# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Mir Wais Hosseini'
_publ_contact_author_email       HOSSEINI@CHIMIE.U-STRASBG.FR

_publ_section_title              
;
In situ reduction of Fe(III) into Fe(II):
an example of post-crystallisation transformation
;
loop_
_publ_author_name
'Mir Wais Hosseini'
'Pierre Dechambenoit'
'Sylvie Ferlay'
'Nathalie Kyritsakas'

# Attachment '13-[Co_CN_6]2_MeOH0.66_511_.cif'

data_e511a
_database_code_depnum_ccdc_archive 'CCDC 742022'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         
'2(C26 H44 N4), 2(C6 Co N6), 6(C0.11 H0.44 O0.11)'

_chemical_formula_sum            'C90.66 H134.64 Co2 N24 OO.66'

_chemical_formula_weight         1696.07

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal

_symmetry_space_group_name_H-M   P-3

_symmetry_space_group_name_Hall  '-P 3'

loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   17.8790(3)

_cell_length_b                   17.8790(3)

_cell_length_c                   8.7221(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.00

_cell_angle_gamma                120.00

_cell_volume                     2414.56(12)

_cell_formula_units_Z            1

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    4534

_cell_measurement_theta_min      2.34

_cell_measurement_theta_max      27.54

_exptl_crystal_description       prism

_exptl_crystal_colour            colorless

_exptl_crystal_size_max          0.16

_exptl_crystal_size_mid          0.12

_exptl_crystal_size_min          0.10

_exptl_crystal_density_meas      none

_exptl_crystal_density_diffrn    1.166

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             908

_exptl_absorpt_coefficient_mu    0.400

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9388

_exptl_absorpt_correction_T_max  0.9611

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      173(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            24800

_diffrn_reflns_av_R_equivalents  0.0473

_diffrn_reflns_av_sigmaI/netI    0.0398

_diffrn_reflns_limit_h_min       -20

_diffrn_reflns_limit_h_max       25

_diffrn_reflns_limit_k_min       -25

_diffrn_reflns_limit_k_max       25

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       12

_diffrn_reflns_theta_min         2.28

_diffrn_reflns_theta_max         30.04

_reflns_number_total             4715

_reflns_number_gt                3582

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0830P)^2^+0.4865P] 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    riding

