7) . . ?
C3' N3 Fe1 116.9(7) . . ?
C5 N3 Fe1 119.9(7) . . ?
C10 N4 C9' 93.8(10) . . ?
C10 N4 C8 125.6(11) . . ?
C9' N4 C8 126.8(10) . . ?
C10 N4 C10' 80.6(10) . . ?
C9' N4 C10' 116.1(11) . . ?
C8 N4 C10' 105.4(8) . . ?
C10 N4 C9 114.8(10) . . ?
C9' N4 C9 81.0(10) . . ?
C8 N4 C9 106.8(7) . . ?
C10' N4 C9 47.6(9) . . ?
N1 C1 Au1 175.0(7) . . ?
N2 C2 Au1 174.6(7) . . ?
N3 C3 C4 127.1(12) . . ?
N3 C3 H3A 116.5 . . ?
C4 C3 H3A 116.5 . . ?
C7 C4 C3 121.0(13) . . ?
C7 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C6 C5 N3 123.6(12) . . ?
C6 C5 H5A 118.2 . . ?
N3 C5 H5A 118.2 . . ?
C5 C6 C7 115.3(11) . . ?
C5 C6 H6A 122.4 . . ?
C7 C6 H6A 122.4 . . ?
N3 C3' C4' 120.8(12) . . ?
N3 C3' H3B 119.6 . . ?
C4' C3' H3B 119.6 . . ?
C3' C4' C7 120.3(12) . . ?
C3' C4' H4B 119.8 . . ?
C7 C4' H4B 119.8 . . ?
N3 C5' C6' 122.6(12) . . ?
N3 C5' H5B 118.7 . . ?
C6' C5' H5B 118.7 . . ?
C5' C6' C7 121.6(12) . . ?
C5' C6' H6B 119.2 . . ?
C7 C6' H6B 119.2 . . ?
C4 C7 C6' 69.1(9) . . ?
C4 C7 C6 120.4(11) . . ?
C6' C7 C6 75.2(9) . . ?
C4 C7 C4' 67.9(9) . . ?
C6' C7 C4' 112.2(10) . . ?
C6 C7 C4' 84.5(10) . . ?
C4 C7 C8 123.7(10) . . ?
C6' C7 C8 123.5(8) . . ?
C6 C7 C8 115.7(9) . . ?
C4' C7 C8 123.7(8) . . ?
N4 C8 C7 113.5(6) . . ?
N4 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
N4 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 N4 108.5(10) 7_566 . ?
C10 C9 H9A 110.0 7_566 . ?
N4 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 7_566 . ?
N4 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N4 C10 C9 115.3(13) . 7_566 ?
N4 C10 H10A 108.4 . . ?
C9 C10 H10A 108.4 7_566 . ?
N4 C10 H10B 108.4 . . ?
C9 C10 H10B 108.4 7_566 . ?
H10A C10 H10B 107.5 . . ?
N4 C9' C10' 116.6(13) . 7_566 ?
N4 C9' H9C 108.1 . . ?
C10' C9' H9C 108.1 7_566 . ?
N4 C9' H9D 108.1 . . ?
C10' C9' H9D 108.1 7_566 . ?
H9C C9' H9D 107.3 . . ?
N4 C10' C9' 110.6(11) . 7_566 ?
N4 C10' H10C 109.5 . . ?
C9' C10' H10C 109.5 7_566 . ?
N4 C10' H10D 109.5 . . ?
C9' C10' H10D 109.5 7_566 . ?
H10C C10' H10D 108.1 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

























































































