# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global
_publ_contact_author_email       duancy@nju.edu.cn

_publ_contact_author_name        'Dr. Duan Chun-ying'
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_publ_contact_author_address     
;
Coordination Chemistry Institute
The State Key Laboratory of Coordinaiton Chemistry
Nanjing University , Nanjing 210093
P. R. China
;
_publ_contact_author_fax         '00 86 25 331 4502'
_publ_contact_author_phone       '00 86 25 359 7006'
_publ_requested_category         ?

#============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title              
;
A three dimensional porous metal-organic framework [Fe4L6¡Á(DMF)3¡Á(H2O)10]
constructed from neutral discrete Fe4L6 pyramids
[H2L = 1,3-benzodihydroxamix acid]
;

loop_
_publ_author_name
_publ_author_address

'Bai Yan'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;
'Guo Dong'
;
Department of Chemistry, Wuhan University, Wuhan, P. R. China.
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;
'Duan Chun-ying'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;
'Pang Ke-liang'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;
'Meng Qing-jin'
;
Coordination Chemistry Institute and State Key Laboratory of
Coordination Chemistry, Nanjing University,Nanjing,210093,
People's Republic of China
;

#=====================================================================
data_sad
_database_code_depnum_ccdc_archive 'CCDC 201192'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H77 Fe4 N15 O37'
_chemical_formula_weight         1787.74

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           Cubic
_symmetry_space_group_name_H-M   'P2(1)3  '

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

_cell_length_a                   27.6415(17)
_cell_length_b                   27.6415(17)
_cell_length_c                   27.6415(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     21120(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3669
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      13.38

_exptl_crystal_description       block
_exptl_crystal_colour            drak-red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7392
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            85354
_diffrn_reflns_av_R_equivalents  0.1388
_diffrn_reflns_av_sigmaI/netI    0.2881
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         24.99
_reflns_number_total             12377
_reflns_number_gt                4010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0700P)^2^+0.0000P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(3)
_refine_ls_number_reflns         12377
_refine_ls_number_parameters     654
_refine_ls_number_restraints     408
_refine_ls_R_factor_all          0.2415
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.2086
_refine_ls_wR_factor_gt          0.1785
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.39165(5) 0.10835(5) 0.89165(5) 0.0568(8) Uani 1 3 d S . .
Fe2 Fe 0.56458(6) -0.16051(6) 0.90140(6) 0.0712(6) Uani 1 1 d . . .
O11 O 0.4185(2) 0.0418(2) 0.8707(2) 0.0533(19) Uani 1 1 d U . .
O12 O 0.4011(3) 0.1156(3) 0.8215(2) 0.065(2) Uani 1 1 d U . .
O13 O 0.5206(3) -0.1091(2) 0.8737(3) 0.068(2) Uani 1 1 d U . .
O14 O 0.5267(3) -0.1972(2) 0.8531(3) 0.079(3) Uani 1 1 d U . .
O15 O 0.6077(3) -0.1122(3) 0.9373(3) 0.073(2) Uani 1 1 d U . .
O16 O 0.6228(3) -0.1564(3) 0.8594(3) 0.088(3) Uani 1 1 d U . .
O17 O 0.6667(3) 0.0368(3) 1.0241(3) 0.081(2) Uani 1 1 d U . .
O18 O 0.7221(3) 0.0715(3) 1.0899(3) 0.086(3) Uani 1 1 d U . .
N11 N 0.4087(3) 0.0732(4) 0.8011(3) 0.062(3) Uani 1 1 d U . .
H11A H 0.4079 0.0706 0.7701 0.074 Uiso 1 1 calc R . .
N12 N 0.4980(4) -0.1676(4) 0.8282(4) 0.081(3) Uani 1 1 d U . .
H12A H 0.4812 -0.1789 0.8046 0.097 Uiso 1 1 calc R . .
N13 N 0.6608(4) -0.1379(4) 0.8844(4) 0.095(3) Uani 1 1 d U . .
H13A H 0.6900 -0.1416 0.8745 0.115 Uiso 1 1 calc R . .
N14 N 0.7379(4) 0.0306(4) 1.0657(4) 0.077(3) Uani 1 1 d U . .