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         4715

_refine_ls_number_parameters     189

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0650

_refine_ls_R_factor_gt           0.0442

_refine_ls_wR_factor_ref         0.1376

_refine_ls_wR_factor_gt          0.1259

_refine_ls_goodness_of_fit_ref   1.024

_refine_ls_restrained_S_all      1.024

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000

loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

C1 C 0.94107(10) 0.54502(10) 0.22842(19) 0.0238(3) Uani 1 1 d . . .
N1 N 0.86316(8) 0.53522(9) 0.23186(15) 0.0248(3) Uani 1 1 d . . .
H1 H 0.8320 0.5150 0.3157 0.030 Uiso 1 1 calc R . .
C2 C 0.82671(10) 0.55680(11) 0.10097(18) 0.0246(3) Uani 1 1 d . . .
H2A H 0.7855 0.5745 0.1378 0.030 Uiso 1 1 calc R . .
H2B H 0.7947 0.5052 0.0353 0.030 Uiso 1 1 calc R . .
C3 C 0.89784(10) 0.62998(10) 0.00693(18) 0.0234(3) Uani 1 1 d . . .
C4 C 0.96453(11) 0.60233(11) -0.03131(18) 0.0261(3) Uani 1 1 d . . .
H4A H 0.9390 0.5534 -0.1044 0.031 Uiso 1 1 calc R . .
H4B H 1.0155 0.6509 -0.0808 0.031 Uiso 1 1 calc R . .
N2 N 0.99162(9) 0.57640(9) 0.10771(15) 0.0263(3) Uani 1 1 d . . .
H2 H 1.0434 0.5820 0.1107 0.032 Uiso 1 1 calc R . .
C5 C 0.85586(12) 0.63726(12) -0.14256(19) 0.0310(4) Uani 1 1 d . . .
H5A H 0.8311 0.5814 -0.1973 0.037 Uiso 1 1 calc R . .
H5B H 0.8074 0.6465 -0.1151 0.037 Uiso 1 1 calc R . .
C6 C 0.91475(19) 0.70809(18) -0.2518(3) 0.0641(8) Uani 1 1 d . . .
H6A H 0.9647 0.7008 -0.2773 0.077 Uiso 1 1 calc R . .
H6B H 0.9371 0.7647 -0.2005 0.077 Uiso 1 1 calc R . .
C7 C 0.8691(2) 0.70775(16) -0.3989(3) 0.0672(8) Uani 1 1 d . . .
H7A H 0.8504 0.6534 -0.4538 0.101 Uiso 1 1 calc R . .
H7B H 0.9089 0.7563 -0.4637 0.101 Uiso 1 1 calc R . .
H7C H 0.8187 0.7134 -0.3742 0.101 Uiso 1 1 calc R . .
C8 C 0.94376(11) 0.71497(11) 0.0987(2) 0.0281(3) Uani 1 1 d . . .
H8A H 0.9729 0.7059 0.1873 0.034 Uiso 1 1 calc R . .
H8B H 0.9894 0.7594 0.0327 0.034 Uiso 1 1 calc R . .
C9 C 0.88874(14) 0.75117(15) 0.1585(3) 0.0485(6) Uani 1 1 d . . .
H9A H 0.8510 0.7135 0.2416 0.058 Uiso 1 1 calc R . .
H9B H 0.8512 0.7509 0.0749 0.058 Uiso 1 1 calc R . .
C10 C 0.94321(17) 0.84289(15) 0.2193(3) 0.0544(6) Uani 1 1 d . . .
H10A H 0.9812 0.8436 0.3011 0.082 Uiso 1 1 calc R . .
H10B H 0.9052 0.8630 0.2601 0.082 Uiso 1 1 calc R . .
H10C H 0.9783 0.8811 0.1359 0.082 Uiso 1 1 calc R . .
C11 C 0.97237(10) 0.52148(11) 0.36758(18) 0.0242(3) Uani 1 1 d . . .
C12 C 1.05363(10) 0.57863(11) 0.42712(19) 0.0260(3) Uani 1 1 d . . .
H12 H 1.0899 0.6320 0.3771 0.031 Uiso 1 1 calc R . .
C13 C 1.08125(10) 0.55703(11) 0.56036(19) 0.0265(3) Uani 1 1 d . . .
H13 H 1.1365 0.5957 0.6021 0.032 Uiso 1 1 calc R . .
Co1 Co 0.6667 0.3333 0.71792(4) 0.01924(12) Uani 1 3 d S . .
C14 C 0.59902(10) 0.23255(10) 0.83859(18) 0.0221(3) Uani 1 1 d . . .
N3 N 0.55562(9) 0.16990(9) 0.90549(17) 0.0291(3) Uani 1 1 d . . .
C15 C 0.56972(10) 0.29761(10) 0.58846(18) 0.0239(3) Uani 1 1 d . . .
N4 N 0.51267(10) 0.27509(10) 0.50508(18) 0.0331(3) Uani 1 1 d . . .
C16 C 0.6667 0.3333 0.2127(7) 0.0167(13) Uani 0.33 3 d SP . .
O1 O 0.5901(5) 0.2437(6) 0.2097(9) 0.0126(15) Uani 0.11 1 d P . .

