# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Roland Meier'
_publ_contact_author_address     
;
Chemistry
Universty of Erlangen
Egerlandstrasse 1
Erlangen
Bavaria
D-91058
GERMANY
;

_publ_contact_author_email       Roland.Meier@chemie.uni-erlangen.de

_publ_section_title              
;
[FeIII(tmdta)]- - twist boat / half chair conformer
ratio reliably deduced from DFT calculated Raman spectra
;
loop_
_publ_author_name
'Roland Meier'
'Frank W. Heinemann'
'Bernd Kallies'
'Harald Krautscheid'
'Nicolai Lehnert'
;
J.Maigut
;
'Florian Paulat'
'R.Van Eldik'
'Gernot Zahn'

# Attachment 'KFe(tmdta).cif'

data_KFe(tmdta)_CCDC649047
_database_code_depnum_ccdc_archive 'CCDC 649047'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H14 Fe K N2 O8'
_chemical_formula_weight         397.19

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.7684(7)
_cell_length_b                   12.4703(7)
_cell_length_c                   12.8511(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.577(6)
_cell_angle_gamma                90.00
_cell_volume                     1392.93(17)
_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            yellow
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_process_details   'optimized faces with STOE X-SHAPE'

_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  'Stoe IPDS-2T'
_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            12562
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         5.32
_diffrn_reflns_theta_max         29.00
_reflns_number_total             3661
_reflns_number_gt                3395
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Stoe, X-AREA'
_computing_cell_refinement       'Stoe, X-AREA '
_computing_data_reduction        'Stoe, X-AREA'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0267P)^2^+0.6494P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0061(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3661
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0584
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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
Fe Fe 0.747801(16) 0.246580(12) 0.240721(12) 0.00644(6) Uani 1 1 d . . .
O1 O 0.57543(9) 0.20132(7) 0.13725(6) 0.01076(16) Uani 1 1 d . . .
O2 O 0.32886(10) 0.23484(7) 0.07486(7) 0.01532(17) Uani 1 1 d . . .
O3 O 0.69208(9) 0.15083(6) 0.35258(6) 0.01009(15) Uani 1 1 d . . .
O4 O 0.50945(10) 0.10650(7) 0.44878(6) 0.01214(16) Uani 1 1 d . . .
O5 O 0.93283(9) 0.16336(6) 0.22230(6) 0.00986(15) Uani 1 1 d . . .
O6 O 1.17178(9) 0.12226(7) 0.29602(7) 0.01272(17) Uani 1 1 d . . .
O7 O 0.81428(9) 0.36440(6) 0.15284(6) 0.00953(15) Uani 1 1 d . . .
O8 O 1.03287(10) 0.44474(7) 0.12649(7) 0.01307(17) Uani 1 1 d . . .
N1 N 0.56741(11) 0.34517(7) 0.29494(7) 0.00776(17) Uani 1 1 d . . .
N2 N 0.91443(11) 0.32610(7) 0.35963(7) 0.00786(17) Uani 1 1 d . . .
C1 C 0.61907(13) 0.45333(9) 0.33488(9) 0.0102(2) Uani 1 1 d . . .
H1A H 0.5269 0.4955 0.3460 0.012 Uiso 1 1 calc R . .
H1B H 0.6682 0.4901 0.2797 0.012 Uiso 1 1 calc R . .
C2 C 0.73163(13) 0.45527(9) 0.43690(9) 0.0124(2) Uani 1 1 d . . .
H2A H 0.7873 0.5245 0.4399 0.015 Uiso 1 1 calc R . .
H2B H 0.6704 0.4543 0.4963 0.015 Uiso 1 1 calc R . .
C3 C 0.85152(13) 0.36552(9) 0.45492(8) 0.0103(2) Uani 1 1 d . . .
H3A H 0.9384 0.3914 0.5058 0.012 Uiso 1 1 calc R . .
H3B H 0.8045 0.3041 0.4877 0.012 Uiso 1 1 calc R . .
C4 C 0.46026(13) 0.35931(9) 0.19655(8) 0.0103(2) Uani 1 1 d . . .
H4A H 0.4970 0.4187 0.1552 0.012 Uiso 1 1 calc R . .
H4B H 0.3571 0.3788 0.2139 0.012 Uiso 1 1 calc R . .
C5 C 0.44839(13) 0.25695(9) 0.13083(8) 0.0102(2) Uani 1 1 d . . .
C6 C 0.49306(12) 0.28027(9) 0.37156(8) 0.0096(2) Uani 1 1 d . . .
H6A H 0.3831 0.2702 0.3442 0.012 Uiso 1 1 calc R . .
H6B H 0.4985 0.3203 0.4385 0.012 Uiso 1 1 calc R . .
C7 C 0.56755(12) 0.17070(9) 0.39303(8) 0.00853(19) Uani 1 1 d . . .
C8 C 1.02237(13) 0.23695(9) 0.39110(8) 0.0097(2) Uani 1 1 d . . .
H8A H 0.9799 0.1912 0.4433 0.012 Uiso 1 1 calc R . .
H8B H 1.1218 0.2665 0.4244 0.012 Uiso 1 1 calc R . .
C9 C 1.04894(13) 0.16915(9) 0.29630(8) 0.00920(19) Uani 1 1 d . . .
C10 C 0.99270(13) 0.41013(9) 0.30425(8) 0.0102(2) Uani 1 1 d . . .
H10A H 1.1055 0.4012 0.3210 0.012 Uiso 1 1 calc R . .
H10B H 0.9655 0.4816 0.3299 0.012 Uiso 1 1 calc R . .
C11 C 0.94827(13) 0.40533(9) 0.18520(8) 0.00922(19) Uani 1 1 d . . .
K K 0.24392(2) 0.470479(19) -0.001680(17) 0.00892(7) Uani 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
Fe 0.00583(9) 0.00717(9) 0.00625(9) 0.00043(5) 0.00057(6) -0.00002(5)
O1 0.0090(4) 0.0124(4) 0.0103(3) -0.0014(3) -0.0008(3) -0.0002(3)
O2 0.0100(4) 0.0236(4) 0.0117(4) -0.0003(3) -0.0011(3) -0.0023(3)
O3 0.0095(4) 0.0102(4) 0.0111(3) 0.0029(3) 0.0032(3) 0.0015(3)
O4 0.0108(4) 0.0115(4) 0.0146(4) 0.0044(3) 0.0034(3) -0.0008(3)
O5 0.0088(4) 0.0106(4) 0.0100(3) -0.0007(3) 0.0003(3) 0.0018(3)
O6 0.0091(4) 0.0124(4) 0.0165(4) 0.0003(3) 0.0011(3) 0.0023(3)
O7 0.0090(4) 0.0105(4) 0.0089(3) 0.0026(3) 0.0005(3) -0.0008(3)
O8 0.0125(4) 0.0144(4) 0.0133(4) 0.0019(3) 0.0055(3) -0.0014(3)
N1 0.0087(4) 0.0074(4) 0.0071(4) 0.0013(3) 0.0009(3) -0.0002(3)
N2 0.0087(4) 0.0081(4) 0.0069(4) 0.0009(3) 0.0013(3) 0.0005(3)
C1 0.0112(5) 0.0068(4) 0.0126(5) -0.0001(4) 0.0019(4) 0.0006(4)
C2 0.0128(5) 0.0119(5) 0.0124(5) -0.0034(4) 0.0016(4) 0.0014(4)
C3 0.0121(5) 0.0116(5) 0.0073(4) -0.0014(4) 0.0015(4) 0.0002(4)
C4 0.0094(5) 0.0121(5) 0.0091(4) 0.0020(4) -0.0001(4) 0.0022(4)
C5 0.0097(5) 0.0136(5) 0.0076(4) 0.0026(4) 0.0014(4) -0.0014(4)
C6 0.0092(5) 0.0102(5) 0.0101(5) 0.0029(4) 0.0036(4) 0.0010(4)
C7 0.0076(5) 0.0100(5) 0.0076(4) 0.0007(4) -0.0007(3) -0.0006(4)
C8 0.0090(5) 0.0104(5) 0.0089(4) 0.0007(4) -0.0015(4) 0.0019(4)
C9 0.0092(5) 0.0079(4) 0.0106(4) 0.0015(4) 0.0017(4) -0.0007(4)
C10 0.0097(5) 0.0105(5) 0.0101(4) 0.0015(4) 0.0006(4) -0.0028(4)
C11 0.0092(5) 0.0076(4) 0.0109(5) 0.0008(4) 0.0018(4) 0.0013(4)
K 0.00736(12) 0.01089(12) 0.00848(11) 0.00009(7) 0.00094(8) -0.00012(7)

_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
Fe O1 1.9598(8) . ?
Fe O5 1.9663(8) . ?
Fe O3 1.9789(8) . ?
Fe O7 1.9869(8) . ?
Fe N1 2.1886(9) . ?
Fe N2 2.2056(9) . ?
O1 C5 1.3056(14) . ?
O2 C5 1.2219(14) . ?
O2 K 3.1565(10) . ?
O3 C7 1.2937(13) . ?
O3 K 2.9598(8) 4_656 ?
O4 C7 1.2288(13) . ?
O4 K 2.6718(8) 2 ?
O4 K 2.7619(9) 4_656 ?
O5 C9 1.3003(13) . ?
O6 C9 1.2261(14) . ?
O6 K 2.8395(9) 2_655 ?
O7 C11 1.2980(14) . ?
O7 K 2.8306(8) 3_665 ?
O8 C11 1.2283(13) . ?
O8 K 2.6541(8) 1_655 ?
O8 K 2.9248(9) 3_665 ?
N1 C4 1.4831(14) . ?
N1 C6 1.4896(13) . ?
N1 C1 1.4921(14) . ?
N2 C8 1.4813(14) . ?
N2 C10 1.4847(14) . ?
N2 C3 1.4913(13) . ?
C1 C2 1.5338(16) . ?
C2 C3 1.5320(16) . ?
C4 C5 1.5265(16) . ?
C4 K 3.2765(11) . ?
C5 K 3.5213(11) . ?
C6 C7 1.5238(15) . ?
C7 K 3.2105(11) 4_656 ?
C8 C9 1.5259(15) . ?
C8 K 3.4143(11) 2_655 ?
C9 K 3.3948(11) 2_655 ?
C10 C11 1.5293(15) . ?
C11 K 3.1229(11) 3_665 ?
K O8 2.6541(8) 1_455 ?
K O4 2.6718(8) 2_554 ?
K O4 2.7620(9) 4_666 ?
K O7 2.8306(8) 3_665 ?
K O6 2.8395(9) 2_454 ?
K O8 2.9248(9) 3_665 ?
K O3 2.9599(8) 4_666 ?
K C11 3.1229(11) 3_665 ?
K C7 3.2106(11) 4_666 ?
K C9 3.3948(11) 2_454 ?