H14A H 0.7656 0.0174 1.0711 0.093 Uiso 1 1 d R . .
C1 C 0.4174(4) 0.0361(4) 0.8267(4) 0.052(3) Uani 1 1 d U . .
C2 C 0.4268(5) -0.0095(5) 0.8036(4) 0.080(3) Uani 1 1 d U . .
C3 C 0.4544(4) -0.0434(4) 0.8311(4) 0.060(3) Uani 1 1 d U . .
H3A H 0.4662 -0.0346 0.8613 0.072 Uiso 1 1 calc R . .
C4 C 0.4642(5) -0.0922(4) 0.8120(4) 0.073(3) Uani 1 1 d U . .
C5 C 0.4477(6) -0.1016(5) 0.7673(5) 0.107(4) Uani 1 1 d U . .
H5A H 0.4546 -0.1315 0.7534 0.129 Uiso 1 1 calc R . .
C6 C 0.4199(6) -0.0671(5) 0.7399(5) 0.115(5) Uani 1 1 d U . .
H6A H 0.4103 -0.0743 0.7085 0.138 Uiso 1 1 calc R . .
C7 C 0.4075(6) -0.0227(5) 0.7605(5) 0.112(4) Uani 1 1 d U . .
H7A H 0.3859 -0.0023 0.7447 0.135 Uiso 1 1 calc R . .
C8 C 0.4951(5) -0.1237(5) 0.8383(5) 0.063(3) Uani 1 1 d U . .
C9 C 0.6511(5) -0.1142(5) 0.9240(5) 0.077(4) Uani 1 1 d U . .
C10 C 0.6889(5) -0.0930(4) 0.9503(5) 0.067(3) Uani 1 1 d U . .
C11 C 0.6810(4) -0.0543(5) 0.9767(4) 0.067(3) Uani 1 1 d U . .
H11B H 0.6503 -0.0406 0.9761 0.081 Uiso 1 1 calc R . .
C12 C 0.7151(5) -0.0331(5) 1.0046(5) 0.077(3) Uani 1 1 d U . .
C13 C 0.7632(5) -0.0523(5) 1.0054(5) 0.093(4) Uani 1 1 d U . .
H13B H 0.7881 -0.0367 1.0218 0.112 Uiso 1 1 calc R . .
C14 C 0.7707(5) -0.0956(5) 0.9805(5) 0.082(4) Uani 1 1 d U . .
H14B H 0.8006 -0.1107 0.9827 0.099 Uiso 1 1 calc R . .
C15 C 0.7360(5) -0.1159(5) 0.9533(5) 0.085(4) Uani 1 1 d U . .
H15A H 0.7421 -0.1444 0.9366 0.102 Uiso 1 1 calc R . .
C16 C 0.7072(5) 0.0136(5) 1.0342(5) 0.076(3) Uani 1 1 d U . .
Fe3 Fe 0.38132(6) -0.38132(6) 1.11868(6) 0.0723(9) Uani 1 3 d S . .
Fe4 Fe 0.53962(6) -0.39641(6) 0.84083(6) 0.0675(5) Uani 1 1 d . . .
O21 O 0.4069(3) -0.3573(3) 1.0530(3) 0.078(2) Uani 1 1 d U . .
O22 O 0.3323(3) -0.3338(3) 1.0967(3) 0.069(2) Uani 1 1 d U . .
O23 O 0.4953(3) -0.3709(3) 0.8940(2) 0.066(2) Uani 1 1 d U . .
O24 O 0.5517(3) -0.3253(3) 0.8371(3) 0.081(2) Uani 1 1 d U . .
O25 O 0.5890(3) -0.4185(3) 0.8922(3) 0.069(2) Uani 1 1 d U . .
O26 O 0.5957(3) -0.4133(3) 0.8006(2) 0.078(3) Uani 1 1 d U . .
O27 O 0.6571(3) -0.5043(3) 1.0378(2) 0.066(2) Uani 1 1 d U . .
O28 O 0.7182(2) -0.4999(3) 1.1073(3) 0.075(2) Uani 1 1 d U . .
N21 N 0.3481(4) -0.3106(4) 1.0589(4) 0.074(3) Uani 1 1 d U . .
