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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_r-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H22 Fe N2 Na O12'
_chemical_formula_weight         441.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'

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

_cell_length_a                   8.3570(12)
_cell_length_b                   8.3570(12)
_cell_length_c                   23.136(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1399.3(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cubic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             687
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.9535
_exptl_absorpt_correction_T_max  1.0414
_exptl_absorpt_process_details   'CrysAlis v171.33.42'

_exptl_special_details           
;
  ?
;

_diffrn_ambient_temperature      293(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  KM4CCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5672
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         4.51
_diffrn_reflns_theta_max         29.58
_reflns_number_total             844
_reflns_number_gt                772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis v171.33.42'
_computing_cell_refinement       'CrysAlis v171.33.42'
_computing_data_reduction        'CrysAlis v171.33.42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.2'
_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)+(0.0150P)²+0.6000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         844
_refine_ls_number_parameters     67
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0520
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.368
_refine_ls_restrained_S_all      1.371
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.048

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
Na1 Na 0.3333 0.6667 0.6667 0.02664(8) Uani 1 6 d S . .
Fe1 Fe 0.6667 0.3333 0.8333 0.02508(3) Uani 1 6 d S . .
O1 O 0.46115(3) 0.31750(3) 0.783893(12) 0.03662(8) Uani 1 1 d . . .
C1 C 0.6667 0.3333 1.12885(4) 0.0602(3) Uani 1 3 d SD . .
C2 C 0.6667 0.3333 1.02411(5) 0.0969(5) Uani 1 3 d SD . .
N1 N 0.59216(13) 0.25217(13) 1.07392(5) 0.0451(3) Uani 0.33 1 d PD . .
O2 O 0.32529(4) 0.42806(4) 0.727524(15) 0.05867(11) Uani 1 1 d . . .
C0 C 0.45383(5) 0.44576(5) 0.756988(18) 0.03652(11) Uani 1 1 d . . .
H0 H 0.5596(7) 0.5687(7) 0.7625(2) 0.0729(18) Uiso 1 1 d . . .
H1 H 0.5591(10) 0.2269(10) 1.1379(3) 0.135(3) Uiso 1 1 d D . .
H2 H 0.5778(14) 0.2360(12) 1.0103(3) 0.178(5) Uiso 1 1 d D . .
H11 H 0.4812(13) 0.2368(18) 1.0698(7) 0.058(5) Uiso 0.33 1 d PD . .
H12 H 0.589(2) 0.1479(15) 1.0687(10) 0.113(7) Uiso 0.33 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Na1 0.02748(10) 0.02748(10) 0.02497(15) 0.000 0.000 0.01374(5)
Fe1 0.02476(3) 0.02476(3) 0.02572(5) 0.000 0.000 0.01238(2)
O1 0.03457(10) 0.03470(10) 0.04071(14) 0.00232(10) -0.00754(10) 0.01739(7)
C1 0.0663(3) 0.0663(3) 0.0480(4) 0.000 0.000 0.03313(17)
C2 0.1225(7) 0.1225(7) 0.0456(5) 0.000 0.000 0.0612(3)
N1 0.0403(4) 0.0361(4) 0.0627(6) -0.0050(4) -0.0096(5) 0.0220(3)
O2 0.05355(13) 0.05677(14) 0.06507(19) 0.01365(14) -0.01887(14) 0.02711(10)
C0 0.03438(14) 0.03587(14) 0.04063(19) 0.00203(15) -0.00231(15) 0.01855(10)

_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.
;
_database_code_depnum_ccdc_archive 'CCDC 1021008'
#######################################################################
#
#                 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_p-1110a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
  ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H22 Fe1 N2 Na1 O12'
_chemical_formula_weight         441.226