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

O1 Fe O5 109.94(3) . . ?
O1 Fe O3 94.41(3) . . ?
O5 Fe O3 93.19(3) . . ?
O1 Fe O7 94.88(3) . . ?
O5 Fe O7 90.76(3) . . ?
O3 Fe O7 168.00(3) . . ?
O1 Fe N1 81.53(3) . . ?
O5 Fe N1 167.76(3) . . ?
O3 Fe N1 81.35(3) . . ?
O7 Fe N1 92.53(3) . . ?
O1 Fe N2 168.73(3) . . ?
O5 Fe N2 80.73(3) . . ?
O3 Fe N2 88.42(3) . . ?
O7 Fe N2 81.03(3) . . ?
N1 Fe N2 88.13(3) . . ?
C5 O1 Fe 117.72(7) . . ?
C5 O2 K 97.02(7) . . ?
C7 O3 Fe 118.60(7) . . ?
C7 O3 K 89.05(6) . 4_656 ?
Fe O3 K 152.23(4) . 4_656 ?
C7 O4 K 144.52(7) . 2 ?
C7 O4 K 99.92(7) . 4_656 ?
K O4 K 113.54(3) 2 4_656 ?
C9 O5 Fe 117.49(7) . . ?
C9 O6 K 106.34(7) . 2_655 ?
C11 O7 Fe 115.45(7) . . ?
C11 O7 K 90.43(6) . 3_665 ?
Fe O7 K 152.64(4) . 3_665 ?
C11 O8 K 163.05(8) . 1_655 ?
C11 O8 K 87.52(7) . 3_665 ?
K O8 K 102.24(3) 1_655 3_665 ?
C4 N1 C6 110.18(8) . . ?
C4 N1 C1 108.38(8) . . ?
C6 N1 C1 113.78(8) . . ?
C4 N1 Fe 101.45(6) . . ?
C6 N1 Fe 107.63(6) . . ?
C1 N1 Fe 114.70(7) . . ?
C8 N2 C10 109.97(9) . . ?
C8 N2 C3 108.38(8) . . ?
C10 N2 C3 113.92(8) . . ?
C8 N2 Fe 101.11(6) . . ?
C10 N2 Fe 106.92(6) . . ?
C3 N2 Fe 115.73(7) . . ?
N1 C1 C2 116.12(9) . . ?
C3 C2 C1 117.97(9) . . ?
N2 C3 C2 115.94(9) . . ?
N1 C4 C5 111.20(9) . . ?
N1 C4 K 161.80(7) . . ?
C5 C4 K 86.18(6) . . ?
O2 C5 O1 125.15(11) . . ?
O2 C5 C4 120.33(10) . . ?
O1 C5 C4 114.45(10) . . ?
O2 C5 K 62.83(6) . . ?
O1 C5 K 143.91(7) . . ?
C4 C5 K 68.19(6) . . ?
N1 C6 C7 113.11(8) . . ?
O4 C7 O3 123.11(10) . . ?
O4 C7 C6 119.27(10) . . ?
O3 C7 C6 117.60(9) . . ?
O4 C7 K 57.93(6) . 4_656 ?
O3 C7 K 67.19(6) . 4_656 ?
C6 C7 K 163.71(7) . 4_656 ?
N2 C8 C9 110.93(9) . . ?
N2 C8 K 171.04(7) . 2_655 ?
C9 C8 K 76.34(6) . 2_655 ?
O6 C9 O5 125.09(10) . . ?
O6 C9 C8 119.56(10) . . ?
O5 C9 C8 115.30(9) . . ?
O6 C9 K 53.38(6) . 2_655 ?
O5 C9 K 142.91(7) . 2_655 ?
C8 C9 K 77.77(6) . 2_655 ?
N2 C10 C11 112.27(9) . . ?
O8 C11 O7 123.71(10) . . ?
O8 C11 C10 120.26(10) . . ?
O7 C11 C10 115.87(9) . . ?
O8 C11 K 69.34(6) . 3_665 ?
O7 C11 K 65.01(6) . 3_665 ?
C10 C11 K 140.99(7) . 3_665 ?
O8 K O4 143.63(3) 1_455 2_554 ?
O8 K O4 120.59(3) 1_455 4_666 ?
O4 K O4 66.46(3) 2_554 4_666 ?
O8 K O7 115.88(3) 1_455 3_665 ?
O4 K O7 100.47(3) 2_554 3_665 ?
O4 K O7 77.68(3) 4_666 3_665 ?
O8 K O6 115.44(3) 1_455 2_454 ?
O4 K O6 74.42(3) 2_554 2_454 ?
O4 K O6 123.24(2) 4_666 2_454 ?
O7 K O6 70.71(2) 3_665 2_454 ?
O8 K O8 77.76(3) 1_455 3_665 ?
O4 K O8 133.26(3) 2_554 3_665 ?
O4 K O8 118.63(3) 4_666 3_665 ?
O7 K O8 45.51(2) 3_665 3_665 ?
O6 K O8 64.95(2) 2_454 3_665 ?
O8 K O3 77.19(3) 1_455 4_666 ?
O4 K O3 109.30(2) 2_554 4_666 ?
O4 K O3 45.46(2) 4_666 4_666 ?
O7 K O3 83.87(3) 3_665 4_666 ?
O6 K O3 154.49(2) 2_454 4_666 ?
O8 K O3 98.81(2) 3_665 4_666 ?
O8 K C11 100.23(3) 1_455 3_665 ?
O4 K C11 113.49(3) 2_554 3_665 ?
O4 K C11 102.03(3) 4_666 3_665 ?
O7 K C11 24.56(3) 3_665 3_665 ?
O6 K C11 58.51(3) 2_454 3_665 ?
O8 K C11 23.14(2) 3_665 3_665 ?
O3 K C11 98.59(3) 4_666 3_665 ?
O8 K O2 81.33(3) 1_455 . ?
O4 K O2 64.06(2) 2_554 . ?
O4 K O2 110.49(3) 4_666 . ?
O7 K O2 154.80(2) 3_665 . ?
O6 K O2 85.47(2) 2_454 . ?
O8 K O2 130.70(2) 3_665 . ?
O3 K O2 119.27(2) 4_666 . ?
C11 K O2 141.14(3) 3_665 . ?
O8 K C7 100.68(3) 1_455 4_666 ?
O4 K C7 88.17(3) 2_554 4_666 ?
O4 K C7 22.15(2) 4_666 4_666 ?
O7 K C7 76.62(3) 3_665 4_666 ?
O6 K C7 139.00(3) 2_454 4_666 ?
O8 K C7 107.45(3) 3_665 4_666 ?
O3 K C7 23.76(2) 4_666 4_666 ?
C11 K C7 97.95(3) 3_665 4_666 ?
O2 K C7 120.11(3) . 4_666 ?
O8 K C4 81.14(3) 1_455 . ?
O4 K C4 66.42(3) 2_554 . ?
O4 K C4 73.39(3) 4_666 . ?
O7 K C4 151.03(3) 3_665 . ?
O6 K C4 125.15(3) 2_454 . ?
O8 K C4 158.88(3) 3_665 . ?
O3 K C4 77.13(3) 4_666 . ?
C11 K C4 175.16(3) 3_665 . ?
O2 K C4 43.55(3) . . ?
C7 K C4 77.22(3) 4_666 . ?
O8 K C9 95.19(3) 1_455 2_454 ?
O4 K C9 90.02(3) 2_554 2_454 ?
O4 K C9 143.35(3) 4_666 2_454 ?
O7 K C9 79.70(3) 3_665 2_454 ?
O6 K C9 20.28(2) 2_454 2_454 ?
O8 K C9 57.87(3) 3_665 2_454 ?
O3 K C9 156.66(3) 4_666 2_454 ?
C11 K C9 60.63(3) 3_665 2_454 ?
O2 K C9 80.51(3) . 2_454 ?
C7 K C9 155.50(3) 4_666 2_454 ?
C4 K C9 124.00(3) . 2_454 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.060


# Attachment '{C(NH2)3}Fe(tmdta)2H2O.CIF'

data_C(NH2)3Fe(tmdta)x2H2O_CCDC649048
_database_code_depnum_ccdc_archive 'CCDC 649048'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
guanidinium trimethyldiaminetetracetatoferrate(III) dihydrate
;
_chemical_name_common            
'guanidinium trimethyldiaminetetracetatoferrate(iii) dihydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H24 Fe N5 O10'
_chemical_formula_structural     '[C(NH2)3][Fe(C11H14ON2O8)].2H2O'
_chemical_formula_weight         454.21

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2(1)/c 1'

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

_cell_length_a                   8.8188(4)
_cell_length_b                   10.6119(6)
_cell_length_c                   19.6967(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.060(3)
_cell_angle_gamma                90.00
_cell_volume                     1840.67(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'rod fragment'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.64
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_type   'via psi scans'
_exptl_absorpt_correction_T_min  0.5532
_exptl_absorpt_correction_T_max  0.6017
_exptl_absorpt_process_details   '20 reflections used'

_exptl_special_details           ?