H21A H 0.3313 -0.2860 1.0498 0.088 Uiso 1 1 calc R . .
N22 N 0.5194(4) -0.3007(4) 0.8660(4) 0.077(3) Uani 1 1 d U . .
H22A H 0.5187 -0.2696 0.8657 0.092 Uiso 1 1 calc R . .
N23 N 0.6340(4) -0.4221(3) 0.8270(4) 0.075(3) Uani 1 1 d U . .
H23A H 0.6615 -0.4271 0.8135 0.090 Uiso 1 1 calc R . .
N24 N 0.7266(3) -0.4778(3) 1.0654(4) 0.077(3) Uani 1 1 d U . .
H24A H 0.7528 -0.4618 1.0605 0.092 Uiso 1 1 calc R . .
C17 C 0.3855(5) -0.3202(4) 1.0339(5) 0.065(3) Uani 1 1 d U . .
C18 C 0.4040(5) -0.2990(5) 0.9904(5) 0.068(3) Uani 1 1 d U . .
C19 C 0.4387(4) -0.3209(4) 0.9639(4) 0.062(3) Uani 1 1 d U . .
H19A H 0.4502 -0.3510 0.9736 0.074 Uiso 1 1 calc R . .
C20 C 0.4572(5) -0.3004(5) 0.9236(5) 0.068(3) Uani 1 1 d U . .
C21 C 0.4396(6) -0.2569(5) 0.9096(5) 0.100(4) Uani 1 1 d U . .
H21B H 0.4516 -0.2420 0.8819 0.120 Uiso 1 1 calc R . .
C22 C 0.4007(6) -0.2325(6) 0.9390(6) 0.131(5) Uani 1 1 d U . .
H22B H 0.3870 -0.2032 0.9298 0.157 Uiso 1 1 calc R . .
C23 C 0.3871(6) -0.2558(5) 0.9790(5) 0.107(4) Uani 1 1 d U . .
H23B H 0.3650 -0.2410 0.9996 0.129 Uiso 1 1 calc R . .
C24 C 0.4898(5) -0.3245(5) 0.8939(4) 0.061(3) Uani 1 1 d U . .
C25 C 0.6300(5) -0.4231(4) 0.8742(5) 0.062(3) Uani 1 1 d U . .
C26 C 0.6730(5) -0.4304(4) 0.9040(4) 0.070(3) Uani 1 1 d U . .
C27 C 0.6652(4) -0.4516(4) 0.9524(4) 0.066(3) Uani 1 1 d U . .
H27A H 0.6346 -0.4619 0.9621 0.079 Uiso 1 1 calc R . .
C28 C 0.7058(5) -0.4558(4) 0.9835(4) 0.072(3) Uani 1 1 d U . .
C29 C 0.7519(5) -0.4438(4) 0.9682(5) 0.089(4) Uani 1 1 d U . .
H29A H 0.7784 -0.4489 0.9883 0.107 Uiso 1 1 calc R . .
C30 C 0.7583(5) -0.4236(5) 0.9218(5) 0.091(4) Uani 1 1 d U . .
H30A H 0.7891 -0.4142 0.9119 0.109 Uiso 1 1 calc R . .
C31 C 0.7211(5) -0.4177(4) 0.8918(5) 0.084(4) Uani 1 1 d U . .
H31A H 0.7270 -0.4045 0.8614 0.101 Uiso 1 1 calc R . .
C32 C 0.6930(5) -0.4814(5) 1.0313(5) 0.070(3) Uani 1 1 d U . .
N31 N 0.3912(5) -0.0703(5) 0.9685(4) 0.108(3) Uani 1 1 d U . .
O31 O 0.3173(4) -0.0641(4) 0.9340(4) 0.130(3) Uani 1 1 d U . .
C33 C 0.3593(6) -0.0478(6) 0.9413(6) 0.114(4) Uani 1 1 d U . .
H33A H 0.3681 -0.0188 0.9268 0.137 Uiso 1 1 calc R . .
C34 C 0.3744(5) -0.1135(6) 1.0008(6) 0.152(5) Uani 1 1 d U . .
