# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182

_publ_contact_author_name        M.Schroder
_publ_contact_author_address     
;
Department of Chemistry
University of Nottingham
Nottingham
NG7 2RD
UNITED KINGDOM
;

_publ_section_title              
;
Twelve-Connected Porous Metal-Organic Frameworks with
High H2 Adsorption
;
_publ_contact_author_email       M.SCHRODER@NOTTINGHAM.AC.UK
loop_
_publ_author_name
M.Schroder
A.J.Blake
N.Champness
E.Cussen
P.Hubberstey
'Junhua Jia'
'Xiang Lin'
G.S.Walker
C.Wilson

# Attachment 'Compound_1.cif'

data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 622764'

_refine_special_details          
;
Electron density in poorly defined solvent region accounted for
using SQUEEZE, which calculated 1144.6 electrons
per unit cell which was assigned as 4.8 molecules of
DMF per Ni3.

The phenyl ring C1 to C6 showed disorder and was modelled
over two partially occupied sites, with occupancies of 0.60
and 0.40.

# SQUEEZE RESULTS (APPEND TO CIF)
#loop_
#_platon_squeeze_void_nr
#_platon_squeeze_void_average_x
#_platon_squeeze_void_average_y
#_platon_squeeze_void_average_z
#_platon_squeeze_void_volume
#_platon_squeeze_void_count_electrons
#1 -0.052 -0.069 -0.001 7626.3 1144.6
#_platon_squeeze_details
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C71.40 H67.60 N7.80 Ni3 O17.80'
_chemical_formula_weight         1495.86

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'R -3c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   18.9996(16)
_cell_length_b                   18.9996(16)
_cell_length_c                   45.997(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14380(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4471
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25