N2 Fe1 N1 C1 75(17) 4_656 . . . ?
N2 Fe1 N1 C1 -105(17) 6_565 . . . ?
N1 Fe1 N1 C1 0(100) 7_666 . . . ?
N3 Fe1 N1 C1 166(17) 7_666 . . . ?
N3 Fe1 N1 C1 -14(17) . . . . ?
N2 Fe1 N3 C5' 141.0(8) 4_656 . . . ?
N2 Fe1 N3 C5' -39.0(8) 6_565 . . . ?
N1 Fe1 N3 C5' -128.9(8) . . . . ?
N1 Fe1 N3 C5' 51.1(8) 7_666 . . . ?
N3 Fe1 N3 C5' 3(100) 7_666 . . . ?
N2 Fe1 N3 C3 -130.7(8) 4_656 . . . ?
N2 Fe1 N3 C3 49.3(8) 6_565 . . . ?
N1 Fe1 N3 C3 -40.6(8) . . . . ?
N1 Fe1 N3 C3 139.4(8) 7_666 . . . ?
N3 Fe1 N3 C3 91(100) 7_666 . . . ?
N2 Fe1 N3 C3' -49.1(8) 4_656 . . . ?
N2 Fe1 N3 C3' 130.9(8) 6_565 . . . ?
N1 Fe1 N3 C3' 41.0(9) . . . . ?
N1 Fe1 N3 C3' -139.0(9) 7_666 . . . ?
N3 Fe1 N3 C3' 172(100) 7_666 . . . ?
N2 Fe1 N3 C5 50.8(7) 4_656 . . . ?
N2 Fe1 N3 C5 -129.2(7) 6_565 . . . ?
N1 Fe1 N3 C5 140.9(7) . . . . ?
N1 Fe1 N3 C5 -39.1(7) 7_666 . . . ?
N3 Fe1 N3 C5 -88(100) 7_666 . . . ?
Fe1 N1 C1 Au1 -63(21) . . . . ?
C2 Au1 C1 N1 -39(11) . . . . ?
Fe1 N2 C2 Au1 6(12) 4_646 . . . ?
C1 Au1 C2 N2 -34(10) . . . . ?
C5' N3 C3 C4 -66.2(14) . . . . ?
C3' N3 C3 C4 70.9(15) . . . . ?
C5 N3 C3 C4 -3.0(16) . . . . ?
Fe1 N3 C3 C4 178.5(10) . . . . ?
N3 C3 C4 C7 -1(2) . . . . ?
C5' N3 C5 C6 63.5(13) . . . . ?
C3 N3 C5 C6 3.2(15) . . . . ?
C3' N3 C5 C6 -60.0(14) . . . . ?
Fe1 N3 C5 C6 -178.1(9) . . . . ?
N3 C5 C6 C7 0.2(17) . . . . ?
C5' N3 C3' C4' -11.3(19) . . . . ?
C3 N3 C3' C4' -59.1(15) . . . . ?
C5 N3 C3' C4' 57.7(15) . . . . ?
Fe1 N3 C3' C4' 178.6(11) . . . . ?
N3 C3' C4' C7 -1(2) . . . . ?
C3 N3 C5' C6' 57.9(13) . . . . ?
C3' N3 C5' C6' 11.0(18) . . . . ?
C5 N3 C5' C6' -63.3(13) . . . . ?
Fe1 N3 C5' C6' -179.4(9) . . . . ?
N3 C5' C6' C7 2(2) . . . . ?
C3 C4 C7 C6' 62.6(14) . . . . ?
C3 C4 C7 C6 5.3(18) . . . . ?
C3 C4 C7 C4' -63.6(13) . . . . ?
C3 C4 C7 C8 179.7(10) . . . . ?
C5' C6' C7 C4 -66.0(14) . . . . ?
C5' C6' C7 C6 65.4(14) . . . . ?
C5' C6' C7 C4' -12.2(17) . . . . ?
C5' C6' C7 C8 176.6(11) . . . . ?
C5 C6 C7 C4 -4.7(16) . . . . ?
C5 C6 C7 C6' -59.1(12) . . . . ?
C5 C6 C7 C4' 55.6(12) . . . . ?
C5 C6 C7 C8 -179.5(9) . . . . ?
C3' C4' C7 C4 66.0(15) . . . . ?
C3' C4' C7 C6' 11.5(18) . . . . ?
C3' C4' C7 C6 -60.0(15) . . . . ?
C3' C4' C7 C8 -177.3(12) . . . . ?
C10 N4 C8 C7 65.5(13) . . . . ?
C9' N4 C8 C7 -64.2(13) . . . . ?
C10' N4 C8 C7 154.9(9) . . . . ?
C9 N4 C8 C7 -155.4(9) . . . . ?
C4 C7 C8 N4 67.5(12) . . . . ?
C6' C7 C8 N4 153.3(10) . . . . ?
C6 C7 C8 N4 -117.9(10) . . . . ?
C4' C7 C8 N4 -16.9(14) . . . . ?
C10 N4 C9 C10 -49.4(18) . . . 7_566 ?
C9' N4 C9 C10 40.7(13) . . . 7_566 ?
C8 N4 C9 C10 166.5(11) . . . 7_566 ?
C10' N4 C9 C10 -97.7(14) . . . 7_566 ?
C9' N4 C10 C9 -29.0(15) . . . 7_566 ?
C8 N4 C10 C9 -170.9(10) . . . 7_566 ?
C10' N4 C10 C9 86.8(14) . . . 7_566 ?
C9 N4 C10 C9 52.8(18) . . . 7_566 ?
C10 N4 C9' C10' 34.6(14) . . . 7_566 ?
C8 N4 C9' C10' 175.8(10) . . . 7_566 ?
C10' N4 C9' C10' -46.8(17) . . . 7_566 ?
C9 N4 C9' C10' -79.9(13) . . . 7_566 ?
C10 N4 C10' C9' -45.5(13) . . . 7_566 ?
C9' N4 C10' C9' 44.2(18) . . . 7_566 ?
C8 N4 C10' C9' -170.0(11) . . . 7_566 ?
C9 N4 C10' C9' 91.1(15) . . . 7_566 ?



_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        27.48

_diffrn_measured_fraction_theta_full 0.988

_refine_diff_density_max         3.182

_refine_diff_density_min         -3.885

_refine_diff_density_rms         0.207



# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.000 0.000 0.004 371 85 ' '
2 0.500 0.500 0.210 371 85 ' '

_platon_squeeze_details          ?



# start Validation Reply Form



_vrf_CHEMW03_fe                  
;

PROBLEM: ALERT: The ratio of given/expected molecular weight as

RESPONSE: This is caused by the given molecular weight being increased 

from the atom count to account for one disordered dimethyl 

formamide molecule, half a disordered

ethanol molecule and one disordered water molecule omitted by SQUEEZE.

;
_database_code_depnum_ccdc_archive 'CCDC 987374'
#######################################################################
#
#                 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_2-273K



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C24 H32 Au2 Fe N9 O2.50'

_chemical_formula_weight         936.37



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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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                   16.7493(16)

_cell_length_b                   14.8047(14)

_cell_length_c                   14.5137(12)

_cell_angle_alpha                90.00

_cell_angle_beta                 113.493(3)

_cell_angle_gamma                90.00

_cell_volume                     3300.6(5)

_cell_formula_units_Z            4

_cell_measurement_temperature    273(2)

_cell_measurement_reflns_used    ?