H34A H 0.3419 -0.1223 0.9923 0.228 Uiso 1 1 calc R . .
H34B H 0.3754 -0.1041 1.0343 0.228 Uiso 1 1 calc R . .
H34C H 0.3955 -0.1406 0.9958 0.228 Uiso 1 1 calc R . .
C35 C 0.4394(5) -0.0540(6) 0.9768(6) 0.135(5) Uani 1 1 d U . .
H35A H 0.4462 -0.0269 0.9561 0.202 Uiso 1 1 calc R . .
H35B H 0.4617 -0.0797 0.9698 0.202 Uiso 1 1 calc R . .
H35C H 0.4429 -0.0443 1.0100 0.202 Uiso 1 1 calc R . .
O32 O 0.8268(6) 0.0016(7) 1.0961(7) 0.221(7) Uani 1 1 d U . .
N32 N 0.8903(8) -0.0301(8) 1.0687(8) 0.229(6) Uani 1 1 d U . .
C36 C 0.8564(10) 0.0150(14) 1.0738(12) 0.221(8) Uani 1 1 d U . .
H36A H 0.8605 0.0458 1.0608 0.265 Uiso 1 1 calc R . .
C37 C 0.9404(9) -0.0242(9) 1.0279(9) 0.278(10) Uani 1 1 d U . .
H37A H 0.9402 0.0076 1.0138 0.417 Uiso 1 1 calc R . .
H37B H 0.9376 -0.0479 1.0027 0.417 Uiso 1 1 calc R . .
H37C H 0.9701 -0.0290 1.0452 0.417 Uiso 1 1 calc R . .
C38 C 0.8775(8) -0.0763(8) 1.1053(10) 0.254(9) Uani 1 1 d U . .
H38A H 0.8497 -0.0685 1.1245 0.381 Uiso 1 1 calc R . .
H38B H 0.9047 -0.0824 1.1261 0.381 Uiso 1 1 calc R . .
H38C H 0.8709 -0.1046 1.0863 0.381 Uiso 1 1 calc R . .
O1W O 0.7468(4) -0.1715(4) 0.8437(4) 0.147(4) Uiso 1 1 d . . .
O2W O 0.5574(6) -0.2338(5) 0.7103(6) 0.225(6) Uiso 1 1 d . . .
O3W O 0.5253(6) -0.3215(6) 0.7103(6) 0.254(7) Uiso 1 1 d . . .
O4W O 0.4417(7) -0.2326(6) 0.7654(6) 0.258(8) Uiso 1 1 d . . .
O5W O 0.7734(7) 0.0449(7) 1.2876(7) 0.258(8) Uiso 0.92 1 d P . .
O6W O 0.7840(9) 0.0681(9) 1.2112(8) 0.243(10) Uiso 0.67 1 d P . .
O7W O 0.6216(12) -0.2343(11) 0.7861(11) 0.239(13) Uiso 0.50 1 d P . .
O8W O 0.7654(8) -0.2346(8) 0.7654(8) 0.225(15) Uiso 0.75 3 d SP . .
O9W O 0.4282(11) -0.0718(11) 0.5718(11) 0.23(2) Uiso 0.50 3 d SP . .
O10W O 0.5771(9) -0.0771(9) 1.0771(9) 0.180(17) Uiso 0.50 3 d SP . .