_diffrn_ambient_temperature      298(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  'Stoe STADI4'
_diffrn_measurement_method       omega-theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4445
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0102
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.01
_reflns_number_total             4445
_reflns_number_gt                4134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Stoe STADI4 software'
_computing_cell_refinement       'Stoe STADI4 software'
_computing_data_reduction        'Stoe STADI4 software'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Eight restraints for distances between next and second next neighbours
were used in the refinement to form a minor disorder part showing correct
bond distances and angles.
DFIX 1.49 .002 C7A N2A C8A N2A C10A N2A
DFIX 1.51 .002 C7A C6 C8A C9 C10A C11
DFIX 2.4 .01 C7A C8A C7A C10A

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0540P)^2^+0.8200P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0150(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4445
_refine_ls_number_parameters     273
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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
Fe1 Fe 0.18656(2) 0.46341(2) 0.212144(11) 0.02511(10) Uani 1 1 d . . .
O1 O 0.34391(15) 0.49284(13) 0.14638(7) 0.0374(3) Uani 1 1 d . A .
O2 O 0.58534(18) 0.45775(19) 0.12597(10) 0.0620(5) Uani 1 1 d . A .
O3 O 0.30176(15) 0.53924(12) 0.28905(7) 0.0384(3) Uani 1 1 d . A .
O4 O 0.4478(2) 0.50023(18) 0.38175(8) 0.0554(4) Uani 1 1 d . A .
O5 O 0.03258(13) 0.40603(13) 0.27491(6) 0.0333(3) Uani 1 1 d . A .
O6 O -0.20344(14) 0.33849(15) 0.28395(7) 0.0428(3) Uani 1 1 d . A .
O7 O 0.05182(15) 0.59332(12) 0.16966(7) 0.0364(3) Uani 1 1 d . A .
O8 O -0.09288(18) 0.64264(14) 0.07794(9) 0.0531(4) Uani 1 1 d . A .
O9 O 0.0675(2) 0.40148(15) 0.41604(8) 0.0478(3) Uani 1 1 d G . .
H9O H 0.0498 0.4175 0.3741 0.072 Uiso 1 1 d G . .
H9P H 0.0817 0.3228 0.4215 0.072 Uiso 1 1 d G . .
O10 O 0.6205(2) 0.6078(2) 0.01431(11) 0.0748(6) Uani 1 1 d G . .
H10O H 0.5824 0.5661 0.0461 0.112 Uiso 1 1 d G . .
H10P H 0.7046 0.6397 0.0286 0.112 Uiso 1 1 d G . .
N1 N 0.33431(14) 0.30377(13) 0.23856(7) 0.0259(3) Uani 1 1 d . A .
N2 N 0.0452(2) 0.34463(15) 0.14203(8) 0.0257(3) Uani 0.940(4) 1 d P A -1
N2A N 0.022(3) 0.3358(19) 0.1572(13) 0.026 Uiso 0.060(4) 1 d PD A -2
N3 N 0.2132(2) 0.57618(19) 0.51515(10) 0.0521(5) Uani 1 1 d . . .
H3N H 0.2221 0.5261 0.4813 0.078 Uiso 1 1 calc R . .
H3M H 0.1452 0.5622 0.5439 0.078 Uiso 1 1 calc R . .
N4 N 0.2865(2) 0.75231(18) 0.57470(9) 0.0479(4) Uani 1 1 d . . .
H4N H 0.3436 0.8177 0.5798 0.072 Uiso 1 1 calc R . .
H4M H 0.2181 0.7373 0.6031 0.072 Uiso 1 1 calc R . .
N5 N 0.4081(3) 0.6967(2) 0.47941(10) 0.0593(5) Uani 1 1 d . . .
H5N H 0.4176 0.6470 0.4454 0.089 Uiso 1 1 calc R . .
H5M H 0.4669 0.7610 0.4848 0.089 Uiso 1 1 calc R . .
C1 C 0.46915(19) 0.43005(19) 0.15326(9) 0.0341(4) Uani 1 1 d . . .
C2 C 0.46856(19) 0.31282(18) 0.19656(10) 0.0371(4) Uani 1 1 d . A .
H2A H 0.4710 0.2395 0.1672 0.045 Uiso 1 1 calc R . .
H2B H 0.5599 0.3116 0.2263 0.045 Uiso 1 1 calc R . .
C3 C 0.3789(2) 0.46560(18) 0.32994(10) 0.0369(4) Uani 1 1 d . . .
C4 C 0.3774(2) 0.32651(19) 0.31147(9) 0.0385(4) Uani 1 1 d . A .
H4A H 0.4774 0.2914 0.3220 0.046 Uiso 1 1 calc R . .
H4B H 0.3062 0.2830 0.3391 0.046 Uiso 1 1 calc R . .
C5 C 0.2567(2) 0.17951(16) 0.23160(10) 0.0353(4) Uani 1 1 d . . .
H5A H 0.1709 0.1798 0.2604 0.042 Uiso 1 1 calc R A .
H5B H 0.3265 0.1150 0.2488 0.042 Uiso 1 1 calc R . .
C6 C 0.1995(2) 0.14235(17) 0.16015(11) 0.0421(4) Uani 1 1 d D A .
H6A H 0.2833 0.1025 0.1385 0.050 Uiso 1 1 calc R . .
H6B H 0.1221 0.0784 0.1646 0.050 Uiso 1 1 calc R . .
C7 C 0.1343(2) 0.24150(18) 0.11171(9) 0.0332(5) Uani 0.940(4) 1 d P A -1
H7A H 0.2175 0.2794 0.0887 0.040 Uiso 0.940(4) 1 calc PR A -1
H7B H 0.0694 0.1996 0.0774 0.040 Uiso 0.940(4) 1 calc PR A -1
C7A C 0.0619(18) 0.2103(16) 0.1294(12) 0.033 Uiso 0.060(4) 1 d PD A -2
H7C H 0.0762 0.2207 0.0813 0.040 Uiso 0.060(4) 1 calc PR A -2
H7D H -0.0251 0.1554 0.1335 0.040 Uiso 0.060(4) 1 calc PR A -2
C8 C -0.0864(2) 0.2997(2) 0.17935(10) 0.0355(5) Uani 0.940(4) 1 d P A -1
H8A H -0.0834 0.2084 0.1815 0.043 Uiso 0.940(4) 1 calc PR A -1
H8B H -0.1793 0.3235 0.1539 0.043 Uiso 0.940(4) 1 calc PR A -1
C8A C -0.138(2) 0.328(3) 0.1777(5) 0.036 Uiso 0.060(4) 1 d PD A -2
H8C H -0.1834 0.2455 0.1697 0.043 Uiso 0.060(4) 1 calc PR A -2
H8D H -0.2029 0.3934 0.1577 0.043 Uiso 0.060(4) 1 calc PR A -2
C9 C -0.09127(19) 0.35149(16) 0.25140(9) 0.0306(3) Uani 1 1 d D . .
C10 C -0.0039(4) 0.4332(2) 0.08703(11) 0.0385(5) Uani 0.940(4) 1 d P A -1
H10A H -0.1009 0.4057 0.0666 0.046 Uiso 0.940(4) 1 calc PR A -1
H10B H 0.0694 0.4319 0.0521 0.046 Uiso 0.940(4) 1 calc PR A -1
C10A C 0.008(8) 0.4278(13) 0.1001(16) 0.039 Uiso 0.060(4) 1 d PD A -2
H10C H -0.0746 0.3989 0.0693 0.046 Uiso 0.060(4) 1 calc PR A -2
H10D H 0.1000 0.4216 0.0756 0.046 Uiso 0.060(4) 1 calc PR A -2
C11 C -0.0191(2) 0.56608(18) 0.11311(10) 0.0347(4) Uani 1 1 d D . .
C12 C 0.3040(2) 0.67458(19) 0.52298(9) 0.0396(4) Uani 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 0.02122(13) 0.02502(14) 0.02906(14) -0.00169(8) 0.00088(9) 0.00095(8)
O1 0.0328(6) 0.0385(7) 0.0417(7) 0.0100(6) 0.0088(5) 0.0021(5)
O2 0.0313(7) 0.0882(14) 0.0680(11) 0.0302(9) 0.0158(7) -0.0030(8)
O3 0.0369(7) 0.0342(7) 0.0430(7) -0.0080(5) -0.0077(6) -0.0014(5)
O4 0.0559(9) 0.0657(10) 0.0427(8) -0.0144(8) -0.0153(7) -0.0017(8)
O5 0.0253(5) 0.0445(7) 0.0304(6) -0.0039(5) 0.0037(4) -0.0029(5)
O6 0.0282(6) 0.0538(9) 0.0475(8) 0.0023(6) 0.0108(5) -0.0026(6)
O7 0.0354(6) 0.0293(6) 0.0437(7) -0.0024(5) -0.0046(5) 0.0069(5)
O8 0.0493(8) 0.0403(8) 0.0673(10) 0.0141(7) -0.0188(7) 0.0033(6)
O9 0.0583(9) 0.0459(8) 0.0391(7) -0.0061(6) 0.0010(6) -0.0034(7)
O10 0.0579(11) 0.0875(15) 0.0771(13) 0.0292(11) -0.0161(10) -0.0090(10)
N1 0.0215(6) 0.0258(6) 0.0305(6) 0.0005(5) 0.0021(5) 0.0002(5)
N2 0.0258(8) 0.0269(7) 0.0246(8) -0.0015(6) 0.0027(6) 0.0018(6)
N3 0.0585(11) 0.0516(11) 0.0467(10) -0.0136(8) 0.0075(8) -0.0108(9)
N4 0.0469(9) 0.0516(10) 0.0456(9) -0.0149(8) 0.0075(7) -0.0059(8)
N5 0.0694(13) 0.0672(13) 0.0431(10) -0.0102(9) 0.0205(9) -0.0177(11)
C1 0.0251(7) 0.0427(9) 0.0350(8) 0.0031(7) 0.0054(6) -0.0031(7)
C2 0.0229(7) 0.0378(9) 0.0515(10) 0.0049(8) 0.0098(7) 0.0039(7)
C3 0.0304(8) 0.0440(10) 0.0360(9) -0.0060(7) 0.0000(7) -0.0026(7)
C4 0.0402(9) 0.0412(10) 0.0331(9) 0.0005(7) -0.0067(7) 0.0069(8)
C5 0.0349(8) 0.0245(8) 0.0460(10) 0.0065(7) -0.0018(7) -0.0022(6)
C6 0.0426(10) 0.0272(8) 0.0555(11) -0.0086(8) -0.0058(8) 0.0036(7)
C7 0.0345(10) 0.0317(9) 0.0336(9) -0.0068(7) 0.0041(7) 0.0017(7)
C8 0.0240(9) 0.0445(12) 0.0380(9) -0.0048(8) 0.0024(7) -0.0080(8)
C9 0.0252(7) 0.0316(8) 0.0352(8) 0.0031(6) 0.0025(6) 0.0026(6)
C10 0.0493(13) 0.0388(10) 0.0265(10) 0.0016(8) -0.0074(11) 0.0058(9)
C11 0.0298(8) 0.0337(8) 0.0405(9) 0.0071(7) -0.0003(7) 0.0008(7)
C12 0.0424(10) 0.0431(10) 0.0331(8) -0.0019(7) 0.0010(7) 0.0007(8)