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 0.0185(7) 0.0230(7) 0.0298(8) 0.0052(6) -0.0001(6) 0.0105(6)
N1 0.0171(6) 0.0309(7) 0.0267(6) 0.0092(5) 0.0027(5) 0.0122(6)
C2 0.0180(7) 0.0267(8) 0.0288(7) 0.0061(6) -0.0006(6) 0.0110(6)
C3 0.0226(7) 0.0216(7) 0.0249(7) 0.0036(6) -0.0014(6) 0.0101(6)
C4 0.0235(8) 0.0280(8) 0.0258(7) 0.0045(6) 0.0032(6) 0.0122(7)
N2 0.0179(6) 0.0306(7) 0.0321(7) 0.0054(6) 0.0022(5) 0.0135(6)
C5 0.0354(9) 0.0269(8) 0.0281(8) 0.0025(6) -0.0074(7) 0.0137(7)
C6 0.0667(17) 0.0540(14) 0.0436(12) 0.0246(11) -0.0116(11) 0.0092(12)
C7 0.103(2) 0.0422(13) 0.0378(11) 0.0088(10) -0.0222(13) 0.0221(14)
C8 0.0261(8) 0.0249(8) 0.0304(8) 0.0017(6) -0.0021(6) 0.0106(7)
C9 0.0446(12) 0.0492(13) 0.0623(14) -0.0237(11) -0.0208(10) 0.0314(11)
C10 0.0651(15) 0.0435(13) 0.0645(14) -0.0160(11) -0.0113(12) 0.0346(12)
C11 0.0202(7) 0.0269(8) 0.0287(8) 0.0060(6) 0.0001(6) 0.0142(6)
C12 0.0202(7) 0.0239(8) 0.0334(8) 0.0081(6) 0.0008(6) 0.0106(6)
C13 0.0183(7) 0.0252(8) 0.0343(8) 0.0049(6) -0.0019(6) 0.0097(7)
Co1 0.01447(13) 0.01447(13) 0.0288(2) 0.000 0.000 0.00723(7)
C14 0.0172(7) 0.0186(7) 0.0315(8) -0.0044(6) -0.0038(6) 0.0095(6)
N3 0.0267(7) 0.0192(7) 0.0378(8) 0.0012(6) -0.0018(6) 0.0088(6)
C15 0.0205(7) 0.0183(7) 0.0327(8) 0.0038(6) 0.0018(6) 0.0097(6)
N4 0.0266(7) 0.0308(8) 0.0401(8) 0.0059(6) -0.0052(6) 0.0130(6)
C16 0.022(2) 0.022(2) 0.006(3) 0.000 0.000 0.0110(11)
O1 0.018(4) 0.020(4) 0.007(3) 0.002(3) -0.001(3) 0.016(4)

_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 1.314(2) . ?
C1 N2 1.316(2) . ?
C1 C11 1.483(2) . ?
N1 C2 1.4588(19) . ?
N1 H1 0.8800 . ?
C2 C3 1.529(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.539(2) . ?
C3 C8 1.542(2) . ?
C3 C5 1.542(2) . ?
C4 N2 1.464(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N2 H2 0.8800 . ?
C5 C6 1.512(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.519(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.515(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.524(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.392(2) 4_766 ?
C11 C12 1.393(2) . ?
C12 C13 1.391(2) . ?
C12 H12 0.9500 . ?
C13 C11 1.392(2) 4_766 ?
C13 H13 0.9500 . ?
Co1 C15 1.8922(16) . ?
Co1 C15 1.8922(16) 3_665 ?
Co1 C15 1.8922(16) 2_655 ?
Co1 C14 1.9074(16) . ?
Co1 C14 1.9074(16) 2_655 ?
Co1 C14 1.9075(16) 3_665 ?
C14 N3 1.152(2) . ?
C15 N4 1.149(2) . ?
C16 O1 1.500(9) 3_665 ?
C16 O1 1.500(9) 2_655 ?
C16 O1 1.500(9) . ?