_cell_measurement_theta_min      ?

_cell_measurement_theta_max      ?



_exptl_crystal_description       block

_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.12

_exptl_crystal_size_mid          0.11

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.884

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1772

_exptl_absorpt_coefficient_mu    9.337

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.4004

_exptl_absorpt_correction_T_max  0.4553

_exptl_absorpt_process_details   ?



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      273(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  ?

_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            12584

_diffrn_reflns_av_R_equivalents  0.0531

_diffrn_reflns_av_sigmaI/netI    0.0504

_diffrn_reflns_limit_h_min       -20

_diffrn_reflns_limit_h_max       21

_diffrn_reflns_limit_k_min       -19

_diffrn_reflns_limit_k_max       19

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       14

_diffrn_reflns_theta_min         3.06

_diffrn_reflns_theta_max         27.46

_reflns_number_total             3742

_reflns_number_gt                2424

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       ?

_computing_cell_refinement       ?

_computing_data_reduction        ?

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    ?

_computing_publication_material  ?



_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)+(0.0749P)²+30.9692P] 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         3742

_refine_ls_number_parameters     198

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0972

_refine_ls_R_factor_gt           0.0660

_refine_ls_wR_factor_ref         0.1921

_refine_ls_wR_factor_gt          0.1731

_refine_ls_goodness_of_fit_ref   1.125

_refine_ls_restrained_S_all      1.125

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group








































Au1 Au 0.73193(4) 0.47635(4) 0.71878(4) 0.1036(3) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.7500 0.5000 0.0546(5) Uani 1 2 d S . .
N1 N 0.7465(7) 0.6336(7) 0.5823(7) 0.083(3) Uani 1 1 d . . .
N2 N 0.7249(7) 0.3310(7) 0.8708(8) 0.083(3) Uani 1 1 d . . .
N3 N 0.6109(7) 0.7690(7) 0.4577(7) 0.073(2) Uani 1 1 d . . .
N4 N 0.3068(7) 0.7782(9) 0.4538(9) 0.097(4) Uani 1 1 d . . .
C1 C 0.7419(9) 0.5736(9) 0.6323(10) 0.091(4) Uani 1 1 d . . .
C2 C 0.7254(10) 0.3823(9) 0.8131(10) 0.096(4) Uani 1 1 d . . .
C3 C 0.5498(17) 0.7138(16) 0.4356(19) 0.072(7) Uani 0.471(15) 1 d P A 1
H3A H 0.5659 0.6543 0.4315 0.087 Uiso 0.471(15) 1 calc PR A 1
C4 C 0.4631(18) 0.7247(18) 0.416(2) 0.078(8) Uani 0.471(15) 1 d P A 1
H4A H 0.4276 0.6744 0.4075 0.094 Uiso 0.471(15) 1 calc PR A 1
C5 C 0.5742(17) 0.8610(13) 0.4513(18) 0.070(7) Uani 0.471(15) 1 d P A 1
H5A H 0.6121 0.9098 0.4643 0.084 Uiso 0.471(15) 1 calc PR A 1
C6 C 0.4865(16) 0.8792(16) 0.427(2) 0.074(7) Uani 0.471(15) 1 d P A 1
H6A H 0.4647 0.9376 0.4220 0.089 Uiso 0.471(15) 1 calc PR A 1
C3' C 0.5821(17) 0.7502(19) 0.5279(18) 0.090(8) Uani 0.529(15) 1 d P A 2
H3B H 0.6202 0.7293 0.5905 0.108 Uiso 0.529(15) 1 calc PR A 2
C4' C 0.4914(15) 0.762(2) 0.5071(19) 0.097(9) Uani 0.529(15) 1 d P A 2
H4B H 0.4699 0.7459 0.5547 0.116 Uiso 0.529(15) 1 calc PR A 2
C5' C 0.5575(16) 0.7757(16) 0.3643(16) 0.080(7) Uani 0.529(15) 1 d P A 2
H5B H 0.5782 0.7706 0.3139 0.095 Uiso 0.529(15) 1 calc PR A 2
C6' C 0.4684(15) 0.7904(17) 0.3390(17) 0.080(7) Uani 0.529(15) 1 d P A 2
H6B H 0.4314 0.7935 0.2713 0.096 Uiso 0.529(15) 1 calc PR A 2
C7 C 0.4327(8) 0.8007(11) 0.4103(9) 0.083(3) Uani 1 1 d . . .
C8 C 0.3394(9) 0.8199(11) 0.3857(10) 0.094(4) Uani 1 1 d . A .
H8A H 0.3315 0.8847 0.3866 0.113 Uiso 1 1 calc R . .
H8B H 0.3052 0.7988 0.3181 0.113 Uiso 1 1 calc R . .
C9 C 0.206(2) 0.774(3) 0.398(3) 0.115(13) Uani 0.53(2) 1 d P . 1
H9A H 0.1903 0.7549 0.3286 0.138 Uiso 0.53(2) 1 calc PR . 1
H9B H 0.1810 0.8333 0.3966 0.138 Uiso 0.53(2) 1 calc PR . 1
C10 C 0.3332(18) 0.7945(19) 0.549(2) 0.093(9) Uani 0.53(2) 1 d P . 1
H10A H 0.3164 0.8554 0.5581 0.112 Uiso 0.53(2) 1 calc PR . 1
H10B H 0.3963 0.7911 0.5794 0.112 Uiso 0.53(2) 1 calc PR . 1
C9' C 0.3007(19) 0.6880(19) 0.468(2) 0.090(10) Uani 0.47(2) 1 d P . 2
H9C H 0.3572 0.6609 0.4831 0.108 Uiso 0.47(2) 1 calc PR . 2
H9D H 0.2604 0.6620 0.4055 0.108 Uiso 0.47(2) 1 calc PR . 2
C10' C 0.2288(19) 0.839(2) 0.450(2) 0.082(8) Uani 0.47(2) 1 d P . 2
H10C H 0.2465 0.9016 0.4577 0.099 Uiso 0.47(2) 1 calc PR . 2
H10D H 0.1808 0.8319 0.3847 0.099 Uiso 0.47(2) 1 calc PR . 2