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'
Na Na 0.0362 0.0249 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.2617(17)
_cell_length_b                   9.0797(18)
_cell_length_c                   12.293(3)
_cell_angle_alpha                95.37(3)
_cell_angle_beta                 90.43(3)
_cell_angle_gamma                89.91(3)
_cell_volume                     918.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3754
_cell_measurement_theta_min      4.58
_cell_measurement_theta_max      53.46

_exptl_crystal_description       cubic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             458
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_T_max  1.1214
_exptl_absorpt_process_details   'CrysAlis v.171.33.42'
_exptl_special_details           
;
  ?
;

_diffrn_ambient_temperature      110(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  KM4CCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8492
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         26.73
_reflns_number_total             3754
_reflns_number_gt                2907
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis v.171.33.42'
_computing_cell_refinement       'CrysAlis v.171.33.42'
_computing_data_reduction        'CrysAlis v.171.33.42'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.2'
_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)+(0.0500P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3754
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0974
_refine_ls_wR_factor_ref         0.2217
_refine_ls_wR_factor_gt          0.2159
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_restrained_S_all      1.363
_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 0.26415(5) 0.25420(5) 0.25218(3) 0.02281(11) Uani 1 1 d . . .
O1 O 0.3511(3) 0.4540(2) 0.19879(17) 0.0269(6) Uani 1 1 d . . .
O2 O 0.1469(3) 0.2414(2) 0.10989(18) 0.0276(6) Uani 1 1 d . . .
O3 O 0.3757(3) 0.2578(3) 0.39789(17) 0.0282(6) Uani 1 1 d . . .
O4 O 0.0654(3) 0.3457(2) 0.31012(17) 0.0262(6) Uani 1 1 d . . .
O5 O 0.1808(3) 0.0502(2) 0.30612(18) 0.0277(6) Uani 1 1 d . . .
O6 O 0.4646(3) 0.1629(3) 0.19170(18) 0.0281(6) Uani 1 1 d . . .
Na1 Na -0.23526(14) -0.24557(13) 0.24933(9) 0.0227(3) Uani 1 1 d . . .
O7 O -0.1255(3) 0.5192(3) 0.3085(2) 0.0391(7) Uani 1 1 d . . .