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 N2 122.07(14) . . ?
N1 C1 C11 117.95(14) . . ?
N2 C1 C11 119.96(14) . . ?
C1 N1 C2 122.05(13) . . ?
C1 N1 H1 119.0 . . ?
C2 N1 H1 119.0 . . ?
N1 C2 C3 110.84(12) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 106.73(13) . . ?
C2 C3 C8 111.73(13) . . ?
C4 C3 C8 108.24(13) . . ?
C2 C3 C5 107.11(13) . . ?
C4 C3 C5 109.39(14) . . ?
C8 C3 C5 113.42(13) . . ?
N2 C4 C3 110.75(13) . . ?
N2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C1 N2 C4 122.14(13) . . ?
C1 N2 H2 118.9 . . ?
C4 N2 H2 118.9 . . ?
C6 C5 C3 116.04(16) . . ?
C6 C5 H5A 108.3 . . ?
C3 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C3 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C5 C6 C7 112.4(2) . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C3 117.41(15) . . ?
C9 C8 H8A 107.9 . . ?
C3 C8 H8A 107.9 . . ?
C9 C8 H8B 107.9 . . ?
C3 C8 H8B 107.9 . . ?
H8A C8 H8B 107.2 . . ?
C8 C9 C10 112.18(18) . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 120.74(14) 4_766 . ?
C13 C11 C1 119.22(14) 4_766 . ?
C12 C11 C1 120.01(14) . . ?
C13 C12 C11 119.52(15) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C11 119.74(15) . 4_766 ?
C12 C13 H13 120.1 . . ?
C11 C13 H13 120.1 4_766 . ?
C15 Co1 C15 88.05(7) . 3_665 ?
C15 Co1 C15 88.04(7) . 2_655 ?
C15 Co1 C15 88.04(7) 3_665 2_655 ?
C15 Co1 C14 88.24(6) . . ?
C15 Co1 C14 176.23(7) 3_665 . ?
C15 Co1 C14 91.19(7) 2_655 . ?
C15 Co1 C14 176.23(7) . 2_655 ?
C15 Co1 C14 91.19(7) 3_665 2_655 ?
C15 Co1 C14 88.24(6) 2_655 2_655 ?
C14 Co1 C14 92.48(6) . 2_655 ?
C15 Co1 C14 91.19(7) . 3_665 ?
C15 Co1 C14 88.24(6) 3_665 3_665 ?
C15 Co1 C14 176.23(7) 2_655 3_665 ?
C14 Co1 C14 92.48(6) . 3_665 ?
C14 Co1 C14 92.48(6) 2_655 3_665 ?
N3 C14 Co1 176.72(14) . . ?
N4 C15 Co1 177.05(16) . . ?
O1 C16 O1 119.97(3) 3_665 2_655 ?
O1 C16 O1 119.97(3) 3_665 . ?
O1 C16 O1 119.97(2) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        30.04

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.656

_refine_diff_density_min         -0.516

_refine_diff_density_rms         0.068

# Attachment 'B914964C_New_Cif_13-[Fe_CN_6]2_MeOH0.66_315_.cif'

data_e315b
_database_code_depnum_ccdc_archive 'CCDC 742023'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'3(C26 H44 N4), 2(C6 Fe N6), 6( C0.11 O0.11 H0.33)'
_chemical_formula_sum            'C90.66 H134.64 Fe2 N24 O0.66'
_chemical_formula_weight         1680.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3
_symmetry_space_group_name_Hall  '-P 3'

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

_cell_length_a                   17.9647(9)
_cell_length_b                   17.9647(9)
_cell_length_c                   8.6670(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2422.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2967
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      25.05