_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



















































Au1 C1 1.961(12) . ?
Au1 C2 1.987(13) . ?
Fe1 N1 2.111(9) 7_666 ?
Fe1 N1 2.111(9) . ?
Fe1 N2 2.123(9) 6_565 ?
Fe1 N2 2.123(9) 4_656 ?
Fe1 N3 2.178(10) 7_666 ?
Fe1 N3 2.178(10) . ?
N1 C1 1.168(15) . ?
N2 C2 1.131(15) . ?
N2 Fe1 2.123(9) 4_646 ?
N3 C3 1.25(2) . ?
N3 C5' 1.30(2) . ?
N3 C3' 1.32(3) . ?
N3 C5 1.48(2) . ?
N4 C10 1.29(3) . ?
N4 C9' 1.36(3) . ?
N4 C8 1.444(17) . ?
N4 C9 1.56(4) . ?
N4 C10' 1.57(3) . ?
C3 C4 1.37(4) . ?
C3 H3A 0.9300 . ?
C4 C7 1.22(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.39(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.43(3) . ?
C6 H6A 0.9300 . ?
C3' C4' 1.44(3) . ?
C3' H3B 0.9300 . ?
C4' C7 1.47(3) . ?
C4' H4B 0.9300 . ?
C5' C6' 1.40(3) . ?
C5' H5B 0.9300 . ?
C6' C7 1.39(3) . ?
C6' H6B 0.9300 . ?
C7 C8 1.485(18) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.57(4) 7_566 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C9 1.57(4) 7_566 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9' C10' 1.51(4) 7_566 ?
C9' H9C 0.9700 . ?
C9' H9D 0.9700 . ?
C10' C9' 1.51(4) 7_566 ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag








































































































C1 Au1 C2 176.7(5) . . ?
N1 Fe1 N1 180.0(3) 7_666 . ?
N1 Fe1 N2 90.1(4) 7_666 6_565 ?
N1 Fe1 N2 89.9(4) . 6_565 ?
N1 Fe1 N2 89.9(4) 7_666 4_656 ?
N1 Fe1 N2 90.1(4) . 4_656 ?
N2 Fe1 N2 180.000(2) 6_565 4_656 ?
N1 Fe1 N3 89.9(4) 7_666 7_666 ?
N1 Fe1 N3 90.1(4) . 7_666 ?
N2 Fe1 N3 89.4(4) 6_565 7_666 ?
N2 Fe1 N3 90.6(4) 4_656 7_666 ?
N1 Fe1 N3 90.1(4) 7_666 . ?
N1 Fe1 N3 89.9(4) . . ?
N2 Fe1 N3 90.6(4) 6_565 . ?
N2 Fe1 N3 89.4(4) 4_656 . ?
N3 Fe1 N3 180.0(5) 7_666 . ?
C1 N1 Fe1 174.4(12) . . ?
C2 N2 Fe1 167.1(10) . 4_646 ?
C3 N3 C5' 68.1(16) . . ?
C3 N3 C3' 63.0(17) . . ?
C5' N3 C3' 120.7(17) . . ?
C3 N3 C5 108.0(17) . . ?
C5' N3 C5 76.6(16) . . ?
C3' N3 C5 88.4(15) . . ?
C3 N3 Fe1 131.5(13) . . ?
C5' N3 Fe1 121.3(13) . . ?
C3' N3 Fe1 115.7(12) . . ?
C5 N3 Fe1 120.5(11) . . ?
C10 N4 C9' 92.0(19) . . ?
C10 N4 C8 126.0(18) . . ?
C9' N4 C8 126.6(18) . . ?
C10 N4 C9 114(2) . . ?
C9' N4 C9 85(2) . . ?
C8 N4 C9 106.7(13) . . ?
C10 N4 C10' 82.0(19) . . ?
C9' N4 C10' 117.0(19) . . ?
C8 N4 C10' 105.5(14) . . ?
C9 N4 C10' 44.6(16) . . ?
N1 C1 Au1 177.7(15) . . ?
N2 C2 Au1 176.4(11) . . ?
N3 C3 C4 132(2) . . ?
N3 C3 H3A 114.1 . . ?
C4 C3 H3A 114.1 . . ?
C7 C4 C3 120(2) . . ?
C7 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C6 C5 N3 124(2) . . ?
C6 C5 H5A 117.9 . . ?
N3 C5 H5A 117.9 . . ?
C5 C6 C7 114.5(18) . . ?
C5 C6 H6A 122.7 . . ?
C7 C6 H6A 122.7 . . ?
N3 C3' C4' 120(2) . . ?
N3 C3' H3B 120.2 . . ?
C4' C3' H3B 120.2 . . ?
C3' C4' C7 120(2) . . ?
C3' C4' H4B 120.1 . . ?
C7 C4' H4B 120.1 . . ?
N3 C5' C6' 120(2) . . ?
N3 C5' H5B 119.8 . . ?
C6' C5' H5B 119.8 . . ?
C7 C6' C5' 123.2(19) . . ?
C7 C6' H6B 118.4 . . ?
C5' C6' H6B 118.4 . . ?
C4 C7 C6' 70.3(18) . . ?
C4 C7 C6 121.3(18) . . ?
C6' C7 C6 77.7(15) . . ?
C4 C7 C4' 58.5(17) . . ?
C6' C7 C4' 110.2(16) . . ?
C6 C7 C4' 90.9(18) . . ?
C4 C7 C8 124.1(18) . . ?
C6' C7 C8 124.3(13) . . ?
C6 C7 C8 114.6(15) . . ?
C4' C7 C8 122.8(14) . . ?
N4 C8 C7 113.7(11) . . ?
N4 C8 H8A 108.8 . . ?
C7 C8 H8A 108.8 . . ?
N4 C8 H8B 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N4 C9 C10 110(2) . 7_566 ?
N4 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 7_566 . ?
N4 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 7_566 . ?
H9A C9 H9B 108.1 . . ?
N4 C10 C9 112(3) . 7_566 ?
N4 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 7_566 . ?
N4 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 7_566 . ?
H10A C10 H10B 107.9 . . ?
N4 C9' C10' 116(2) . 7_566 ?
N4 C9' H9C 108.2 . . ?
C10' C9' H9C 108.2 7_566 . ?
N4 C9' H9D 108.2 . . ?
C10' C9' H9D 108.2 7_566 . ?
H9C C9' H9D 107.3 . . ?
C9' C10' N4 110(2) 7_566 . ?
C9' C10' H10C 109.6 7_566 . ?
N4 C10' H10C 109.6 . . ?
C9' C10' H10D 109.6 7_566 . ?
N4 C10' H10D 109.6 . . ?
H10C C10' H10D 108.1 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag

























































