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 0.0568(8) 0.0568(8) 0.0568(8) 0.0069(9) -0.0069(9) 0.0069(9)
Fe2 0.0811(13) 0.0492(11) 0.0833(14) -0.0073(10) 0.0109(11) 0.0017(10)
O11 0.085(5) 0.049(5) 0.026(4) -0.012(4) -0.008(4) -0.001(4)
O12 0.106(6) 0.047(5) 0.041(4) 0.004(4) 0.008(4) 0.016(5)
O13 0.077(6) 0.046(5) 0.081(6) -0.016(4) 0.016(5) -0.005(4)
O14 0.100(7) 0.028(5) 0.109(7) -0.007(5) -0.006(5) 0.004(4)
O15 0.060(5) 0.069(5) 0.092(6) -0.010(4) 0.004(5) -0.010(5)
O16 0.091(7) 0.101(6) 0.074(6) -0.012(5) 0.025(5) -0.006(5)
O17 0.057(5) 0.104(6) 0.082(6) -0.004(5) -0.009(5) 0.009(5)
O18 0.055(5) 0.109(7) 0.093(6) -0.030(6) -0.024(5) 0.012(5)
N11 0.093(7) 0.054(6) 0.039(6) 0.002(5) 0.014(5) 0.002(6)
N12 0.105(8) 0.048(7) 0.090(7) -0.013(6) -0.022(6) 0.005(6)
N13 0.067(7) 0.130(9) 0.090(8) -0.013(7) 0.004(7) -0.035(7)
N14 0.055(7) 0.092(8) 0.084(8) -0.003(6) -0.020(6) -0.002(6)
C1 0.098(7) 0.027(6) 0.030(6) 0.002(6) 0.009(6) 0.006(6)
C2 0.141(9) 0.062(8) 0.036(7) 0.015(6) -0.014(7) 0.000(7)
C3 0.070(7) 0.050(7) 0.060(7) -0.009(6) 0.001(6) -0.002(6)
C4 0.113(8) 0.056(7) 0.050(7) 0.002(6) -0.039(7) 0.001(7)
C5 0.183(11) 0.055(8) 0.083(9) -0.023(7) -0.045(9) 0.023(8)
C6 0.195(12) 0.071(9) 0.077(9) -0.020(8) -0.066(9) 0.005(9)
C7 0.202(12) 0.057(8) 0.078(9) 0.000(7) -0.048(9) 0.026(9)
C8 0.090(8) 0.041(7) 0.059(7) -0.026(7) -0.003(7) 0.009(7)
C9 0.071(8) 0.072(8) 0.090(8) -0.014(7) 0.012(8) 0.005(8)
C10 0.050(7) 0.056(7) 0.096(8) -0.031(6) 0.004(7) 0.001(6)
C11 0.040(7) 0.082(9) 0.080(8) 0.007(7) -0.012(6) -0.009(7)
C12 0.072(8) 0.081(8) 0.079(8) 0.012(7) 0.016(7) 0.003(7)
C13 0.091(9) 0.081(9) 0.107(9) -0.015(8) 0.001(8) 0.009(8)
C14 0.088(9) 0.066(8) 0.093(9) -0.013(7) -0.003(7) 0.007(7)
C15 0.081(9) 0.071(8) 0.104(9) 0.000(7) -0.001(8) -0.041(7)
C16 0.055(8) 0.087(8) 0.086(9) 0.012(7) 0.033(7) 0.012(7)
Fe3 0.0723(9) 0.0723(9) 0.0723(9) -0.0055(10) 0.0055(10) 0.0055(10)
Fe4 0.1076(15) 0.0496(11) 0.0454(11) -0.0014(9) -0.0006(10) -0.0124(10)
O21 0.095(6) 0.083(6) 0.057(5) -0.015(4) 0.022(5) 0.013(5)
O22 0.067(5) 0.081(6) 0.057(5) 0.007(5) 0.016(4) 0.008(5)
O23 0.084(5) 0.053(5) 0.063(5) -0.004(5) 0.023(4) 0.003(4)
O24 0.119(7) 0.065(6) 0.061(5) -0.016(4) 0.004(5) -0.026(5)
O25 0.080(6) 0.074(5) 0.052(5) 0.010(4) 0.014(5) -0.004(5)
O26 0.114(7) 0.083(6) 0.037(5) -0.002(4) -0.025(5) 0.008(5)
O27 0.046(5) 0.088(6) 0.065(5) 0.028(4) -0.001(4) -0.026(4)
O28 0.064(5) 0.122(7) 0.038(5) 0.020(5) -0.012(4) -0.021(4)