_exptl_crystal_description       COLUMN
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4662
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Bruker SADABS v2.05 (2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24743
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         24.97
_reflns_number_total             2812
_reflns_number_gt                2342
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ' ?'
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_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^)+(0.0895P)^2^+1.6386P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2812
_refine_ls_number_parameters     112
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1293
_refine_ls_wR_factor_gt          0.1265
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.115
_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
Ni Ni 0.56233(2) 0.22900(2) 0.0833 0.01709(18) Uani 1 2 d S . .
O1H O 0.6667 0.3333 0.0833 0.0369(11) Uani 1 6 d S . .
N1 N 0.45211(15) 0.11878(15) 0.0833 0.0266(7) Uani 1 2 d S . .
C1 C 0.2732(3) -0.1144(3) 0.02400(11) 0.0346(11) Uiso 0.60 1 d PD A 1
H1 H 0.2271 -0.1135 0.0315 0.042 Uiso 0.60 1 calc PR A 1
C2 C 0.2656(3) -0.1602(3) -0.00054(9) 0.0285(9) Uiso 0.60 1 d PD A 1
H2 H 0.2128 -0.1962 -0.0080 0.034 Uiso 0.60 1 calc PR A 1
C4 C 0.4074(2) -0.1151(2) 0.00179(9) 0.0265(9) Uiso 0.60 1 d PD A 1
H4 H 0.4522 -0.1200 -0.0047 0.032 Uiso 0.60 1 calc PR A 1
C5 C 0.4154(3) -0.0705(3) 0.02611(9) 0.0295(9) Uiso 0.60 1 d PD A 1
H5 H 0.4672 -0.0403 0.0351 0.035 Uiso 0.60 1 calc PR A 1
C6 C 0.3501(3) -0.0685(3) 0.03788(10) 0.0257(11) Uiso 0.60 1 d PD A 1
C1A C 0.2880(4) -0.1342(4) 0.03126(15) 0.0279(14) Uiso 0.40 1 d PD A 2
H1A H 0.2545 -0.1590 0.0477 0.033 Uiso 0.40 1 calc PR A 2
C2A C 0.2830(4) -0.1806(4) 0.00757(15) 0.0312(15) Uiso 0.40 1 d PD A 2
H2A H 0.2405 -0.2357 0.0074 0.037 Uiso 0.40 1 calc PR A 2
C4A C 0.3806(5) -0.0640(5) -0.01779(17) 0.0450(18) Uiso 0.40 1 d PD A 2
H4A H 0.4058 -0.0400 -0.0358 0.054 Uiso 0.40 1 calc PR A 2
C5A C 0.3876(5) -0.0181(5) 0.00561(17) 0.0490(19) Uiso 0.40 1 d PD A 2
H5A H 0.4248 0.0387 0.0048 0.059 Uiso 0.40 1 calc PR A 2
C6A C 0.3418(3) -0.0512(4) 0.03109(13) 0.0154(13) Uiso 0.40 1 d PD A 2
C3 C 0.33134(15) -0.15508(17) -0.01424(6) 0.0376(7) Uani 1 1 d D . .
C7 C 0.36034(16) -0.00763(17) 0.06017(6) 0.0432(8) Uani 1 1 d . . .
C8 C 0.3063(2) -0.0271(2) 0.0833 0.0518(13) Uani 1 2 d S A .
H8 H 0.2563 -0.0771 0.0833 0.062 Uiso 1 2 calc SR . .
C9 C 0.43225(15) 0.06691(16) 0.06136(5) 0.0315(6) Uani 1 1 d . A .
H9 H 0.4692 0.0814 0.0456 0.038 Uiso 1 1 calc R . .
C10 C 0.32655(14) -0.20220(15) -0.04110(5) 0.0250(5) Uani 1 1 d . A .
O1 O 0.25947(10) -0.26462(10) -0.04626(3) 0.0267(4) Uani 1 1 d . . .
O2 O 0.39046(10) -0.17476(10) -0.05594(4) 0.0270(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
Ni 0.0176(2) 0.0176(2) 0.0154(3) -0.00104(8) 0.00104(8) 0.00830(19)
O1H 0.0147(13) 0.0147(13) 0.081(4) 0.000 0.000 0.0074(6)
N1 0.0258(11) 0.0258(11) 0.0259(16) -0.0048(6) 0.0048(6) 0.0110(13)
C3 0.0220(13) 0.0333(15) 0.0430(16) -0.0154(13) 0.0105(11) 0.0029(11)
C7 0.0280(14) 0.0388(16) 0.0443(17) -0.0180(13) 0.0133(12) 0.0029(13)
C8 0.0346(15) 0.0346(15) 0.058(3) -0.0238(13) 0.0238(13) -0.0038(18)
C9 0.0264(13) 0.0345(15) 0.0243(13) -0.0096(11) 0.0063(10) 0.0083(11)
C10 0.0232(13) 0.0251(13) 0.0256(13) -0.0013(10) 0.0045(10) 0.0113(11)
O1 0.0238(9) 0.0257(9) 0.0234(9) -0.0062(7) 0.0028(7) 0.0069(8)
O2 0.0226(9) 0.0230(9) 0.0307(10) -0.0046(7) 0.0065(7) 0.0079(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
Ni O1H 1.9823(4) . ?
Ni O1 2.0473(16) 36_545 ?
Ni O1 2.0473(16) 21 ?
Ni O2 2.0923(16) 34 ?
Ni O2 2.0925(16) 19_655 ?
Ni N1 2.094(3) . ?
O1H Ni 1.9823(4) 2_655 ?
O1H Ni 1.9823(4) 3_665 ?
N1 C9 1.328(3) 16_544 ?
N1 C9 1.328(3) . ?
C1 C2 1.388(6) . ?
C1 C6 1.424(7) . ?
C2 C3 1.359(5) . ?
C4 C5 1.365(6) . ?
C4 C3 1.453(5) . ?
C5 C6 1.370(6) . ?
C6 C7 1.484(5) . ?
C1A C2A 1.375(9) . ?
C1A C6A 1.385(9) . ?
C2A C3 1.281(7) . ?
C4A C5A 1.350(11) . ?
C4A C3 1.509(8) . ?
C5A C6A 1.407(10) . ?
C6A C7 1.519(6) . ?
C3 C10 1.502(3) . ?
C7 C9 1.393(4) . ?
C7 C8 1.396(3) . ?
C8 C7 1.395(3) 16_544 ?
C10 O1 1.255(3) . ?
C10 O2 1.257(3) . ?
O2 Ni 2.0925(16) 19_655 ?
O1 Ni 2.0473(16) 20 ?