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             901.2
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9653
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16085
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         27.54
_reflns_number_total             3720
_reflns_number_gt                2588
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0515P)^2^+0.6668P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3720
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1159
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.60462(12) 0.05943(12) 0.2716(3) 0.0294(5) Uani 1 1 d . . .
N1 N 0.67237(10) 0.13649(10) 0.2680(2) 0.0304(4) Uani 1 1 d . . .
H1 H 0.6830 0.1674 0.1835 0.036 Uiso 1 1 calc R . .
C2 C 0.73096(12) 0.17321(12) 0.3985(2) 0.0301(5) Uani 1 1 d . . .
H2A H 0.7121 0.2056 0.4648 0.036 Uiso 1 1 calc R . .
H2B H 0.7895 0.2139 0.3602 0.036 Uiso 1 1 calc R . .
C3 C 0.73316(12) 0.10260(12) 0.4933(2) 0.0293(5) Uani 1 1 d . . .
C4 C 0.63905(12) 0.03633(12) 0.5327(3) 0.0320(5) Uani 1 1 d . . .
H4A H 0.6366 -0.0145 0.5824 0.038 Uiso 1 1 calc R . .
H4B H 0.6162 0.0620 0.6066 0.038 Uiso 1 1 calc R . .
C5 C 0.78223(14) 0.14471(14) 0.6427(3) 0.0372(5) Uani 1 1 d . . .
H5A H 0.8397 0.1928 0.6145 0.045 Uiso 1 1 calc R . .
H5B H 0.7514 0.1696 0.6974 0.045 Uiso 1 1 calc R . .
C6 C 0.7943(2) 0.0864(2) 0.7541(3) 0.0706(9) Uani 1 1 d . . .
H6A H 0.7373 0.0373 0.7817 0.085 Uiso 1 1 calc R . .
H6B H 0.8275 0.0631 0.7023 0.085 Uiso 1 1 calc R . .
C7 C 0.8407(2) 0.1325(2) 0.8999(3) 0.0772(10) Uani 1 1 d . . .
H7A H 0.8968 0.1817 0.8733 0.116 Uiso 1 1 calc R . .
H7B H 0.8488 0.0929 0.9661 0.116 Uiso 1 1 calc R . .
H7C H 0.8064 0.1526 0.9549 0.116 Uiso 1 1 calc R . .
C8 C 0.77154(13) 0.05679(13) 0.4011(3) 0.0329(5) Uani 1 1 d . . .
H8A H 0.7689 0.0103 0.4665 0.039 Uiso 1 1 calc R . .
H8B H 0.7342 0.0291 0.3105 0.039 Uiso 1 1 calc R . .
C9 C 0.86283(15) 0.11073(16) 0.3439(3) 0.0531(7) Uani 1 1 d . . .
H9A H 0.8995 0.1470 0.4296 0.064 Uiso 1 1 calc R . .
H9B H 0.8643 0.1494 0.2611 0.064 Uiso 1 1 calc R . .
C10 C 0.89956(17) 0.05616(18) 0.2821(4) 0.0615(8) Uani 1 1 d . . .
H10A H 0.9030 0.0214 0.3660 0.092 Uiso 1 1 calc R . .
H10B H 0.9572 0.0938 0.2402 0.092 Uiso 1 1 calc R . .
H10C H 0.8621 0.0182 0.2004 0.092 Uiso 1 1 calc R . .
N2 N 0.58601(10) 0.00948(10) 0.3935(2) 0.0319(4) Uani 1 1 d . . .
H2 H 0.5400 -0.0420 0.3910 0.038 Uiso 1 1 calc R . .
C11 C 0.54967(12) 0.02795(12) 0.1325(2) 0.0300(5) Uani 1 1 d . . .
C12 C 0.52444(12) -0.05354(12) 0.0731(3) 0.0320(5) Uani 1 1 d . . .
H12 H 0.5412 -0.0898 0.1234 0.038 Uiso 1 1 calc R . .
C13 C 0.47497(12) -0.08117(12) -0.0589(3) 0.0326(5) Uani 1 1 d . . .
H13 H 0.4577 -0.1366 -0.0997 0.039 Uiso 1 1 calc R . .
Fe1 Fe 0.6667 0.3333 0.77529(6) 0.02553(15) Uani 1 3 d S . .
C14 C 0.59724(12) 0.23022(12) 0.6526(3) 0.0277(4) Uani 1 1 d . . .
N3 N 0.55355(11) 0.16752(10) 0.5863(2) 0.0352(4) Uani 1 1 d . . .
C15 C 0.70374(12) 0.27170(12) 0.9095(3) 0.0302(5) Uani 1 1 d . . .
N4 N 0.72632(11) 0.23816(11) 0.9943(2) 0.0405(5) Uani 1 1 d . . .
C16 C 0.6667 0.3333 0.2808(13) 0.032(2) Uani 0.33 3 d SP . .
O1 O 0.6546(8) 0.4101(7) 0.2859(15) 0.032(3) Uiso 0.11 1 d P . .