N1 Fe1 N1 C1 -49(100) 7_666 . . . ?
N2 Fe1 N1 C1 -148(11) 6_565 . . . ?
N2 Fe1 N1 C1 32(11) 4_656 . . . ?
N3 Fe1 N1 C1 123(11) 7_666 . . . ?
N3 Fe1 N1 C1 -57(11) . . . . ?
N1 Fe1 N3 C3 142.3(18) 7_666 . . . ?
N1 Fe1 N3 C3 -37.7(18) . . . . ?
N2 Fe1 N3 C3 52.2(18) 6_565 . . . ?
N2 Fe1 N3 C3 -127.8(18) 4_656 . . . ?
N3 Fe1 N3 C3 -41(100) 7_666 . . . ?
N1 Fe1 N3 C5' 54.9(15) 7_666 . . . ?
N1 Fe1 N3 C5' -125.1(15) . . . . ?
N2 Fe1 N3 C5' -35.3(15) 6_565 . . . ?
N2 Fe1 N3 C5' 144.7(15) 4_656 . . . ?
N3 Fe1 N3 C5' -128(100) 7_666 . . . ?
N1 Fe1 N3 C3' -141.9(15) 7_666 . . . ?
N1 Fe1 N3 C3' 38.1(15) . . . . ?
N2 Fe1 N3 C3' 128.0(15) 6_565 . . . ?
N2 Fe1 N3 C3' -52.0(15) 4_656 . . . ?
N3 Fe1 N3 C3' 35(100) 7_666 . . . ?
N1 Fe1 N3 C5 -37.6(12) 7_666 . . . ?
N1 Fe1 N3 C5 142.4(12) . . . . ?
N2 Fe1 N3 C5 -127.7(12) 6_565 . . . ?
N2 Fe1 N3 C5 52.3(12) 4_656 . . . ?
N3 Fe1 N3 C5 139(100) 7_666 . . . ?
Fe1 N1 C1 Au1 5(40) . . . . ?
C2 Au1 C1 N1 -54(36) . . . . ?
Fe1 N2 C2 Au1 -11(31) 4_646 . . . ?
C1 Au1 C2 N2 -17(34) . . . . ?
C5' N3 C3 C4 -73(3) . . . . ?
C3' N3 C3 C4 73(3) . . . . ?
C5 N3 C3 C4 -6(3) . . . . ?
Fe1 N3 C3 C4 174(2) . . . . ?
N3 C3 C4 C7 7(5) . . . . ?
C3 N3 C5 C6 2(3) . . . . ?
C5' N3 C5 C6 63(2) . . . . ?
C3' N3 C5 C6 -59(3) . . . . ?
Fe1 N3 C5 C6 -178.5(18) . . . . ?
N3 C5 C6 C7 1(3) . . . . ?
C3 N3 C3' C4' -56(3) . . . . ?
C5' N3 C3' C4' -18(4) . . . . ?
C5 N3 C3' C4' 56(3) . . . . ?
Fe1 N3 C3' C4' 179(2) . . . . ?
N3 C3' C4' C7 -4(4) . . . . ?
C3 N3 C5' C6' 55(2) . . . . ?
C3' N3 C5' C6' 19(3) . . . . ?
C5 N3 C5' C6' -61(2) . . . . ?
Fe1 N3 C5' C6' -178.2(17) . . . . ?
N3 C5' C6' C7 1(4) . . . . ?
C3 C4 C7 C6' 59(3) . . . . ?
C3 C4 C7 C6 -2(4) . . . . ?
C3 C4 C7 C4' -72(3) . . . . ?
C3 C4 C7 C8 177.5(18) . . . . ?
C5' C6' C7 C4 -64(3) . . . . ?
C5' C6' C7 C6 66(3) . . . . ?
C5' C6' C7 C4' -20(3) . . . . ?
C5' C6' C7 C8 178(2) . . . . ?
C5 C6 C7 C4 -1(3) . . . . ?
C5 C6 C7 C6' -58(2) . . . . ?
C5 C6 C7 C4' 52(2) . . . . ?
C5 C6 C7 C8 179.3(17) . . . . ?
C3' C4' C7 C4 71(3) . . . . ?
C3' C4' C7 C6' 21(4) . . . . ?
C3' C4' C7 C6 -56(3) . . . . ?
C3' C4' C7 C8 -177(2) . . . . ?
C10 N4 C8 C7 63(2) . . . . ?
C9' N4 C8 C7 -64(2) . . . . ?
C9 N4 C8 C7 -159(2) . . . . ?
C10' N4 C8 C7 154.1(17) . . . . ?
C4 C7 C8 N4 58(2) . . . . ?
C6' C7 C8 N4 145.8(19) . . . . ?
C6 C7 C8 N4 -122.6(17) . . . . ?
C4' C7 C8 N4 -14(3) . . . . ?
C10 N4 C9 C10 -53(4) . . . 7_566 ?
C9' N4 C9 C10 37(3) . . . 7_566 ?
C8 N4 C9 C10 163(2) . . . 7_566 ?
C10' N4 C9 C10 -101(3) . . . 7_566 ?
C9' N4 C10 C9 -31(3) . . . 7_566 ?
C8 N4 C10 C9 -170.7(18) . . . 7_566 ?
C9 N4 C10 C9 54(4) . . . 7_566 ?
C10' N4 C10 C9 86(3) . . . 7_566 ?
C10 N4 C9' C10' 36(3) . . . 7_566 ?
C8 N4 C9' C10' 175.1(18) . . . 7_566 ?
C9 N4 C9' C10' -78(3) . . . 7_566 ?
C10' N4 C9' C10' -46(3) . . . 7_566 ?
C10 N4 C10' C9' -44(2) . . . 7_566 ?
C9' N4 C10' C9' 44(3) . . . 7_566 ?
C8 N4 C10' C9' -170(2) . . . 7_566 ?
C9 N4 C10' C9' 92(3) . . . 7_566 ?