_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 O3 1.9518(13) . ?
Fe1 O1 1.9729(13) . ?
Fe1 O7 1.9765(12) . ?
Fe1 O5 1.9805(12) . ?
Fe1 N1 2.1832(13) . ?
Fe1 N2 2.2058(16) . ?
Fe1 N2A 2.22(2) . ?
O1 C1 1.291(2) . ?
O2 C1 1.218(2) . ?
O3 C3 1.290(2) . ?
O4 C3 1.216(2) . ?
O5 C9 1.299(2) . ?
O6 C9 1.215(2) . ?
O7 C11 1.281(2) . ?
O8 C11 1.231(2) . ?
O9 H9O 0.8501 . ?
O9 H9P 0.8501 . ?
O10 H10O 0.8501 . ?
O10 H10P 0.8500 . ?
N1 C2 1.483(2) . ?
N1 C4 1.485(2) . ?
N1 C5 1.489(2) . ?
N2 C10 1.481(2) . ?
N2 C8 1.486(2) . ?
N2 C7 1.491(2) . ?
N2A C8A 1.490(2) . ?
N2A C7A 1.490(2) . ?
N2A C10A 1.490(2) . ?
N3 C12 1.320(3) . ?
N3 H3N 0.8600 . ?
N3 H3M 0.8600 . ?
N4 C12 1.326(3) . ?
N4 H4N 0.8600 . ?
N4 H4M 0.8600 . ?
N5 C12 1.311(3) . ?
N5 H5N 0.8600 . ?
N5 H5M 0.8600 . ?
C1 C2 1.508(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.520(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.521(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7A 1.510(2) . ?
C6 C7 1.513(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7A H7C 0.9700 . ?
C7A H7D 0.9700 . ?
C8 C9 1.525(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8A C9 1.510(2) . ?
C8A H8C 0.9700 . ?
C8A H8D 0.9700 . ?
C10 C11 1.509(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10A C11 1.511(2) . ?
C10A H10C 0.9700 . ?
C10A 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
O3 Fe1 O1 95.11(6) . . ?
O3 Fe1 O7 108.50(6) . . ?
O1 Fe1 O7 92.27(6) . . ?
O3 Fe1 O5 89.32(5) . . ?
O1 Fe1 O5 171.18(6) . . ?
O7 Fe1 O5 93.55(6) . . ?
O3 Fe1 N1 81.70(5) . . ?
O1 Fe1 N1 81.23(5) . . ?
O7 Fe1 N1 168.47(5) . . ?
O5 Fe1 N1 91.89(5) . . ?
O3 Fe1 N2 167.09(6) . . ?
O1 Fe1 N2 94.20(6) . . ?
O7 Fe1 N2 80.02(6) . . ?
O5 Fe1 N2 80.31(6) . . ?
N1 Fe1 N2 90.91(6) . . ?
O3 Fe1 N2A 158.1(7) . . ?
O1 Fe1 N2A 103.9(6) . . ?
O7 Fe1 N2A 81.7(7) . . ?
O5 Fe1 N2A 70.4(6) . . ?
N1 Fe1 N2A 90.6(7) . . ?
N2 Fe1 N2A 9.9(6) . . ?
C1 O1 Fe1 118.50(11) . . ?
C3 O3 Fe1 118.05(12) . . ?
C9 O5 Fe1 120.39(11) . . ?
C11 O7 Fe1 117.74(12) . . ?
H9O O9 H9P 109.7 . . ?
H10O O10 H10P 109.7 . . ?
C2 N1 C4 110.99(14) . . ?
C2 N1 C5 112.51(14) . . ?
C4 N1 C5 109.00(14) . . ?
C2 N1 Fe1 107.50(10) . . ?
C4 N1 Fe1 102.88(10) . . ?
C5 N1 Fe1 113.55(10) . . ?
C10 N2 C8 111.1(2) . . ?
C10 N2 C7 108.22(16) . . ?
C8 N2 C7 113.89(16) . . ?
C10 N2 Fe1 103.23(14) . . ?
C8 N2 Fe1 107.71(11) . . ?
C7 N2 Fe1 112.22(12) . . ?
C8A N2A C7A 107.2(7) . . ?
C8A N2A C10A 102(4) . . ?
C7A N2A C10A 108.7(6) . . ?
C8A N2A Fe1 120.4(10) . . ?
C7A N2A Fe1 124.1(17) . . ?
C10A N2A Fe1 90(2) . . ?
C12 N3 H3N 120.0 . . ?
C12 N3 H3M 120.0 . . ?
H3N N3 H3M 120.0 . . ?
C12 N4 H4N 120.0 . . ?
C12 N4 H4M 120.0 . . ?
H4N N4 H4M 120.0 . . ?
C12 N5 H5N 120.0 . . ?
C12 N5 H5M 120.0 . . ?
H5N N5 H5M 120.0 . . ?
O2 C1 O1 124.35(18) . . ?
O2 C1 C2 118.48(17) . . ?
O1 C1 C2 117.15(15) . . ?
N1 C2 C1 113.31(14) . . ?
N1 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
O4 C3 O3 124.33(19) . . ?
O4 C3 C4 119.47(19) . . ?
O3 C3 C4 116.17(16) . . ?
N1 C4 C3 112.81(15) . . ?
N1 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N1 C5 C6 116.29(15) . . ?
N1 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N1 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.4 . . ?
C7A C6 C7 31.3(10) . . ?
C7A C6 C5 117.8(9) . . ?
C7 C6 C5 119.94(15) . . ?
C7A C6 H6A 130.3 . . ?
C7 C6 H6A 107.3 . . ?
C5 C6 H6A 107.3 . . ?
C7A C6 H6B 79.4 . . ?
C7 C6 H6B 107.3 . . ?
C5 C6 H6B 107.3 . . ?
H6A C6 H6B 106.9 . . ?
N2 C7 C6 116.65(16) . . ?
N2 C7 H7A 108.1 . . ?
C6 C7 H7A 108.1 . . ?
N2 C7 H7B 108.1 . . ?
C6 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
N2A C7A C6 118.8(18) . . ?
N2A C7A H7C 107.6 . . ?
C6 C7A H7C 107.6 . . ?
N2A C7A H7D 107.6 . . ?
C6 C7A H7D 107.6 . . ?
H7C C7A H7D 107.1 . . ?
N2 C8 C9 113.96(15) . . ?
N2 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N2 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
N2A C8A C9 92.1(13) . . ?
N2A C8A H8C 113.3 . . ?
C9 C8A H8C 113.3 . . ?
N2A C8A H8D 113.3 . . ?
C9 C8A H8D 113.3 . . ?
H8C C8A H8D 110.6 . . ?
O6 C9 O5 123.72(17) . . ?
O6 C9 C8A 107.5(10) . . ?
O5 C9 C8A 126.8(11) . . ?
O6 C9 C8 120.95(16) . . ?
O5 C9 C8 115.31(15) . . ?
C8A C9 C8 20.7(8) . . ?
N2 C10 C11 111.82(16) . . ?
N2 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
N2A C10A C11 121.0(19) . . ?
N2A C10A H10C 107.1 . . ?
C11 C10A H10C 107.1 . . ?
N2A C10A H10D 107.1 . . ?
C11 C10A H10D 107.1 . . ?
H10C C10A H10D 106.8 . . ?
O8 C11 O7 124.01(19) . . ?
O8 C11 C10 118.62(18) . . ?
O7 C11 C10 117.30(16) . . ?
O8 C11 C10A 128.9(18) . . ?
O7 C11 C10A 107.1(18) . . ?
C10 C11 C10A 10.5(15) . . ?
N5 C12 N3 120.45(19) . . ?
N5 C12 N4 120.4(2) . . ?
N3 C12 N4 119.15(19) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.063