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 0.0249(9) 0.0225(9) 0.0391(13) 0.0004(9) -0.0044(9) 0.0106(8)
N1 0.0288(8) 0.0217(8) 0.0347(11) 0.0029(7) -0.0078(7) 0.0081(7)
C2 0.0252(9) 0.0235(9) 0.0368(13) -0.0031(8) -0.0085(9) 0.0085(8)
C3 0.0286(10) 0.0276(10) 0.0324(12) -0.0016(9) -0.0055(9) 0.0144(8)
C4 0.0338(11) 0.0280(10) 0.0341(13) 0.0036(9) -0.0016(9) 0.0153(9)
C5 0.0407(12) 0.0412(12) 0.0357(13) -0.0066(10) -0.0085(10) 0.0249(10)
C6 0.106(2) 0.076(2) 0.0512(18) -0.0117(15) -0.0344(18) 0.0624(19)
C7 0.114(3) 0.117(3) 0.0445(18) -0.0211(18) -0.0298(18) 0.090(2)
C8 0.0355(11) 0.0302(10) 0.0353(13) -0.0015(9) -0.0042(9) 0.0182(9)
C9 0.0384(13) 0.0513(14) 0.0632(18) -0.0200(13) -0.0001(12) 0.0176(11)
C10 0.0496(15) 0.0712(18) 0.071(2) -0.0113(16) 0.0035(14) 0.0353(14)
N2 0.0254(8) 0.0219(8) 0.0400(11) 0.0033(8) -0.0041(8) 0.0056(7)
C11 0.0230(9) 0.0242(9) 0.0380(13) 0.0012(9) -0.0042(9) 0.0083(8)
C12 0.0289(10) 0.0236(9) 0.0422(14) 0.0004(9) -0.0075(9) 0.0122(8)
C13 0.0289(10) 0.0208(9) 0.0446(13) -0.0018(9) -0.0060(9) 0.0098(8)
Fe1 0.01850(17) 0.01850(17) 0.0396(3) 0.000 0.000 0.00925(8)
C14 0.0228(9) 0.0224(9) 0.0396(13) 0.0050(9) 0.0049(9) 0.0126(8)
N3 0.0316(9) 0.0241(9) 0.0468(12) -0.0003(8) 0.0012(8) 0.0116(7)
C15 0.0230(9) 0.0246(10) 0.0430(13) 0.0013(9) 0.0048(9) 0.0118(8)
N4 0.0377(10) 0.0378(10) 0.0502(13) 0.0122(9) 0.0069(9) 0.0219(9)
C16 0.035(3) 0.035(3) 0.028(6) 0.000 0.000 0.0174(17)