O8 O 0.6649(3) -0.0020(3) 0.1915(2) 0.0360(7) Uani 1 1 d . . .
O9 O 0.0054(3) -0.1331(3) 0.3167(2) 0.0374(7) Uani 1 1 d . . .
O10 O 0.5343(3) 0.6327(3) 0.1860(2) 0.0395(7) Uani 1 1 d . . .
O11 O 0.3771(3) 0.2278(3) 0.57972(17) 0.0336(6) Uani 1 1 d . . .
O12 O 0.1211(3) 0.2418(3) -0.06890(19) 0.0398(7) Uani 1 1 d . . .
C1 C 0.2006(4) 0.2595(4) 0.0126(3) 0.0257(8) Uani 1 1 d . . .
C2 C 0.0459(4) -0.0064(4) 0.2850(2) 0.0256(8) Uani 1 1 d . . .
C3 C -0.0054(4) 0.4624(4) 0.2711(3) 0.0294(8) Uani 1 1 d . . .
C4 C 0.4887(4) 0.5103(4) 0.2199(3) 0.0276(8) Uani 1 1 d . . .
C5 C 0.5381(4) 0.0480(4) 0.2280(3) 0.0260(8) Uani 1 1 d . . .
C6 C 0.3085(4) 0.2408(4) 0.4917(3) 0.0287(8) Uani 1 1 d . . .
C7 C 0.7504(4) 0.3441(4) 0.0383(3) 0.0353(9) Uani 1 1 d . . .
H7A H 0.7972 0.3810 0.1062 0.050 Uiso 1 1 calc . . .
H7B H 0.6360 0.3544 0.0419 0.050 Uiso 1 1 calc . . .
H7C H 0.7907 0.3983 -0.0181 0.050 Uiso 1 1 calc . . .
C8 C 0.2778(7) -0.1356(5) 0.0727(4) 0.0615(14) Uani 1 1 d . . .
H8A H 0.2492 -0.0340 0.0847 0.050 Uiso 1 1 calc . . .
H8B H 0.3920 -0.1444 0.0660 0.050 Uiso 1 1 calc . . .
H8C H 0.2428 -0.1859 0.1326 0.050 Uiso 1 1 calc . . .
C9 C 0.2570(5) 0.6124(5) 0.4525(4) 0.0593(13) Uani 1 1 d . . .
H9A H 0.3230 0.5767 0.5081 0.050 Uiso 1 1 calc . . .
H9B H 0.2877 0.5655 0.3834 0.050 Uiso 1 1 calc . . .
H9C H 0.1468 0.5910 0.4658 0.050 Uiso 1 1 calc . . .
C10 C 0.7604(5) 0.1640(4) 0.4499(3) 0.0387(10) Uani 1 1 d . . .
H10A H 0.7032 0.2058 0.3929 0.050 Uiso 1 1 calc . . .
H10B H 0.7305 0.0632 0.4510 0.050 Uiso 1 1 calc . . .
H10C H 0.8735 0.1704 0.4378 0.050 Uiso 1 1 calc . . .
N1 N -0.2093(5) 0.1930(5) 0.0158(3) 0.0574(12) Uani 1 1 d . . .
H1A H -0.1072 0.1845 0.0097 0.050 Uiso 1 1 calc . . .
H1B H -0.2385 0.1459 0.0689 0.050 Uiso 1 1 calc . . .
N2 N 0.7235(5) 0.2389(5) 0.5469(3) 0.0647(13) Uani 1 1 d . . .
H2A H 0.7833 0.2078 0.5965 0.050 Uiso 1 1 calc . . .
H2B H 0.6258 0.2210 0.5623 0.050 Uiso 1 1 calc . . .
H1 H 0.2947 0.3011 -0.0014 0.048 Uiso 1 1 d . . .
H2 H -0.0272 0.0407 0.2532 0.051 Uiso 1 1 d . . .
H3 H 0.0322 0.4987 0.2016 0.078 Uiso 1 1 d . . .
H4 H 0.5520 0.4482 0.2624 0.029 Uiso 1 1 d . . .
H5 H 0.4986 -0.0005 0.2764 0.009 Uiso 1 1 d . . .
H6 H 0.2215 0.2346 0.4913 0.026 Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12