# Attachment 'LiFe(tmdta)3H2O.cif'

data_LiFe(tmdta)3H2O_CCDC649049
_database_code_depnum_ccdc_archive 'CCDC 649049'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H14 Fe N2 O8 1-, Li 1+ 3(H2 O)'
_chemical_formula_sum            'C11 H20 Fe Li N2 O11'
_chemical_formula_weight         419.08

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'
Li Li -0.0003 0.0001 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.888(2)
_cell_length_b                   10.284(3)
_cell_length_c                   17.782(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.87(2)
_cell_angle_gamma                90.00
_cell_volume                     1616.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    58
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      12.25

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_type   Psi-scan
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_T_max  0.367
_exptl_absorpt_process_details   
;
North A C T, Phillips, D C, Mathews F S, Acta Cryst. A24 (1968), 351-359.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'Nicolet R3m/V'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        3.89
_diffrn_reflns_number            5652
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         30.00
_reflns_number_total             4713
_reflns_number_gt                3411
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'P3/PC (Siemens Analytical X-Ray Instr., 1989)'
_computing_cell_refinement       'P3/PC (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction        
'XDISK (Siemens Analytical X-Ray Instr. , 1989)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL 5.1 (Bruker AXS, 1998)'

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

Similarity restraints (SADI) have been used in order to reach
agreement between bond length and bond angle data of the
main and disordered part of the structure.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'difmap except PART2 geom'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4713
_refine_ls_number_parameters     312
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.994
_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
Li1 Li 0.7894(5) 0.0714(4) 0.4734(2) 0.0332(9) Uani 1 1 d . A .
Fe1 Fe 1.06114(3) -0.02304(3) 0.205153(16) 0.01917(9) Uani 1 1 d . A .
N1 N 1.19616(18) 0.10188(18) 0.13662(9) 0.0199(3) Uani 1 1 d D . .
N2 N 0.90462(18) 0.13123(18) 0.22821(10) 0.0209(3) Uani 1 1 d . . .
O1 O 1.22616(16) 0.03171(17) 0.28238(8) 0.0274(3) Uani 1 1 d . . .
O2 O 1.47205(18) 0.0768(2) 0.29982(10) 0.0391(4) Uani 1 1 d . . .
O3 O 1.17971(18) -0.15197(16) 0.15362(10) 0.0307(4) Uani 1 1 d . . .
O4 O 1.2493(3) -0.1928(2) 0.03757(15) 0.0475(7) Uani 0.913(6) 1 d PD A 1
O5 O 0.96049(17) -0.10075(16) 0.28994(9) 0.0278(3) Uani 1 1 d . . .
O6 O 0.85943(19) -0.05147(17) 0.39604(9) 0.0329(4) Uani 1 1 d . . .
O7 O 0.89210(17) -0.06331(17) 0.12619(9) 0.0295(4) Uani 1 1 d . . .
O8 O 0.64096(19) -0.0632(2) 0.10439(12) 0.0461(5) Uani 1 1 d . . .
O9 O 0.7557(3) -0.0402(2) 0.55512(11) 0.0459(5) Uani 1 1 d . . .
O10 O 0.6171(2) 0.1729(2) 0.43226(12) 0.0426(5) Uani 1 1 d . . .
O11 O 0.9304(2) 0.2125(2) 0.50168(15) 0.0507(6) Uani 1 1 d . . .
C1 C 1.1535(3) 0.2416(3) 0.12104(15) 0.0281(6) Uani 0.913(6) 1 d PD A 1
C2 C 0.9891(3) 0.2737(3) 0.12667(14) 0.0305(5) Uani 1 1 d D . .
H2C H 0.8939 0.2832 0.0953 0.060 Uiso 0.087(6) 1 calc PR A 2
H2D H 1.0416 0.3560 0.1236 0.060 Uiso 0.087(6) 1 calc PR A 2
C3 C 0.9474(3) 0.2659(2) 0.20731(14) 0.0284(5) Uani 1 1 d . A .
C4 C 1.3536(2) 0.0703(2) 0.25963(12) 0.0254(4) Uani 1 1 d D A .
C5 C 1.3531(3) 0.0984(3) 0.17654(14) 0.0244(6) Uani 0.913(6) 1 d PD A 1
C6 C 1.2117(3) -0.1180(3) 0.08650(15) 0.0332(5) Uani 1 1 d D A .
C7 C 1.1947(5) 0.0246(3) 0.06686(15) 0.0273(8) Uani 0.913(6) 1 d PD A 1
C8 C 0.9051(2) -0.0206(2) 0.33544(12) 0.0247(4) Uani 1 1 d . A .
C9 C 0.9009(3) 0.1213(2) 0.31135(13) 0.0275(5) Uani 1 1 d . A .
C10 C 0.7579(2) -0.0184(2) 0.13546(12) 0.0279(4) Uani 1 1 d . A .
C11 C 0.7531(2) 0.0958(3) 0.18866(15) 0.0304(5) Uani 1 1 d . A .
H1A H 1.182(4) 0.259(4) 0.071(2) 0.060 Uiso 0.913(6) 1 d P A 1
H1B H 1.218(4) 0.293(4) 0.159(2) 0.060 Uiso 0.913(6) 1 d P A 1
H2A H 0.971(4) 0.356(4) 0.107(2) 0.060 Uiso 0.913(6) 1 d P A 1
H2B H 0.919(4) 0.217(4) 0.090(2) 0.060 Uiso 0.913(6) 1 d P A 1
H3A H 1.030(4) 0.293(3) 0.244(2) 0.060 Uiso 1 1 d . . .
H3B H 0.857(4) 0.329(3) 0.2121(19) 0.060 Uiso 1 1 d . . .
H5A H 1.404(4) 0.176(4) 0.169(2) 0.060 Uiso 0.913(6) 1 d P A 1
H5B H 1.408(4) 0.023(4) 0.152(2) 0.060 Uiso 0.913(6) 1 d P A 1
H7A H 1.274(5) 0.044(4) 0.046(2) 0.060 Uiso 0.913(6) 1 d P A 1
H7B H 1.094(4) 0.034(4) 0.037(2) 0.060 Uiso 0.913(6) 1 d P A 1
H9A H 0.985(4) 0.162(4) 0.3325(19) 0.060 Uiso 1 1 d . . .
H9B H 0.814(4) 0.159(3) 0.3277(19) 0.060 Uiso 1 1 d . . .
H9C H 0.747(4) -0.120(4) 0.553(2) 0.060 Uiso 1 1 d . . .
H9D H 0.750(4) -0.027(4) 0.597(2) 0.060 Uiso 1 1 d . . .
H10A H 0.560(4) 0.142(4) 0.401(2) 0.060 Uiso 1 1 d . . .
H10B H 0.614(4) 0.250(4) 0.419(2) 0.060 Uiso 1 1 d . . .
H11A H 0.721(4) 0.161(3) 0.156(2) 0.060 Uiso 1 1 d . . .
H11B H 0.684(4) 0.076(3) 0.225(2) 0.060 Uiso 1 1 d . . .
H11C H 0.942(4) 0.274(4) 0.475(2) 0.060 Uiso 1 1 d . . .
H11D H 1.001(4) 0.198(4) 0.522(2) 0.060 Uiso 1 1 d . . .
O4' O 1.305(2) -0.210(2) 0.0735(16) 0.038(6) Uiso 0.087(6) 1 d PD A 2
C1' C 1.077(2) 0.179(2) 0.0867(11) 0.024(6) Uiso 0.087(6) 1 d PD A 2
H1'A H 1.1279 0.2258 0.0490 0.060 Uiso 0.087(6) 1 calc PR A 2
H1'B H 1.0075 0.1184 0.0601 0.060 Uiso 0.087(6) 1 calc PR A 2
C5' C 1.326(3) 0.149(3) 0.1860(14) 0.043(10) Uiso 0.087(6) 1 d PD A 2
H5'A H 1.3099 0.2397 0.1984 0.060 Uiso 0.087(6) 1 calc PR A 2
H5'B H 1.4159 0.1448 0.1592 0.060 Uiso 0.087(6) 1 calc PR A 2
C7' C 1.218(12) 0.0231(18) 0.070(2) 0.10(4) Uiso 0.087(6) 1 d PD A 2
H7'A H 1.3157 0.0437 0.0534 0.060 Uiso 0.087(6) 1 calc PR A 2
H7'B H 1.1407 0.0447 0.0299 0.060 Uiso 0.087(6) 1 calc PR A 2