_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        27.46

_diffrn_measured_fraction_theta_full 0.991

_refine_diff_density_max         2.105

_refine_diff_density_min         -3.028

_refine_diff_density_rms         0.160



# SQUEEZE RESULTS (APPEND TO CIF)

# Note: Data are Listed for all Voids in the P1 Unit Cell

# i.e. Centre of Gravity, Solvent Accessible Volume,

# Recovered number of Electrons in the Void and

# Details about the Squeezed Material

loop_

_platon_squeeze_void_nr

_platon_squeeze_void_average_x

_platon_squeeze_void_average_y

_platon_squeeze_void_average_z

_platon_squeeze_void_volume

_platon_squeeze_void_count_electrons

_platon_squeeze_void_content


1 0.000 0.000 -0.007 462 64 ' '
2 0.500 0.500 -0.005 462 64 ' '

_platon_squeeze_details          ?



# start Validation Reply Form



_vrf_CHEMW03_fe                  
;

PROBLEM: ALERT: The ratio of given/expected molecular weight as

RESPONSE: This is caused by the given molecular weight being increased 

from the atom count to account for one disordered dimethyl 

formamide molecule, half a disordered

ethanol molecule and one disordered water molecule omitted by SQUEEZE.

;
_database_code_depnum_ccdc_archive 'CCDC 987375'
#######################################################################
#
#                 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_3-150K



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
; 

 ? 

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C20 H20 Fe N8 Ni'

_chemical_formula_weight         487.00



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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_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                   11.5168(11)

_cell_length_b                   10.1374(8)

_cell_length_c                   9.6121(9)

_cell_angle_alpha                90.00

_cell_angle_beta                 103.266(3)

_cell_angle_gamma                90.00

_cell_volume                     1092.27(17)

_cell_formula_units_Z            2

_cell_measurement_temperature    150(2)

_cell_measurement_reflns_used    4472

_cell_measurement_theta_min      3.635

_cell_measurement_theta_max      27.460



_exptl_crystal_description       block

_exptl_crystal_colour            'light yellow'

_exptl_crystal_size_max          0.07

_exptl_crystal_size_mid          0.05

_exptl_crystal_size_min          0.04

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.481

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             500

_exptl_absorpt_coefficient_mu    1.549

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.8993

_exptl_absorpt_correction_T_max  0.9406

_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'



_exptl_special_details           
; 

 ? 