Fe1 0.0258(2) 0.0232(2) 0.01698(19) -0.01114(16) -0.00064(16) -0.00582(18)
O1 0.0304(10) 0.0239(11) 0.0236(10) -0.0129(9) -0.0010(9) -0.0087(9)
O2 0.0278(10) 0.0273(11) 0.0250(11) -0.0123(9) -0.0028(9) -0.0064(9)
O3 0.0310(11) 0.0299(12) 0.0208(10) -0.0123(9) -0.0028(9) -0.0043(10)
O4 0.0255(10) 0.0280(11) 0.0224(10) -0.0127(9) 0.0009(8) -0.0032(9)
O5 0.0279(10) 0.0287(12) 0.0235(10) -0.0130(9) -0.0022(9) -0.0058(9)
O6 0.0291(10) 0.0282(11) 0.0240(11) -0.0133(9) 0.0000(9) -0.0020(9)
Na1 0.0270(5) 0.0215(6) 0.0168(5) -0.0132(4) -0.0001(4) -0.0071(5)
O7 0.0383(13) 0.0349(13) 0.0409(14) -0.0137(11) 0.0037(11) 0.0022(11)
O8 0.0409(12) 0.0317(13) 0.0329(12) -0.0114(11) 0.0086(10) 0.0039(11)
O9 0.0468(13) 0.0287(12) 0.0343(12) -0.0093(10) -0.0117(11) -0.0142(11)
O10 0.0417(13) 0.0287(12) 0.0458(14) -0.0077(11) -0.0061(11) -0.0147(11)
O11 0.0391(12) 0.0422(13) 0.0165(10) -0.0129(10) 0.0009(9) -0.0122(11)
O12 0.0355(12) 0.0533(15) 0.0254(11) -0.0242(11) -0.0042(10) -0.0054(12)
C1 0.0285(14) 0.0226(15) 0.0245(15) -0.0051(13) -0.0007(12) -0.0040(13)
C2 0.0284(14) 0.0272(16) 0.0195(14) -0.0068(13) -0.0017(12) -0.0002(13)
C3 0.0280(15) 0.0343(18) 0.0231(15) -0.0116(14) -0.0020(12) -0.0003(14)
C4 0.0337(15) 0.0279(16) 0.0187(14) -0.0108(13) 0.0007(12) -0.0068(14)
C5 0.0309(15) 0.0253(16) 0.0203(14) -0.0060(13) -0.0007(12) -0.0099(13)
C6 0.0324(15) 0.0243(16) 0.0276(16) -0.0068(14) 0.0008(13) -0.0062(13)
C7 0.0388(17) 0.0313(18) 0.0330(17) -0.0125(15) 0.0008(14) -0.0081(15)
C8 0.087(3) 0.050(2) 0.041(2) -0.0272(19) 0.002(2) 0.002(2)
C9 0.054(2) 0.052(2) 0.063(2) -0.0408(19) -0.009(2) -0.003(2)
C10 0.0423(18) 0.0372(19) 0.0324(17) -0.0181(15) -0.0016(15) -0.0028(16)
N1 0.054(2) 0.062(2) 0.053(2) -0.0121(19) 0.0154(17) -0.0036(19)
N2 0.063(2) 0.071(3) 0.055(2) -0.020(2) -0.0170(18) 0.019(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
Fe1 O4 1.948(2) . ?
Fe1 O6 1.970(2) . ?
Fe1 O2 1.987(2) . ?
Fe1 O3 2.006(2) . ?
Fe1 O1 2.115(2) . ?
Fe1 O5 2.141(2) . ?
O1 C4 1.263(4) . ?
O2 C1 1.303(4) . ?
O3 C6 1.306(4) . ?
O4 C3 1.336(4) . ?
O5 C2 1.244(4) . ?
O6 C5 1.318(4) . ?
Na1 O10 2.297(3) 1_445 ?
Na1 O9 2.346(3) . ?
Na1 O11 2.406(3) 2_556 ?
Na1 O12 2.420(3) 2 ?
Na1 O7 2.487(3) 1_545 ?
Na1 O8 2.521(3) 1_455 ?
O7 C3 1.193(4) . ?
O7 Na1 2.487(3) 1_565 ?
O8 C5 1.214(4) . ?
O8 Na1 2.521(3) 1_655 ?
O9 C2 1.294(4) . ?
O10 C4 1.280(4) . ?
O10 Na1 2.297(3) 1_665 ?
O11 C6 1.233(4) . ?
O11 Na1 2.406(3) 2_556 ?
O12 C1 1.192(4) . ?
O12 Na1 2.420(3) 2 ?
C1 H1 0.8899 . ?
C2 H2 0.8529 . ?
C3 H3 0.9955 . ?
C4 H4 0.9567 . ?
C5 H5 0.8399 . ?
C6 H6 0.7216 . ?
C7 N1 1.414(5) 1_655 ?
C7 H7A 0.9500 . ?
C7 H7B 0.9500 . ?
C7 H7C 0.9500 . ?
C8 N1 1.289(6) 2 ?
C8 H8A 0.9500 . ?
C8 H8B 0.9500 . ?
C8 H8C 0.9500 . ?
C9 N2 1.359(6) 2_666 ?
C9 H9A 0.9500 . ?
C9 H9B 0.9500 . ?
C9 H9C 0.9500 . ?
C10 N2 1.353(5) . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C10 H10C 0.9500 . ?
N1 C8 1.289(6) 2 ?
N1 C7 1.414(5) 1_455 ?
N1 H1A 0.8500 . ?
N1 H1B 0.8500 . ?
N2 C9 1.359(6) 2_666 ?
N2 H2A 0.8500 . ?
N2 H2B 0.8500 . ?