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
Li1 0.038(2) 0.035(2) 0.027(2) 0.0058(17) 0.0055(16) 0.0059(18)
Fe1 0.01777(13) 0.02199(15) 0.01820(14) -0.00069(12) 0.00401(9) 0.00049(12)
N1 0.0205(8) 0.0231(9) 0.0162(8) 0.0008(7) 0.0023(6) 0.0011(6)
N2 0.0190(7) 0.0241(9) 0.0200(8) -0.0017(7) 0.0038(6) 0.0008(7)
O1 0.0245(7) 0.0394(9) 0.0184(7) 0.0010(7) 0.0025(6) -0.0043(7)
O2 0.0250(8) 0.0584(12) 0.0321(9) -0.0063(9) -0.0054(7) -0.0010(8)
O3 0.0298(8) 0.0276(9) 0.0366(9) -0.0027(7) 0.0119(7) 0.0014(7)
O4 0.0667(16) 0.0378(12) 0.0424(14) -0.0160(11) 0.0262(13) -0.0030(11)
O5 0.0314(8) 0.0257(8) 0.0284(8) 0.0011(7) 0.0137(7) 0.0006(6)
O6 0.0377(9) 0.0388(10) 0.0242(8) 0.0042(7) 0.0129(7) -0.0002(7)
O7 0.0228(7) 0.0373(9) 0.0285(8) -0.0095(7) 0.0025(6) 0.0011(7)
O8 0.0243(8) 0.0610(13) 0.0521(12) -0.0224(10) -0.0006(8) -0.0056(8)
O9 0.0751(14) 0.0398(12) 0.0245(9) 0.0035(9) 0.0136(9) -0.0021(11)
O10 0.0437(10) 0.0431(12) 0.0381(11) -0.0003(9) -0.0094(8) 0.0071(9)
O11 0.0380(11) 0.0514(14) 0.0635(16) -0.0027(12) 0.0087(10) -0.0045(10)
C1 0.0336(13) 0.0249(13) 0.0272(13) 0.0051(10) 0.0094(10) -0.0006(10)
C2 0.0352(12) 0.0289(12) 0.0283(11) 0.0098(10) 0.0071(9) 0.0077(10)
C3 0.0347(12) 0.0217(11) 0.0303(11) -0.0001(9) 0.0111(9) 0.0018(9)
C4 0.0258(10) 0.0282(11) 0.0220(10) -0.0032(9) 0.0023(8) 0.0013(9)
C5 0.0202(11) 0.0308(15) 0.0222(12) -0.0002(10) 0.0023(9) -0.0052(10)
C6 0.0312(11) 0.0327(13) 0.0379(13) -0.0119(11) 0.0138(10) -0.0078(10)
C7 0.0314(14) 0.0340(16) 0.0174(11) -0.0070(10) 0.0064(9) -0.0075(11)
C8 0.0229(9) 0.0292(11) 0.0222(10) 0.0008(9) 0.0039(7) -0.0017(9)
C9 0.0337(11) 0.0292(12) 0.0211(10) -0.0021(9) 0.0102(9) 0.0016(9)
C10 0.0241(9) 0.0351(12) 0.0247(10) -0.0015(10) 0.0033(8) -0.0024(9)
C11 0.0188(9) 0.0362(13) 0.0358(13) -0.0058(10) 0.0006(9) 0.0012(9)

_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
Li1 O9 1.899(5) . ?
Li1 O10 1.934(5) . ?
Li1 O11 1.948(5) . ?
Li1 O6 2.013(5) . ?
Fe1 O3 1.9763(17) . ?
Fe1 O1 1.9855(16) . ?
Fe1 O7 1.9922(16) . ?
Fe1 O5 1.9970(16) . ?
Fe1 N2 2.1765(18) . ?
Fe1 N1 2.2079(18) . ?
N1 C7' 1.46(2) . ?
N1 C5' 1.463(18) . ?
N1 C7 1.472(3) . ?
N1 C5 1.500(3) . ?
N1 C1 1.505(3) . ?
N1 C1' 1.532(16) . ?
N2 C9 1.486(3) . ?
N2 C3 1.493(3) . ?
N2 C11 1.499(3) . ?
O1 C4 1.303(3) . ?
O2 C4 1.212(3) . ?
O3 C6 1.303(3) . ?
O4 C6 1.233(3) . ?
O5 C8 1.287(3) . ?
O6 C8 1.231(3) . ?
O7 C10 1.305(3) . ?
O8 C10 1.217(3) . ?
O9 H9C 0.83(4) . ?
O9 H9D 0.76(4) . ?
O10 H10A 0.78(4) . ?
O10 H10B 0.83(4) . ?
O11 H11C 0.80(4) . ?
O11 H11D 0.70(4) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.97(4) . ?
C1 H1B 1.00(4) . ?
C2 C1' 1.475(16) . ?
C2 C3 1.520(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 H2A 0.93(4) . ?
C2 H2B 1.04(4) . ?
C3 H3A 0.98(3) . ?
C3 H3B 1.05(3) . ?
C4 C5 1.505(3) . ?
C4 C5' 1.538(18) . ?
C5 H5A 0.93(4) . ?
C5 H5B 1.04(4) . ?
C6 O4' 1.299(16) . ?
C6 C7' 1.48(2) . ?
C6 C7 1.511(4) . ?
C7 H7A 0.86(4) . ?
C7 H7B 1.00(4) . ?
C8 C9 1.521(3) . ?
C9 H9A 0.91(3) . ?
C9 H9B 0.94(3) . ?
C10 C11 1.511(3) . ?
C11 H11A 0.91(4) . ?
C11 H11B 0.95(4) . ?
C1' H1A 1.30(4) . ?
C1' H2B 1.47(4) . ?
C1' H1'A 0.9700 . ?
C1' H1'B 0.9700 . ?
C5' H5A 0.83(4) . ?
C5' H5'A 0.9700 . ?
C5' H5'B 0.9700 . ?
C7' H7A 0.73(7) . ?
C7' H7B 1.20(11) . ?
C7' H7'A 0.9700 . ?
C7' H7'B 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