;



_diffrn_ambient_temperature      150(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  'Rigaku R-AXIS SPIDER IP'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            6638

_diffrn_reflns_av_R_equivalents  0.0625

_diffrn_reflns_av_sigmaI/netI    0.0679

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -12

_diffrn_reflns_limit_k_max       12

_diffrn_reflns_limit_l_min       -7

_diffrn_reflns_limit_l_max       11

_diffrn_reflns_theta_min         3.20

_diffrn_reflns_theta_max         26.00

_reflns_number_total             2073

_reflns_number_gt                1329

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'

_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'

_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'

_computing_structure_solution    'Bruker SHELXTL'

_computing_structure_refinement  'Bruker SHELXTL'

_computing_molecular_graphics    'Bruker SHELXTL'

_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)+(0.0411P)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         2073

_refine_ls_number_parameters     139

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0701

_refine_ls_R_factor_gt           0.0396

_refine_ls_wR_factor_ref         0.0989

_refine_ls_wR_factor_gt          0.0846

_refine_ls_goodness_of_fit_ref   0.982

_refine_ls_restrained_S_all      0.982

_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


























Fe1 Fe 1.0000 1.0000 0.5000 0.01708(18) Uani 1 2 d S . .
Ni1 Ni 1.0000 1.0000 0.0000 0.01882(18) Uani 1 2 d S . .
N1 N 1.1616(2) 0.9497(2) 0.4224(3) 0.0214(6) Uani 1 1 d . . .
N2 N 1.4838(2) 0.9592(3) 0.1381(3) 0.0274(7) Uani 1 1 d . . .
N3 N 0.9127(2) 1.0171(2) 0.2725(3) 0.0241(7) Uani 1 1 d . . .
N4 N 1.0430(2) 1.2942(2) 0.0021(3) 0.0244(6) Uani 1 1 d . . .
C1 C 1.1613(3) 0.8435(3) 0.3388(4) 0.0227(8) Uani 1 1 d . . .
H1 H 1.0933 0.7875 0.3211 0.027 Uiso 1 1 calc R . .
C2 C 1.2545(3) 0.8115(3) 0.2772(4) 0.0269(8) Uani 1 1 d . . .
H2 H 1.2499 0.7348 0.2194 0.032 Uiso 1 1 calc R . .
C3 C 1.3549(3) 0.8909(3) 0.2994(4) 0.0254(8) Uani 1 1 d . . .
C4 C 1.3546(3) 1.0028(3) 0.3823(5) 0.0344(9) Uani 1 1 d . . .
H4 H 1.4203 1.0619 0.3979 0.041 Uiso 1 1 calc R . .
C5 C 1.2587(3) 1.0284(3) 0.4424(4) 0.0301(9) Uani 1 1 d . . .
H5 H 1.2612 1.1048 0.5003 0.036 Uiso 1 1 calc R . .
C6 C 1.4588(3) 0.8562(3) 0.2350(4) 0.0340(9) Uani 1 1 d . . .
H6A H 1.5307 0.8425 0.3129 0.041 Uiso 1 1 calc R . .
H6B H 1.4414 0.7723 0.1816 0.041 Uiso 1 1 calc R . .
C7 C 1.5909(3) 0.9237(3) 0.0886(4) 0.0341(9) Uani 1 1 d . . .
H7A H 1.5789 0.8371 0.0398 0.041 Uiso 1 1 calc R . .
H7B H 1.6597 0.9160 0.1716 0.041 Uiso 1 1 calc R . .
C8 C 1.3825(3) 0.9728(3) 0.0137(4) 0.0326(9) Uani 1 1 d . . .
H8A H 1.3101 0.9983 0.0463 0.039 Uiso 1 1 calc R . .
H8B H 1.3669 0.8870 -0.0364 0.039 Uiso 1 1 calc R . .
C9 C 0.9387(3) 1.0147(2) 0.1646(4) 0.0201(7) Uani 1 1 d . . .
C10 C 1.0320(3) 1.1810(3) 0.0031(3) 0.0209(7) Uani 1 1 d . . .






_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



































Fe1 N4 2.144(2) 4_586 ?
Fe1 N4 2.144(2) 2_745 ?
Fe1 N3 2.194(3) 3_776 ?
Fe1 N3 2.194(3) . ?
Fe1 N1 2.217(3) . ?
Fe1 N1 2.217(3) 3_776 ?
Ni1 C10 1.870(3) . ?
Ni1 C10 1.870(3) 3_775 ?
Ni1 C9 1.880(4) . ?
Ni1 C9 1.880(4) 3_775 ?
N1 C1 1.343(4) . ?
N1 C5 1.351(4) . ?
N2 C7 1.466(5) . ?
N2 C6 1.471(4) . ?
N2 C8 1.473(4) . ?
N3 C9 1.144(5) . ?
N4 C10 1.155(4) . ?
N4 Fe1 2.144(2) 2_755 ?
C1 C2 1.378(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.384(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(5) . ?
C3 C6 1.510(5) . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.516(5) 3_875 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C7 1.516(5) 3_875 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag
































