N21 0.071(7) 0.080(7) 0.071(7) -0.003(6) 0.014(6) 0.022(6)
N22 0.101(8) 0.058(7) 0.072(7) -0.036(6) 0.005(6) -0.013(6)
N23 0.093(8) 0.087(7) 0.046(7) -0.010(6) 0.019(6) -0.006(6)
N24 0.059(6) 0.095(7) 0.076(8) 0.008(6) -0.007(6) -0.031(6)
C17 0.071(8) 0.051(7) 0.072(8) -0.004(6) -0.025(7) 0.036(6)
C18 0.094(8) 0.053(7) 0.055(7) 0.026(6) -0.007(7) 0.008(7)
C19 0.074(8) 0.055(8) 0.057(8) -0.002(6) -0.005(7) -0.007(6)
C20 0.094(8) 0.050(7) 0.060(8) -0.012(7) -0.009(7) 0.009(7)
C21 0.137(11) 0.099(10) 0.065(9) 0.005(8) 0.002(8) -0.009(9)
C22 0.162(12) 0.125(11) 0.106(11) 0.016(9) 0.006(10) 0.025(10)
C23 0.152(11) 0.098(10) 0.072(9) 0.049(8) 0.037(8) 0.024(9)
C24 0.077(8) 0.053(7) 0.053(7) 0.001(7) 0.018(6) -0.022(7)
C25 0.072(8) 0.061(7) 0.051(7) -0.001(6) -0.007(7) -0.015(7)
C26 0.069(8) 0.081(7) 0.061(7) -0.006(6) 0.002(7) -0.012(7)
C27 0.055(7) 0.094(8) 0.050(7) 0.004(6) 0.011(6) 0.009(7)
C28 0.080(8) 0.083(8) 0.053(7) 0.014(6) -0.013(7) -0.003(7)
C29 0.068(8) 0.096(9) 0.103(10) 0.036(8) -0.002(8) -0.014(7)
C30 0.065(9) 0.125(10) 0.083(10) 0.017(8) 0.006(7) -0.036(8)
C31 0.072(9) 0.099(9) 0.081(9) 0.006(8) 0.020(8) -0.016(8)
C32 0.070(8) 0.087(8) 0.052(7) 0.012(7) -0.002(7) -0.011(7)
N31 0.085(7) 0.133(8) 0.105(7) 0.010(6) 0.003(7) 0.029(7)
O31 0.083(7) 0.189(9) 0.117(7) 0.024(7) -0.007(6) 0.053(7)
C33 0.098(8) 0.141(9) 0.105(8) 0.007(7) -0.002(8) 0.034(8)
C34 0.128(11) 0.177(12) 0.152(11) 0.025(10) -0.016(10) 0.043(10)
C35 0.096(10) 0.163(11) 0.144(11) -0.006(10) 0.006(10) -0.019(10)
O32 0.193(15) 0.208(14) 0.261(17) -0.047(12) -0.090(13) 0.047(12)
N32 0.209(14) 0.204(13) 0.274(17) -0.018(12) -0.057(12) 0.023(13)
C36 0.204(16) 0.198(15) 0.261(18) -0.027(14) -0.062(14) 0.016(14)
C37 0.23(2) 0.235(18) 0.36(2) -0.033(19) -0.113(17) -0.004(18)
C38 0.219(17) 0.184(17) 0.36(2) -0.005(17) -0.001(18) 0.042(16)

_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 O12 1.968(6) 12_565 ?
Fe1 O12 1.968(6) . ?
Fe1 O12 1.968(6) 6_456 ?
Fe1 O11 2.067(6) 12_565 ?
Fe1 O11 2.067(6) . ?
Fe1 O11 2.067(6) 6_456 ?
Fe2 O14 1.977(8) . ?
Fe2 O18 1.987(7) 6_456 ?
Fe2 O16 1.988(8) . ?
Fe2 O13 2.020(8) . ?
Fe2 O15 2.045(7) . ?
Fe2 O17 2.050(8) 6_456 ?
O11 C1 1.225(10) . ?
O12 N11 1.319(9) . ?
O13 C8 1.274(12) . ?
O14 N12 1.331(10) . ?
O15 C9 1.256(13) . ?
O16 N13 1.356(10) . ?
O17 C16 1.320(14) . ?
O17 Fe2 2.050(8) 12_565 ?
O18 N14 1.383(11) . ?
O18 Fe2 1.987(7) 12_565 ?
N11 C1 1.268(11) . ?
N12 C8 1.247(12) . ?
N13 C9 1.305(14) . ?
N14 C16 1.302(15) . ?
C1 C2 1.436(14) . ?
C2 C7 1.356(15) . ?