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
O1H Ni O1 92.07(5) . 36_545 ?
O1H Ni O1 92.07(5) . 21 ?
O1 Ni O1 175.86(9) 36_545 21 ?
O1H Ni O2 91.83(4) . 34 ?
O1 Ni O2 86.44(7) 36_545 34 ?
O1 Ni O2 93.43(7) 21 34 ?
O1H Ni O2 91.83(4) . 19_655 ?
O1 Ni O2 93.43(7) 36_545 19_655 ?
O1 Ni O2 86.44(7) 21 19_655 ?
O2 Ni O2 176.34(9) 34 19_655 ?
O1H Ni N1 180.00(14) . . ?
O1 Ni N1 87.93(5) 36_545 . ?
O1 Ni N1 87.93(5) 21 . ?
O2 Ni N1 88.17(4) 34 . ?
O2 Ni N1 88.17(4) 19_655 . ?
Ni O1H Ni 120.0 2_655 . ?
Ni O1H Ni 120.0 2_655 3_665 ?
Ni O1H Ni 120.0 . 3_665 ?
C9 N1 C9 118.2(3) 16_544 . ?
C9 N1 Ni 120.88(15) 16_544 . ?
C9 N1 Ni 120.88(15) . . ?
C2 C1 C6 120.1(4) . . ?
C3 C2 C1 121.9(4) . . ?
C5 C4 C3 120.9(4) . . ?
C4 C5 C6 121.3(4) . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C7 121.8(4) . . ?
C1 C6 C7 118.7(4) . . ?
C2A C1A C6A 120.1(6) . . ?
C3 C2A C1A 124.8(6) . . ?
C5A C4A C3 117.3(7) . . ?
C4A C5A C6A 122.4(8) . . ?
C1A C6A C5A 117.0(6) . . ?
C1A C6A C7 117.0(5) . . ?
C5A C6A C7 124.5(5) . . ?
C2A C3 C2 31.7(3) . . ?
C2A C3 C4 98.0(4) . . ?
C2 C3 C4 116.1(3) . . ?
C2A C3 C10 126.9(4) . . ?
C2 C3 C10 124.0(3) . . ?
C4 C3 C10 118.5(3) . . ?
C2A C3 C4A 115.8(5) . . ?
C2 C3 C4A 98.8(4) . . ?
C4 C3 C4A 64.6(3) . . ?
C10 C3 C4A 114.4(4) . . ?
C9 C7 C8 117.2(2) . . ?
C9 C7 C6 119.9(3) . . ?
C8 C7 C6 121.9(3) . . ?
C9 C7 C6A 115.5(3) . . ?
C8 C7 C6A 126.1(3) . . ?
C6 C7 C6A 20.3(2) . . ?
C7 C8 C7 119.9(3) 16_544 . ?
N1 C9 C7 123.7(2) . . ?
O1 C10 O2 127.1(2) . . ?
O1 C10 C3 116.7(2) . . ?
O2 C10 C3 116.2(2) . . ?
C10 O2 Ni 133.31(15) . 19_655 ?
C10 O1 Ni 126.14(15) . 20 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.071

# Attachment 'Compound_2.cif'

data_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 622765'

_refine_special_details          
;
# SQUEEZE RESULTS (APPEND TO CIF)
#loop_
#_platon_squeeze_void_nr
#_platon_squeeze_void_average_x
#_platon_squeeze_void_average_y
#_platon_squeeze_void_average_z
#_platon_squeeze_void_volume
#_platon_squeeze_void_count_electrons
#1 -0.058 0.005 -0.001 7828.8 1004.8
#_platon_squeeze_details
The electrons found correspond to 4DMF/Fe3.
These molecules have been included in the formula.
Phenyl rings modelled over two partially occupied sites C4-C9
with occupancy 0.7 and C4'- C9' with occupancy 0.3.
C-C bond distances of disordered phenyl rings are restrained.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H33 Fe3 N3 O13,4(C3H7NO)'
_chemical_formula_sum            'C69 H61 Fe3 N7 O17'
_chemical_formula_weight         1427.80

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           Trigonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   19.2442(14)
_cell_length_b                   19.2442(14)
_cell_length_c                   45.613(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14629(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2727
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      21.63