_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 1.309(2) . ?
C1 N2 1.316(3) . ?
C1 C11 1.480(3) . ?
N1 C2 1.459(2) . ?
N1 H1 0.8800 . ?
C2 C3 1.528(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.536(3) . ?
C3 C8 1.536(3) . ?
C3 C4 1.542(3) . ?
C4 N2 1.462(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.518(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.512(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.512(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.527(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N2 H2 0.8800 . ?
C11 C13 1.393(3) 4_655 ?
C11 C12 1.396(3) . ?
C12 C13 1.380(3) . ?
C12 H12 0.9500 . ?
C13 C11 1.393(3) 4_655 ?
C13 H13 0.9500 . ?
Fe1 C15 1.939(2) 2_655 ?
Fe1 C15 1.939(2) . ?
Fe1 C15 1.939(2) 3_665 ?
Fe1 C14 1.951(2) . ?
Fe1 C14 1.951(2) 2_655 ?
Fe1 C14 1.951(2) 3_665 ?
C14 N3 1.154(2) . ?
C15 N4 1.146(3) . ?
C16 O1 1.500(12) 3_665 ?
C16 O1 1.500(12) . ?
C16 O1 1.500(12) 2_655 ?

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 N2 121.66(19) . . ?
N1 C1 C11 118.33(18) . . ?
N2 C1 C11 119.99(17) . . ?
C1 N1 C2 122.60(17) . . ?
C1 N1 H1 118.7 . . ?
C2 N1 H1 118.7 . . ?
N1 C2 C3 110.73(15) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C5 106.94(15) . . ?
C2 C3 C8 111.68(17) . . ?
C5 C3 C8 113.69(16) . . ?
C2 C3 C4 106.65(15) . . ?
C5 C3 C4 109.34(17) . . ?
C8 C3 C4 108.30(16) . . ?
N2 C4 C3 110.73(17) . . ?
N2 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C3 116.18(19) . . ?
C6 C5 H5A 108.2 . . ?
C3 C5 H5A 108.2 . . ?
C6 C5 H5B 108.2 . . ?
C3 C5 H5B 108.2 . . ?
H5A C5 H5B 107.4 . . ?
C7 C6 C5 112.6(2) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C3 117.44(17) . . ?
C9 C8 H8A 107.9 . . ?
C3 C8 H8A 107.9 . . ?
C9 C8 H8B 107.9 . . ?
C3 C8 H8B 107.9 . . ?
H8A C8 H8B 107.2 . . ?
C8 C9 C10 112.5(2) . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C1 N2 C4 122.42(16) . . ?
C1 N2 H2 118.8 . . ?
C4 N2 H2 118.8 . . ?
C13 C11 C12 120.21(19) 4_655 . ?
C13 C11 C1 119.40(18) 4_655 . ?
C12 C11 C1 120.38(17) . . ?
C13 C12 C11 119.71(18) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C11 120.08(18) . 4_655 ?
C12 C13 H13 120.0 . . ?
C11 C13 H13 120.0 4_655 . ?
C15 Fe1 C15 87.74(9) 2_655 . ?
C15 Fe1 C15 87.74(9) 2_655 3_665 ?
C15 Fe1 C15 87.74(9) . 3_665 ?
C15 Fe1 C14 175.39(9) 2_655 . ?
C15 Fe1 C14 91.36(8) . . ?
C15 Fe1 C14 87.71(8) 3_665 . ?
C15 Fe1 C14 91.36(8) 2_655 2_655 ?
C15 Fe1 C14 87.71(8) . 2_655 ?
C15 Fe1 C14 175.39(9) 3_665 2_655 ?
C14 Fe1 C14 93.12(8) . 2_655 ?
C15 Fe1 C14 87.71(8) 2_655 3_665 ?
C15 Fe1 C14 175.39(9) . 3_665 ?
C15 Fe1 C14 91.36(8) 3_665 3_665 ?
C14 Fe1 C14 93.12(8) . 3_665 ?
C14 Fe1 C14 93.12(8) 2_655 3_665 ?
N3 C14 Fe1 176.60(19) . . ?
N4 C15 Fe1 176.64(19) . . ?
O1 C16 O1 119.91(7) 3_665 . ?
O1 C16 O1 119.91(7) 3_665 2_655 ?
O1 C16 O1 119.92(7) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.053