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
O4 Fe1 O6 179.22(10) . . ?
O4 Fe1 O2 84.45(9) . . ?
O6 Fe1 O2 94.89(9) . . ?
O4 Fe1 O3 94.90(9) . . ?
O6 Fe1 O3 85.78(9) . . ?
O2 Fe1 O3 176.95(10) . . ?
O4 Fe1 O1 93.14(9) . . ?
O6 Fe1 O1 86.35(9) . . ?
O2 Fe1 O1 82.70(9) . . ?
O3 Fe1 O1 100.32(9) . . ?
O4 Fe1 O5 87.91(9) . . ?
O6 Fe1 O5 92.60(9) . . ?
O2 Fe1 O5 97.77(9) . . ?
O3 Fe1 O5 79.22(9) . . ?
O1 Fe1 O5 178.89(9) . . ?
C4 O1 Fe1 126.0(2) . . ?
C1 O2 Fe1 129.7(2) . . ?
C6 O3 Fe1 126.8(2) . . ?
C3 O4 Fe1 124.1(2) . . ?
C2 O5 Fe1 125.4(2) . . ?
C5 O6 Fe1 125.1(2) . . ?
O10 Na1 O9 176.99(11) 1_445 . ?
O10 Na1 O11 83.02(10) 1_445 2_556 ?
O9 Na1 O11 96.76(9) . 2_556 ?
O10 Na1 O12 93.74(10) 1_445 2 ?
O9 Na1 O12 86.85(9) . 2 ?
O11 Na1 O12 172.19(10) 2_556 2 ?
O10 Na1 O7 89.92(10) 1_445 1_545 ?
O9 Na1 O7 87.08(10) . 1_545 ?
O11 Na1 O7 84.96(10) 2_556 1_545 ?
O12 Na1 O7 102.18(10) 2 1_545 ?
O10 Na1 O8 92.49(10) 1_445 1_455 ?
O9 Na1 O8 90.51(10) . 1_455 ?
O11 Na1 O8 95.61(9) 2_556 1_455 ?
O12 Na1 O8 77.39(10) 2 1_455 ?
O7 Na1 O8 177.58(9) 1_545 1_455 ?
C3 O7 Na1 122.7(2) . 1_565 ?
C5 O8 Na1 118.9(2) . 1_655 ?
C2 O9 Na1 119.0(2) . . ?
C4 O10 Na1 122.7(2) . 1_665 ?
C6 O11 Na1 122.6(2) . 2_556 ?
C1 O12 Na1 122.8(2) . 2 ?
O12 C1 O2 124.3(3) . . ?
O12 C1 H1 109.9 . . ?
O2 C1 H1 125.1 . . ?
O5 C2 O9 122.2(3) . . ?
O5 C2 H2 120.7 . . ?
O9 C2 H2 116.9 . . ?
O7 C3 O4 123.5(3) . . ?
O7 C3 H3 115.5 . . ?
O4 C3 H3 120.5 . . ?
O1 C4 O10 123.2(3) . . ?
O1 C4 H4 110.6 . . ?
O10 C4 H4 126.2 . . ?
O8 C5 O6 123.4(3) . . ?
O8 C5 H5 113.6 . . ?
O6 C5 H5 122.9 . . ?
O11 C6 O3 127.5(3) . . ?
O11 C6 H6 116.4 . . ?
O3 C6 H6 116.1 . . ?
N1 C7 H7A 109.5 1_655 . ?
N1 C7 H7B 109.5 1_655 . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 1_655 . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 H8A 109.5 2 . ?
N1 C8 H8B 109.5 2 . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 2 . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 2_666 . ?
N2 C9 H9B 109.5 2_666 . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 2_666 . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 N1 C7 111.8(4) 2 1_455 ?