C2 C3 1.427(14) . ?
C3 C4 1.473(14) . ?
C4 C5 1.344(14) . ?
C4 C8 1.419(15) . ?
C5 C6 1.440(17) . ?
C6 C7 1.394(16) . ?
C9 C10 1.402(16) . ?
C10 C11 1.314(14) . ?
C10 C15 1.448(15) . ?
C11 C12 1.351(15) . ?
C12 C13 1.429(16) . ?
C12 C16 1.546(17) . ?
C13 C14 1.398(15) . ?
C14 C15 1.341(14) . ?
Fe3 O22 1.983(7) 7_656 ?
Fe3 O22 1.983(7) . ?
Fe3 O22 1.983(7) 10_536 ?
Fe3 O21 2.057(7) 7_656 ?
Fe3 O21 2.057(7) . ?
Fe3 O21 2.057(7) 10_536 ?
Fe4 O26 1.963(8) . ?
Fe4 O28 1.971(7) 10_536 ?
Fe4 O24 1.998(7) . ?
Fe4 O23 2.039(7) . ?
Fe4 O25 2.063(7) . ?
Fe4 O27 2.064(7) 10_536 ?
O21 C17 1.297(11) . ?
O22 N21 1.300(10) . ?
O23 C24 1.294(12) . ?
O24 N22 1.379(10) . ?
O25 C25 1.242(12) . ?
O26 N23 1.308(11) . ?
O27 C32 1.191(13) . ?
O27 Fe4 2.064(7) 7_656 ?
O28 N24 1.330(11) . ?
O28 Fe4 1.971(7) 7_656 ?
N21 C17 1.272(13) . ?
N22 C24 1.302(12) . ?
N23 C25 1.310(13) . ?
N24 C32 1.326(13) . ?
C17 C18 1.431(16) . ?
C18 C23 1.321(15) . ?
C18 C19 1.352(14) . ?
C19 C20 1.351(14) . ?
C20 C21 1.352(15) . ?
C20 C24 1.389(15) . ?
C21 C22 1.508(19) . ?
C22 C23 1.333(16) . ?
C25 C26 1.460(15) . ?
C26 C31 1.417(15) . ?
C26 C27 1.475(14) . ?
C27 C28 1.420(14) . ?
C28 C29 1.384(15) . ?
C28 C32 1.540(15) . ?
C29 C30 1.412(15) . ?
C30 C31 1.330(15) . ?
N31 C33 1.315(17) . ?
N31 C35 1.425(15) . ?
N31 C34 1.563(17) . ?
O31 C33 1.262(16) . ?
O32 C36 1.09(3) . ?
N32 C36 1.57(4) . ?
N32 C38 1.67(3) . ?
N32 C37 1.79(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
O12 Fe1 O12 92.5(3) 12_565 . ?
O12 Fe1 O12 92.5(3) 12_565 6_456 ?
O12 Fe1 O12 92.5(3) . 6_456 ?
O12 Fe1 O11 76.5(3) 12_565 12_565 ?
O12 Fe1 O11 101.9(3) . 12_565 ?
O12 Fe1 O11 162.1(3) 6_456 12_565 ?
O12 Fe1 O11 162.1(3) 12_565 . ?
O12 Fe1 O11 76.5(3) . . ?
O12 Fe1 O11 101.9(3) 6_456 . ?
O11 Fe1 O11 91.8(3) 12_565 . ?
O12 Fe1 O11 101.9(3) 12_565 6_456 ?
O12 Fe1 O11 162.1(3) . 6_456 ?
O12 Fe1 O11 76.5(3) 6_456 6_456 ?
O11 Fe1 O11 91.8(3) 12_565 6_456 ?
O11 Fe1 O11 91.8(3) . 6_456 ?
O14 Fe2 O18 90.1(3) . 6_456 ?
O14 Fe2 O16 93.7(4) . . ?
O18 Fe2 O16 89.2(3) 6_456 . ?
O14 Fe2 O13 77.6(3) . . ?
O18 Fe2 O13 163.1(3) 6_456 . ?
O16 Fe2 O13 103.0(3) . . ?
O14 Fe2 O15 166.1(3) . . ?