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.033
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.024
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    0.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4476
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   '(SADABS version 2.10; Bruker, 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.6906
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury Laboratory Station 9.8'
_diffrn_radiation_monochromator  'silicon (111)'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28211
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.38
_reflns_number_total             3333
_reflns_number_gt                2246
_reflns_threshold_expression     >2\s(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_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^)+(0.1043P)^2^] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3333
_refine_ls_number_parameters     111
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1772
_refine_ls_wR_factor_gt          0.1668
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.015
_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
Fe Fe 0.56783(3) 0.3333 0.0833 0.0307(2) Uani 1 2 d S . .
N1 N 0.4529(2) 0.3333 0.0833 0.0370(9) Uani 1 2 d S . .
C1 C 0.4344(2) 0.3688(2) 0.06189(7) 0.0438(9) Uani 1 1 d . A .
H1A H 0.4723 0.3946 0.0466 0.053 Uiso 1 1 calc R . .
C2 C 0.3623(2) 0.3700(3) 0.06076(9) 0.0576(11) Uani 1 1 d . . .
C3 C 0.3079(3) 0.3333 0.0833 0.0640(18) Uani 1 2 d S . .
H3A H 0.2586 0.3333 0.0833 0.077 Uiso 1 2 calc SR . .
C10 C 0.32804(19) 0.5303(2) -0.04061(7) 0.0359(8) Uani 1 1 d . . .
O2 O 0.39255(13) 0.57218(14) -0.05459(5) 0.0406(6) Uani 1 1 d . . .
O1 O 0.26053(14) 0.52102(14) -0.04746(5) 0.0403(6) Uani 1 1 d . . .
C4 C 0.3519(3) 0.4196(3) 0.03771(12) 0.0379(13) Uiso 0.70 1 d PD A 1
C5 C 0.4164(3) 0.4892(3) 0.02710(10) 0.0438(12) Uiso 0.70 1 d PD A 1
H5A H 0.4667 0.5118 0.0369 0.053 Uiso 0.70 1 calc PR A 1
C6 C 0.4087(3) 0.5263(3) 0.00236(10) 0.0440(12) Uiso 0.70 1 d PD A 1
H6A H 0.4541 0.5732 -0.0050 0.053 Uiso 0.70 1 calc PR A 1
C7 C 0.3357(3) 0.4958(3) -0.01172(12) 0.0341(14) Uiso 0.70 1 d PD A 1
C8 C 0.2690(3) 0.4259(3) -0.00109(12) 0.0476(13) Uiso 0.70 1 d PD A 1
H8A H 0.2188 0.4045 -0.0108 0.057 Uiso 0.70 1 calc PR A 1
C9 C 0.2765(4) 0.3880(4) 0.02363(12) 0.0528(15) Uiso 0.70 1 d PD A 1
H9A H 0.2312 0.3412 0.0311 0.063 Uiso 0.70 1 calc PR A 1
C4' C 0.3448(5) 0.3936(6) 0.03095(19) 0.019(2) Uiso 0.30 1 d PD A 2
C5' C 0.3890(7) 0.4082(7) 0.00510(19) 0.046(3) Uiso 0.30 1 d PD A 2
H5'A H 0.4260 0.3893 0.0040 0.055 Uiso 0.30 1 calc PR A 2
C6' C 0.3826(6) 0.4483(6) -0.0189(2) 0.042(3) Uiso 0.30 1 d PD A 2
H6'A H 0.4145 0.4569 -0.0359 0.050 Uiso 0.30 1 calc PR A 2
C7' C 0.3285(6) 0.4756(7) -0.0176(2) 0.018(2) Uiso 0.30 1 d PD A 2
C8' C 0.2831(6) 0.4617(6) 0.00755(17) 0.028(2) Uiso 0.30 1 d PD A 2
H8'A H 0.2454 0.4799 0.0082 0.034 Uiso 0.30 1 calc PR A 2
C9' C 0.2906(7) 0.4224(7) 0.0317(2) 0.033(2) Uiso 0.30 1 d PD A 2
H9'A H 0.2591 0.4149 0.0487 0.040 Uiso 0.30 1 calc PR A 2
O1H O 0.6667 0.3333 0.0833 0.0335(12) Uani 1 6 d S . .