N4 Fe1 N4 180.000(1) 4_586 2_745 ?
N4 Fe1 N3 90.89(10) 4_586 3_776 ?
N4 Fe1 N3 89.11(10) 2_745 3_776 ?
N4 Fe1 N3 89.11(10) 4_586 . ?
N4 Fe1 N3 90.89(10) 2_745 . ?
N3 Fe1 N3 180.0 3_776 . ?
N4 Fe1 N1 90.98(10) 4_586 . ?
N4 Fe1 N1 89.02(10) 2_745 . ?
N3 Fe1 N1 95.10(11) 3_776 . ?
N3 Fe1 N1 84.90(10) . . ?
N4 Fe1 N1 89.02(10) 4_586 3_776 ?
N4 Fe1 N1 90.98(10) 2_745 3_776 ?
N3 Fe1 N1 84.90(10) 3_776 3_776 ?
N3 Fe1 N1 95.10(10) . 3_776 ?
N1 Fe1 N1 180.0 . 3_776 ?
C10 Ni1 C10 180.000(1) . 3_775 ?
C10 Ni1 C9 91.12(13) . . ?
C10 Ni1 C9 88.88(13) 3_775 . ?
C10 Ni1 C9 88.88(13) . 3_775 ?
C10 Ni1 C9 91.12(13) 3_775 3_775 ?
C9 Ni1 C9 180.000(1) . 3_775 ?
C1 N1 C5 116.5(3) . . ?
C1 N1 Fe1 119.9(2) . . ?
C5 N1 Fe1 123.2(2) . . ?
C7 N2 C6 109.4(3) . . ?
C7 N2 C8 109.1(3) . . ?
C6 N2 C8 110.3(3) . . ?
C9 N3 Fe1 138.3(3) . . ?
C10 N4 Fe1 160.3(3) . 2_755 ?
N1 C1 C2 123.4(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 120.2(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 116.9(3) . . ?
C2 C3 C6 120.9(3) . . ?
C4 C3 C6 122.2(3) . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 123.0(3) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
N2 C6 C3 112.5(3) . . ?
N2 C6 H6A 109.1 . . ?
C3 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C3 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N2 C7 C8 110.5(3) . 3_875 ?
N2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 3_875 . ?
N2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 3_875 . ?
H7A C7 H7B 108.1 . . ?
N2 C8 C7 110.6(3) . 3_875 ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 3_875 . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 3_875 . ?
H8A C8 H8B 108.1 . . ?
N3 C9 Ni1 172.5(3) . . ?
N4 C10 Ni1 175.1(3) . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag









































N4 Fe1 N1 C1 -149.4(2) 4_586 . . . ?
N4 Fe1 N1 C1 30.6(2) 2_745 . . . ?
N3 Fe1 N1 C1 119.6(2) 3_776 . . . ?
N3 Fe1 N1 C1 -60.4(2) . . . . ?
N1 Fe1 N1 C1 -108(100) 3_776 . . . ?
N4 Fe1 N1 C5 23.5(3) 4_586 . . . ?
N4 Fe1 N1 C5 -156.5(3) 2_745 . . . ?
N3 Fe1 N1 C5 -67.5(3) 3_776 . . . ?
N3 Fe1 N1 C5 112.5(3) . . . . ?
N1 Fe1 N1 C5 65(100) 3_776 . . . ?
N4 Fe1 N3 C9 84.2(3) 4_586 . . . ?
N4 Fe1 N3 C9 -95.8(3) 2_745 . . . ?
N3 Fe1 N3 C9 11(100) 3_776 . . . ?
N1 Fe1 N3 C9 -6.9(3) . . . . ?
N1 Fe1 N3 C9 173.1(3) 3_776 . . . ?
C5 N1 C1 C2 1.4(5) . . . . ?
Fe1 N1 C1 C2 174.8(3) . . . . ?
N1 C1 C2 C3 -0.4(5) . . . . ?
C1 C2 C3 C4 -1.4(5) . . . . ?
C1 C2 C3 C6 178.9(3) . . . . ?
C2 C3 C4 C5 2.1(5) . . . . ?
C6 C3 C4 C5 -178.2(3) . . . . ?
C1 N1 C5 C4 -0.6(5) . . . . ?
Fe1 N1 C5 C4 -173.7(3) . . . . ?
C3 C4 C5 N1 -1.2(6) . . . . ?
C7 N2 C6 C3 175.7(3) . . . . ?
C8 N2 C6 C3 -64.3(4) . . . . ?
C2 C3 C6 N2 120.0(3) . . . . ?
C4 C3 C6 N2 -59.7(5) . . . . ?
C6 N2 C7 C8 179.0(3) . . . 3_875 ?
C8 N2 C7 C8 58.2(4) . . . 3_875 ?
C7 N2 C8 C7 -58.3(4) . . . 3_875 ?
C6 N2 C8 C7 -178.5(3) . . . 3_875 ?
Fe1 N3 C9 Ni1 19(2) . . . . ?
C10 Ni1 C9 N3 -107(2) . . . . ?
C10 Ni1 C9 N3 73(2) 3_775 . . . ?
C9 Ni1 C9 N3 151(100) 3_775 . . . ?
Fe1 N4 C10 Ni1 16(4) 2_755 . . . ?
C10 Ni1 C10 N4 -16(4) 3_775 . . . ?
C9 Ni1 C10 N4 -71(4) . . . . ?
C9 Ni1 C10 N4 109(4) 3_775 . . . ?



_diffrn_measured_fraction_theta_max 0.966

_diffrn_reflns_theta_full        26.00

_diffrn_measured_fraction_theta_full 0.966

_refine_diff_density_max         0.550

_refine_diff_density_min         -0.483

_refine_diff_density_rms         0.083







#_eof

#End of Crystallographic Information File

_database_code_depnum_ccdc_archive 'CCDC 987376'