O9 Li1 O10 115.8(2) . . ?
O9 Li1 O11 113.6(2) . . ?
O10 Li1 O11 99.2(2) . . ?
O9 Li1 O6 103.1(2) . . ?
O10 Li1 O6 111.6(2) . . ?
O11 Li1 O6 114.1(2) . . ?
O3 Fe1 O1 96.88(7) . . ?
O3 Fe1 O7 86.17(7) . . ?
O1 Fe1 O7 175.53(7) . . ?
O3 Fe1 O5 112.51(7) . . ?
O1 Fe1 O5 86.99(7) . . ?
O7 Fe1 O5 94.88(7) . . ?
O3 Fe1 N2 163.29(7) . . ?
O1 Fe1 N2 95.98(7) . . ?
O7 Fe1 N2 80.43(7) . . ?
O5 Fe1 N2 78.77(7) . . ?
O3 Fe1 N1 77.80(7) . . ?
O1 Fe1 N1 79.16(6) . . ?
O7 Fe1 N1 98.35(7) . . ?
O5 Fe1 N1 163.80(7) . . ?
N2 Fe1 N1 94.23(7) . . ?
C7' N1 C5' 120(5) . . ?
C7' N1 C7 8(5) . . ?
C5' N1 C7 128.6(18) . . ?
C7' N1 C5 100(4) . . ?
C5' N1 C5 23.6(17) . . ?
C7 N1 C5 108.3(2) . . ?
C7' N1 C1 115.7(16) . . ?
C5' N1 C1 87.8(14) . . ?
C7 N1 C1 112.3(2) . . ?
C5 N1 C1 108.3(2) . . ?
C7' N1 C1' 88(3) . . ?
C5' N1 C1' 129.1(16) . . ?
C7 N1 C1' 81.1(7) . . ?
C5 N1 C1' 147.1(10) . . ?
C1 N1 C1' 41.5(9) . . ?
C7' N1 Fe1 104(2) . . ?
C5' N1 Fe1 107.7(9) . . ?
C7 N1 Fe1 101.08(15) . . ?
C5 N1 Fe1 104.87(13) . . ?
C1 N1 Fe1 121.08(14) . . ?
C1' N1 Fe1 103.9(9) . . ?
C9 N2 C3 110.09(18) . . ?
C9 N2 C11 109.86(18) . . ?
C3 N2 C11 110.37(18) . . ?
C9 N2 Fe1 102.54(13) . . ?
C3 N2 Fe1 116.45(13) . . ?
C11 N2 Fe1 107.17(13) . . ?
C4 O1 Fe1 118.40(13) . . ?
C6 O3 Fe1 114.94(16) . . ?
C8 O5 Fe1 116.61(14) . . ?
C8 O6 Li1 126.1(2) . . ?
C10 O7 Fe1 118.06(14) . . ?
Li1 O9 H9C 126(3) . . ?
Li1 O9 H9D 132(3) . . ?
H9C O9 H9D 102(4) . . ?
Li1 O10 H10A 119(3) . . ?
Li1 O10 H10B 129(2) . . ?
H10A O10 H10B 101(3) . . ?
Li1 O11 H11C 124(3) . . ?
Li1 O11 H11D 119(3) . . ?
H11C O11 H11D 108(4) . . ?
N1 C1 C2 115.1(2) . . ?
N1 C1 H1A 105(2) . . ?
C2 C1 H1A 111(2) . . ?
N1 C1 H1B 105(2) . . ?
C2 C1 H1B 109(2) . . ?
H1A C1 H1B 110(3) . . ?
C1' C2 C1 42.2(9) . . ?
C1' C2 C3 127.8(8) . . ?
C1 C2 C3 112.5(2) . . ?
C1' C2 H2C 105.3 . . ?
C1 C2 H2C 141.0 . . ?
C3 C2 H2C 105.3 . . ?
C1' C2 H2D 105.3 . . ?
C1 C2 H2D 73.4 . . ?
C3 C2 H2D 105.3 . . ?
H2C C2 H2D 106.0 . . ?
C1' C2 H2A 120(2) . . ?
C1 C2 H2A 108(2) . . ?
C3 C2 H2A 110(2) . . ?
H2C C2 H2A 65.3 . . ?
H2D C2 H2A 41.0 . . ?
C1' C2 H2B 69(2) . . ?
C1 C2 H2B 111(2) . . ?
C3 C2 H2B 112(2) . . ?
H2C C2 H2B 42.3 . . ?
H2D C2 H2B 135.7 . . ?
H2A C2 H2B 102(3) . . ?
N2 C3 C2 112.13(19) . . ?
N2 C3 H3A 107(2) . . ?
C2 C3 H3A 112(2) . . ?
N2 C3 H3B 109.8(18) . . ?
C2 C3 H3B 108.0(19) . . ?
H3A C3 H3B 108(3) . . ?
O2 C4 O1 124.3(2) . . ?
O2 C4 C5 118.9(2) . . ?
O1 C4 C5 116.62(18) . . ?
O2 C4 C5' 121.6(9) . . ?
O1 C4 C5' 111.0(11) . . ?
C5 C4 C5' 22.9(16) . . ?
N1 C5 C4 112.23(19) . . ?
N1 C5 H5A 111(2) . . ?
C4 C5 H5A 110(2) . . ?
N1 C5 H5B 106(2) . . ?
C4 C5 H5B 108(2) . . ?
H5A C5 H5B 109(3) . . ?
O4 C6 O4' 36.2(12) . . ?
O4 C6 O3 125.4(3) . . ?
O4' C6 O3 99.8(12) . . ?
O4 C6 C7' 117.1(11) . . ?
O4' C6 C7' 130(4) . . ?
O3 C6 C7' 117.1(9) . . ?
O4 C6 C7 118.0(2) . . ?
O4' C6 C7 136.0(11) . . ?
O3 C6 C7 116.5(2) . . ?
C7' C6 C7 8(4) . . ?
N1 C7 C6 109.7(2) . . ?
N1 C7 H7A 108(3) . . ?
C6 C7 H7A 105(3) . . ?
N1 C7 H7B 109(2) . . ?
C6 C7 H7B 106(2) . . ?
H7A C7 H7B 118(3) . . ?
O6 C8 O5 124.5(2) . . ?
O6 C8 C9 119.5(2) . . ?
O5 C8 C9 115.94(18) . . ?
N2 C9 C8 110.10(18) . . ?
N2 C9 H9A 106(2) . . ?
C8 C9 H9A 110(2) . . ?
N2 C9 H9B 113(2) . . ?
C8 C9 H9B 108(2) . . ?
H9A C9 H9B 110(3) . . ?
O8 C10 O7 123.9(2) . . ?
O8 C10 C11 120.1(2) . . ?
O7 C10 C11 116.04(19) . . ?
N2 C11 C10 113.63(18) . . ?
N2 C11 H11A 109(2) . . ?
C10 C11 H11A 102(2) . . ?
N2 C11 H11B 110(2) . . ?
C10 C11 H11B 108(2) . . ?
H11A C11 H11B 113(3) . . ?
C2 C1' N1 115.5(12) . . ?
C2 C1' H1A 97(2) . . ?
N1 C1' H1A 89(2) . . ?
C2 C1' H2B 41.2(16) . . ?
N1 C1' H2B 136(2) . . ?
H1A C1' H2B 124(3) . . ?
C2 C1' H1'A 108.4 . . ?
N1 C1' H1'A 108.4 . . ?
H1A C1' H1'A 30.9 . . ?
H2B C1' H1'A 114.3 . . ?
C2 C1' H1'B 108.4 . . ?
N1 C1' H1'B 108.4 . . ?
H1A C1' H1'B 137.9 . . ?
H2B C1' H1'B 67.8 . . ?
H1'A C1' H1'B 107.5 . . ?
N1 C5' C4 112.4(14) . . ?
N1 C5' H5A 122(4) . . ?
C4 C5' H5A 114(4) . . ?
N1 C5' H5'A 109.1 . . ?
C4 C5' H5'A 109.1 . . ?
H5A C5' H5'A 85.3 . . ?
N1 C5' H5'B 109.1 . . ?
C4 C5' H5'B 109.1 . . ?
H5A C5' H5'B 22.9 . . ?
H5'A C5' H5'B 107.9 . . ?
N1 C7' C6 112.2(16) . . ?
N1 C7' H7A 119(7) . . ?
C6 C7' H7A 117(7) . . ?
N1 C7' H7B 99(5) . . ?
C6 C7' H7B 98(5) . . ?
H7A C7' H7B 109(8) . . ?
N1 C7' H7'A 109.2 . . ?
C6 C7' H7'A 109.2 . . ?
H7A C7' H7'A 20.3 . . ?
H7B C7' H7'A 128.9 . . ?
N1 C7' H7'B 109.2 . . ?
C6 C7' H7'B 109.2 . . ?
H7A C7' H7'B 87.6 . . ?
H7B C7' H7'B 21.0 . . ?
H7'A C7' H7'B 107.9 . . ?

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
O9 H9C O4 0.83(4) 1.94(4) 2.764(3) 172(4) 4_556
O9 H9C O4' 0.83(4) 1.84(4) 2.62(2) 155(4) 4_556
O9 H9D O1 0.76(4) 2.13(4) 2.879(3) 165(4) 3_756
O10 H10A O2 0.78(4) 2.00(4) 2.750(3) 160(4) 1_455
O10 H10B O7 0.83(4) 2.07(4) 2.903(3) 174(4) 2_655
O11 H11C O8 0.80(4) 2.27(4) 3.006(3) 154(3) 2_655
O11 H11C O4' 0.80(4) 2.49(4) 2.929(18) 115(3) 2_755
O11 H11D O6 0.70(4) 2.36(4) 2.974(3) 147(4) 3_756

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.079

# Attachment 'NH4Fe(tmdta)x0.5H2O.cif'

data_NH4Fe(tmdta)x0.5H2O_CCDC649050
_database_code_depnum_ccdc_archive 'CCDC 649050'

_audit_creation_date             2007-08-06T13:23:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C11 H14 Fe N2 O8, H4 N, 0.5 (H2 O)'
_chemical_formula_sum            'C11 H19 Fe N3 O8.50'
_chemical_formula_weight         385.14
_chemical_compound_source        'synthesis as described'

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6446(13)
_cell_length_b                   11.0545(10)
_cell_length_c                   16.837(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.859(9)
_cell_angle_gamma                90
_cell_volume                     1562.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      9.821
_cell_measurement_theta_max      15.726
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       cube
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_correction_T_min  0.5045
_exptl_absorpt_correction_T_max  0.8764

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_orient_matrix_type       
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_ub_11      0.078776
_diffrn_orient_matrix_ub_12      0.058701
_diffrn_orient_matrix_ub_13      -0.012829
_diffrn_orient_matrix_ub_21      0.047604
_diffrn_orient_matrix_ub_22      0.011409
_diffrn_orient_matrix_ub_23      0.059951
_diffrn_orient_matrix_ub_31      0.075913
_diffrn_orient_matrix_ub_32      -0.06795
_diffrn_orient_matrix_ub_33      -0.001055
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         3
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        3
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 0 -4
1 -2 3
-2 -3 -2

_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_number            7134
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             3573
_reflns_number_gt                2094
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

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

Water solvent molecule disordered over two sites with occupancies 0.5.
22 restraints are applied in the model for this water molcule
and the terahedral NH4 cation
(SADI O91 H91 O91 H92;
SADI N3 H1 N3 H2 N3 H3 N3 H4;
SADI H1 H2 H1 H3 H1 H4 H2 H3 H2 H4 H3 H4)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.1653P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef       0.0020(7)
_refine_ls_number_reflns         3573
_refine_ls_number_parameters     236
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.077