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 0.0367(3) 0.0343(4) 0.0204(3) 0.0012(3) 0.00062(13) 0.01717(19)
N1 0.0424(16) 0.044(2) 0.0252(18) 0.0099(17) 0.0049(8) 0.0220(11)
C1 0.042(2) 0.056(2) 0.0313(17) 0.0129(16) 0.0015(15) 0.0232(18)
C2 0.046(2) 0.079(3) 0.051(2) 0.033(2) 0.0130(18) 0.033(2)
C3 0.054(2) 0.091(5) 0.060(4) 0.048(3) 0.0239(17) 0.045(2)
C10 0.0341(18) 0.0404(18) 0.0336(17) 0.0064(14) 0.0063(14) 0.0189(15)
O2 0.0362(13) 0.0495(14) 0.0409(13) 0.0138(11) 0.0062(10) 0.0250(12)
O1 0.0374(13) 0.0488(14) 0.0345(12) 0.0096(10) 0.0031(10) 0.0214(11)
O1H 0.0371(18) 0.0371(18) 0.026(3) 0.000 0.000 0.0185(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
Fe O1H 1.9020(7) . ?
Fe O1 2.047(2) 36 ?
Fe O1 2.047(2) 20 ?
Fe O2 2.054(2) 35_545 ?
Fe O2 2.054(2) 19_665 ?
Fe N1 2.212(4) . ?
N1 C1 1.338(4) 17_554 ?
N1 C1 1.338(4) . ?
C1 C2 1.400(5) . ?
C2 C3 1.384(5) . ?
C2 C4 1.500(6) . ?
C2 C4' 1.524(9) . ?
C3 C2 1.384(5) 17_554 ?
C10 O1 1.259(4) . ?
C10 O2 1.263(4) . ?
C10 C7' 1.492(9) . ?
C10 C7 1.516(6) . ?
O2 Fe 2.054(2) 19_665 ?
O1 Fe 2.047(2) 21 ?
C4 C5 1.381(5) . ?
C4 C9 1.417(8) . ?
C5 C6 1.382(5) . ?
C6 C7 1.381(5) . ?
C7 C8 1.401(5) . ?
C8 C9 1.388(5) . ?
C4' C5' 1.398(7) . ?
C4' C9' 1.405(14) . ?
C5' C6' 1.380(7) . ?
C6' C7' 1.380(7) . ?
C7' C8' 1.384(7) . ?
C8' C9' 1.382(7) . ?
O1H Fe 1.9020(7) 2_655 ?
O1H Fe 1.9020(7) 3_665 ?

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
O1H Fe O1 95.60(7) . 36 ?
O1H Fe O1 95.60(7) . 20 ?
O1 Fe O1 168.79(13) 36 20 ?
O1H Fe O2 94.09(6) . 35_545 ?
O1 Fe O2 86.42(10) 36 35_545 ?
O1 Fe O2 92.78(10) 20 35_545 ?
O1H Fe O2 94.10(6) . 19_665 ?
O1 Fe O2 92.79(10) 36 19_665 ?
O1 Fe O2 86.41(10) 20 19_665 ?
O2 Fe O2 171.81(13) 35_545 19_665 ?
O1H Fe N1 180.0 . . ?
O1 Fe N1 84.40(7) 36 . ?
O1 Fe N1 84.40(7) 20 . ?
O2 Fe N1 85.91(6) 35_545 . ?
O2 Fe N1 85.90(6) 19_665 . ?
C1 N1 C1 117.3(4) 17_554 . ?
C1 N1 Fe 121.4(2) 17_554 . ?
C1 N1 Fe 121.4(2) . . ?
N1 C1 C2 123.6(3) . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C4 122.5(4) . . ?
C1 C2 C4 119.0(3) . . ?
C3 C2 C4' 126.3(5) . . ?
C1 C2 C4' 114.0(4) . . ?
C2 C3 C2 119.8(5) 17_554 . ?
O1 C10 O2 125.5(3) . . ?
O1 C10 C7' 116.4(4) . . ?
O2 C10 C7' 117.0(4) . . ?
O1 C10 C7 118.2(3) . . ?
O2 C10 C7 116.0(3) . . ?
C10 O2 Fe 134.2(2) . 19_665 ?
C10 O1 Fe 126.7(2) . 21 ?
C5 C4 C9 119.3(5) . . ?
C5 C4 C2 121.4(4) . . ?
C9 C4 C2 118.7(4) . . ?
C4 C5 C6 120.6(5) . . ?
C7 C6 C5 120.6(5) . . ?
C6 C7 C8 119.7(5) . . ?
C6 C7 C10 121.3(4) . . ?
C8 C7 C10 118.6(4) . . ?
C9 C8 C7 120.0(5) . . ?
C8 C9 C4 119.7(5) . . ?
C5' C4' C9' 115.9(8) . . ?
C5' C4' C2 127.5(8) . . ?
C9' C4' C2 114.6(7) . . ?
C6' C5' C4' 124.5(10) . . ?
C7' C6' C5' 118.2(9) . . ?
C6' C7' C8' 119.2(9) . . ?
C6' C7' C10 120.6(7) . . ?
C8' C7' C10 119.5(7) . . ?
C9' C8' C7' 122.3(9) . . ?
C8' C9' C4' 119.9(9) . . ?
Fe O1H Fe 120.0 2_655 3_665 ?
Fe O1H Fe 120.0 2_655 . ?
Fe O1H Fe 120.0 3_665 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.075