C8 N1 H1A 109.3 2 . ?
C7 N1 H1A 109.3 1_455 . ?
C8 N1 H1B 109.3 2 . ?
C7 N1 H1B 109.3 1_455 . ?
H1A N1 H1B 107.9 . . ?
C10 N2 C9 113.2(4) . 2_666 ?
C10 N2 H2A 108.9 . . ?
C9 N2 H2A 108.9 2_666 . ?
C10 N2 H2B 108.9 . . ?
C9 N2 H2B 108.9 2_666 . ?
H2A N2 H2B 107.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7A O7 0.95 2.75 3.685(4) 168.3 1_655
C7 H7B O1 0.95 3.13 3.936(4) 143.3 .
C7 H7B O6 0.95 3.01 3.535(5) 116.2 .
C7 H7B O10 0.95 3.07 3.535(4) 112.0 .
C7 H7B O10 0.95 3.14 3.632(5) 114.2 2_665
C7 H7C O1 0.95 2.94 3.677(5) 135.8 2_665
C8 H8A O2 0.95 2.63 3.577(5) 175.3 .
C8 H8A O5 0.95 2.82 3.293(5) 111.9 .
C8 H8A O6 0.95 2.76 3.332(5) 119.3 .
C8 H8B O8 0.95 2.95 3.666(6) 132.9 .
C8 H8B O10 0.95 2.86 3.369(6) 114.6 1_545
C8 H8C O9 0.95 3.01 3.762(6) 137.1 .
C9 H9A O3 0.95 3.07 3.674(5) 122.8 2_666
C9 H9A O7 0.95 2.99 3.457(6) 111.8 2_566
C9 H9B O1 0.95 2.46 3.405(5) 175.8 .
C9 H9B O3 0.95 2.91 3.373(5) 111.5 .
C9 H9B O4 0.95 2.80 3.258(5) 110.8 .
C9 H9C O7 0.95 2.99 3.672(5) 130.1 .
C10 H10A O3 0.95 2.75 3.361(4) 123.2 .
C10 H10A O6 0.95 3.15 3.991(4) 148.9 .
C10 H10A O8 0.95 2.99 3.473(4) 113.3 .
C10 H10B O11 0.95 2.78 3.721(5) 170.7 2_656
C10 H10C O4 0.95 2.83 3.555(5) 133.6 1_655
C10 H10C O5 0.95 3.16 3.999(4) 148.4 1_655
N1 H1A O2 0.85 2.46 3.170(4) 141.9 .
N1 H1A O12 0.85 2.21 2.977(5) 150.0 .
N1 H1B O6 0.85 2.89 3.494(4) 130.1 1_455
N1 H1B O8 0.85 2.26 3.104(5) 171.5 1_455
N2 H2A O5 0.85 2.74 3.412(5) 136.7 2_656
N2 H2A O9 0.85 2.18 2.998(5) 161.7 2_656
N2 H2B O3 0.85 2.92 3.409(5) 118.5 .
N2 H2B O11 0.85 2.07 2.896(5) 164.8 .
C1 H1 O10 0.89 2.80 3.501(4) 137.2 2_665
C2 H2 O8 0.85 2.67 3.344(4) 137.3 1_455
C4 H4 O3 0.96 2.91 3.449(4) 116.8 .
C4 H4 O7 0.96 2.78 3.359(4) 119.4 1_655
C5 H5 O5 0.84 2.69 3.110(4) 112.8 .
C5 H5 O11 0.84 3.02 3.664(4) 135.7 2_656
C6 H6 O4 0.72 2.83 3.201(4) 114.8 .

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        26.73
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         2.807
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.172
_database_code_depnum_ccdc_archive 'CCDC 1020996'