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

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5091(4) 1.0594(3) 0.7775(2) 0.0411(8) Uani 1 1 d . . .
H1A H 0.4326 1.1237 0.7589 0.049 Uiso 1 1 calc R . .
H1B H 0.5813 1.0582 0.7414 0.049 Uiso 1 1 calc R . .
C2 C 0.6048(4) 1.0906(3) 0.8634(2) 0.0444(9) Uani 1 1 d . . .
H2A H 0.5322 1.1282 0.8919 0.053 Uiso 1 1 calc R . .
H2B H 0.6822 1.1517 0.858 0.053 Uiso 1 1 calc R . .
C3 C 0.6942(4) 0.9912(3) 0.9189(2) 0.0396(8) Uani 1 1 d . . .
H3A H 0.7818 1.028 0.9585 0.048 Uiso 1 1 calc R . .
H3B H 0.6227 0.9559 0.949 0.048 Uiso 1 1 calc R . .
C11 C 0.3126(5) 0.7868(4) 0.6611(2) 0.0516(10) Uani 1 1 d . . .
C12 C 0.3388(4) 0.9213(3) 0.6804(2) 0.0460(9) Uani 1 1 d . . .
H12A H 0.4029 0.9557 0.646 0.055 Uiso 1 1 calc R . .
H12B H 0.2368 0.9625 0.6681 0.055 Uiso 1 1 calc R . .
C21 C 0.3365(4) 0.8317(3) 0.8813(2) 0.0351(7) Uani 1 1 d . . .
C22 C 0.3050(4) 0.9352(3) 0.8212(2) 0.0374(8) Uani 1 1 d . . .
H22A H 0.1984 0.9269 0.7865 0.045 Uiso 1 1 calc R . .
H22B H 0.3089 1.0106 0.8512 0.045 Uiso 1 1 calc R . .
C31 C 0.8399(4) 0.8812(3) 0.7431(2) 0.0358(7) Uani 1 1 d . . .
C32 C 0.8732(4) 0.9364(3) 0.8286(2) 0.0399(8) Uani 1 1 d . . .
H32A H 0.981 0.9163 0.8579 0.048 Uiso 1 1 calc R . .
H32B H 0.8655 1.0237 0.824 0.048 Uiso 1 1 calc R . .
C41 C 0.8369(5) 0.6745(3) 0.9025(3) 0.0493(10) Uani 1 1 d . . .
C42 C 0.8392(4) 0.8011(3) 0.9381(2) 0.0455(9) Uani 1 1 d . . .
H42A H 0.786 0.7999 0.9827 0.055 Uiso 1 1 calc R . .
H42B H 0.9488 0.8256 0.9603 0.055 Uiso 1 1 calc R . .
Fe1 Fe 0.57517(6) 0.78289(4) 0.79401(3) 0.03807(17) Uani 1 1 d . . .
N1 N 0.4209(3) 0.9414(2) 0.76876(16) 0.0322(6) Uani 1 1 d . . .
N2 N 0.7595(3) 0.8919(2) 0.87597(16) 0.0319(6) Uani 1 1 d . . .
N3 N 0.7656(6) 0.8900(3) 0.5360(2) 0.0820(15) Uani 1 1 d D . .
O11 O 0.4078(3) 0.7134(2) 0.70765(17) 0.0569(7) Uani 1 1 d . . .
O12 O 0.2067(4) 0.7556(3) 0.60198(18) 0.0740(9) Uani 1 1 d . . .
O21 O 0.4565(3) 0.76255(19) 0.88086(15) 0.0431(6) Uani 1 1 d . . .
O22 O 0.2470(3) 0.8170(2) 0.92742(16) 0.0529(7) Uani 1 1 d . . .
O31 O 0.6995(3) 0.8358(2) 0.71468(14) 0.0417(6) Uani 1 1 d . . .
O32 O 0.9433(3) 0.8851(2) 0.70468(15) 0.0488(6) Uani 1 1 d . . .
O41 O 0.7258(3) 0.6523(2) 0.83853(19) 0.0541(7) Uani 1 1 d . . .
O42 O 0.9348(4) 0.5989(2) 0.9371(2) 0.0738(9) Uani 1 1 d . . .
O91 O 0.0374(8) 0.9112(5) 0.4993(4) 0.0641(17) Uani 0.5 1 d PD . .
H1 H 0.823(4) 0.872(3) 0.5834(16) 0.096 Uiso 1 1 d D . .
H2 H 0.674(3) 0.913(3) 0.540(2) 0.096 Uiso 1 1 d D . .
H3 H 0.756(4) 0.828(3) 0.5051(19) 0.096 Uiso 1 1 d D . .
H4 H 0.810(4) 0.947(3) 0.516(2) 0.096 Uiso 1 1 d D . .
H91 H 0.106(11) 0.862(8) 0.530(6) 0.096 Uiso 0.5 1 d PD . .
H92 H 0.008(12) 0.866(8) 0.456(5) 0.096 Uiso 0.5 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
C1 0.0398(18) 0.0327(17) 0.054(2) 0.0045(16) 0.0163(18) -0.0014(14)
C2 0.043(2) 0.0316(17) 0.059(2) -0.0122(16) 0.0127(18) -0.0030(15)
C3 0.0394(19) 0.0403(18) 0.040(2) -0.0121(15) 0.0122(16) -0.0009(15)
C11 0.045(2) 0.069(3) 0.047(2) -0.020(2) 0.0236(19) -0.019(2)
C12 0.0374(19) 0.066(2) 0.0340(19) 0.0055(18) 0.0073(16) -0.0072(17)
C21 0.0268(16) 0.0392(17) 0.040(2) -0.0033(15) 0.0085(15) -0.0058(14)
C22 0.0333(17) 0.0347(17) 0.048(2) 0.0019(16) 0.0172(16) 0.0015(13)
C31 0.0356(17) 0.0363(17) 0.0383(19) 0.0001(14) 0.0145(16) 0.0025(14)
C32 0.0357(18) 0.0448(19) 0.043(2) -0.0039(16) 0.0168(16) -0.0055(15)
C41 0.049(2) 0.0391(19) 0.064(3) 0.0150(19) 0.023(2) 0.0073(17)
C42 0.045(2) 0.051(2) 0.040(2) 0.0075(17) 0.0086(17) 0.0049(16)
Fe1 0.0329(3) 0.0312(2) 0.0538(3) -0.0086(3) 0.0176(2) -0.0029(2)
N1 0.0289(14) 0.0322(13) 0.0368(16) 0.0009(12) 0.0102(12) -0.0030(11)
N2 0.0326(14) 0.0324(13) 0.0319(15) -0.0026(11) 0.0097(12) 0.0017(11)
N3 0.135(4) 0.056(2) 0.044(2) -0.0038(17) 0.002(2) -0.001(2)
O11 0.0479(15) 0.0522(15) 0.0693(18) -0.0221(15) 0.0113(14) -0.0129(14)
O12 0.0601(17) 0.113(3) 0.0484(17) -0.0284(17) 0.0124(15) -0.0325(18)
O21 0.0405(12) 0.0376(12) 0.0557(16) 0.0132(11) 0.0199(12) 0.0067(10)
O22 0.0514(15) 0.0615(16) 0.0546(16) 0.0177(13) 0.0302(14) 0.0095(12)
O31 0.0317(12) 0.0550(14) 0.0392(14) -0.0111(11) 0.0101(11) -0.0032(11)
O32 0.0389(14) 0.0641(16) 0.0494(16) -0.0046(13) 0.0226(13) -0.0046(12)
O41 0.0459(15) 0.0338(13) 0.084(2) -0.0065(14) 0.0176(15) 0.0057(11)
O42 0.0661(19) 0.0481(16) 0.104(3) 0.0250(16) 0.0136(19) 0.0169(15)
O91 0.076(5) 0.055(4) 0.058(4) -0.008(3) 0.009(4) -0.005(3)

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

_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
C1 N1 1.500(4) . ?
C1 C2 1.523(5) . ?
C2 C3 1.527(5) . ?
C3 N2 1.498(4) . ?
C11 O12 1.229(5) . ?
C11 O11 1.281(5) . ?
C11 C12 1.527(5) . ?
C12 N1 1.503(4) . ?
C21 O22 1.231(4) . ?
C21 O21 1.291(4) . ?
C21 C22 1.508(5) . ?
C22 N1 1.488(4) . ?
C31 O32 1.223(4) . ?
C31 O31 1.294(4) . ?
C31 C32 1.526(5) . ?
C32 N2 1.490(4) . ?
C41 O42 1.232(4) . ?
C41 O41 1.284(5) . ?
C41 C42 1.521(5) . ?
C42 N2 1.493(4) . ?
Fe1 O11 1.947(3) . ?
Fe1 O41 1.968(3) . ?
Fe1 O21 1.990(2) . ?
Fe1 O31 1.992(2) . ?
Fe1 N1 2.182(3) . ?
Fe1 N2 2.200(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 116.0(3) . . ?
C1 C2 C3 119.9(3) . . ?
N2 C3 C2 115.2(3) . . ?
O12 C11 O11 124.2(4) . . ?
O12 C11 C12 119.3(4) . . ?
O11 C11 C12 116.5(3) . . ?
N1 C12 C11 111.5(3) . . ?
O22 C21 O21 123.6(3) . . ?
O22 C21 C22 118.9(3) . . ?
O21 C21 C22 117.5(3) . . ?
N1 C22 C21 113.2(2) . . ?
O32 C31 O31 123.9(3) . . ?
O32 C31 C32 119.2(3) . . ?
O31 C31 C32 116.9(3) . . ?
N2 C32 C31 111.9(3) . . ?
O42 C41 O41 124.0(4) . . ?
O42 C41 C42 119.7(4) . . ?
O41 C41 C42 116.3(3) . . ?
N2 C42 C41 112.5(3) . . ?
O11 Fe1 O41 107.49(11) . . ?
O11 Fe1 O21 94.73(11) . . ?
O41 Fe1 O21 92.74(10) . . ?
O11 Fe1 O31 92.23(10) . . ?
O41 Fe1 O31 93.25(11) . . ?
O21 Fe1 O31 169.03(9) . . ?
O11 Fe1 N1 82.03(11) . . ?
O41 Fe1 N1 168.88(11) . . ?
O21 Fe1 N1 80.53(9) . . ?
O31 Fe1 N1 92.08(9) . . ?
O11 Fe1 N2 168.98(11) . . ?
O41 Fe1 N2 81.31(11) . . ?
O21 Fe1 N2 91.39(10) . . ?
O31 Fe1 N2 80.44(9) . . ?
N1 Fe1 N2 89.97(10) . . ?
C22 N1 C1 112.4(2) . . ?
C22 N1 C12 110.8(3) . . ?
C1 N1 C12 109.6(2) . . ?
C22 N1 Fe1 108.33(17) . . ?
C1 N1 Fe1 114.00(19) . . ?
C12 N1 Fe1 101.27(19) . . ?
C32 N2 C42 110.1(3) . . ?
C32 N2 C3 112.9(2) . . ?
C42 N2 C3 108.6(2) . . ?
C32 N2 Fe1 108.45(19) . . ?
C42 N2 Fe1 102.42(19) . . ?
C3 N2 Fe1 113.86(19) . . ?
C11 O11 Fe1 117.4(2) . . ?
C21 O21 Fe1 119.6(2) . . ?
C31 O31 Fe1 118.3(2) . . ?
C41 O41 Fe1 118.3(2) . . ?