O18 Fe2 O15 99.9(3) 6_456 . ?
O16 Fe2 O15 77.0(3) . . ?
O13 Fe2 O15 94.3(3) . . ?
O14 Fe2 O17 103.4(3) . 6_456 ?
O18 Fe2 O17 78.8(3) 6_456 6_456 ?
O16 Fe2 O17 159.0(3) . 6_456 ?
O13 Fe2 O17 92.6(3) . 6_456 ?
O15 Fe2 O17 88.1(3) . 6_456 ?
C1 O11 Fe1 112.5(7) . . ?
N11 O12 Fe1 110.5(5) . . ?
C8 O13 Fe2 113.7(7) . . ?
N12 O14 Fe2 110.5(6) . . ?
C9 O15 Fe2 112.7(9) . . ?
N13 O16 Fe2 110.5(6) . . ?
C16 O17 Fe2 111.0(8) . 12_565 ?
N14 O18 Fe2 114.1(6) . 12_565 ?
C1 N11 O12 120.8(9) . . ?
C8 N12 O14 121.4(11) . . ?
C9 N13 O16 117.3(12) . . ?
C16 N14 O18 114.3(11) . . ?
O11 C1 N11 117.0(10) . . ?
O11 C1 C2 123.3(10) . . ?
N11 C1 C2 119.6(11) . . ?
C7 C2 C3 120.0(12) . . ?
C7 C2 C1 123.8(12) . . ?
C3 C2 C1 115.9(11) . . ?
C2 C3 C4 120.6(11) . . ?
C5 C4 C8 123.7(13) . . ?
C5 C4 C3 116.3(11) . . ?
C8 C4 C3 119.4(11) . . ?
C4 C5 C6 122.4(12) . . ?
C7 C6 C5 120.0(12) . . ?
C2 C7 C6 119.9(13) . . ?
N12 C8 O13 116.4(12) . . ?
N12 C8 C4 121.5(13) . . ?
O13 C8 C4 122.1(11) . . ?
O15 C9 N13 117.6(14) . . ?
O15 C9 C10 122.9(13) . . ?
N13 C9 C10 119.5(14) . . ?
C11 C10 C9 120.3(12) . . ?
C11 C10 C15 118.2(12) . . ?
C9 C10 C15 121.2(12) . . ?
C10 C11 C12 123.6(13) . . ?
C11 C12 C13 119.8(13) . . ?
C11 C12 C16 124.5(14) . . ?
C13 C12 C16 115.6(13) . . ?
C14 C13 C12 116.5(13) . . ?
C15 C14 C13 121.9(14) . . ?
C14 C15 C10 119.4(13) . . ?
N14 C16 O17 121.3(13) . . ?
N14 C16 C12 124.2(13) . . ?
O17 C16 C12 114.4(14) . . ?
O22 Fe3 O22 87.7(3) 7_656 . ?
O22 Fe3 O22 87.7(3) 7_656 10_536 ?
O22 Fe3 O22 87.7(3) . 10_536 ?
O22 Fe3 O21 75.6(3) 7_656 7_656 ?
O22 Fe3 O21 158.3(3) . 7_656 ?
O22 Fe3 O21 105.0(3) 10_536 7_656 ?
O22 Fe3 O21 105.0(3) 7_656 . ?
O22 Fe3 O21 75.6(3) . . ?
O22 Fe3 O21 158.3(3) 10_536 . ?
O21 Fe3 O21 95.3(3) 7_656 . ?
O22 Fe3 O21 158.3(3) 7_656 10_536 ?
O22 Fe3 O21 105.0(3) . 10_536 ?
O22 Fe3 O21 75.6(3) 10_536 10_536 ?
O21 Fe3 O21 95.3(3) 7_656 10_536 ?
O21 Fe3 O21 95.3(3) . 10_536 ?
O26 Fe4 O28 89.1(3) . 10_536 ?
O26 Fe4 O24 94.2(3) . . ?
O28 Fe4 O24 89.9(3) 10_536 . ?
O26 Fe4 O23 164.7(3) . . ?
O28 Fe4 O23 104.2(3) 10_536 . ?
O24 Fe4 O23 78.3(3) . . ?
O26 Fe4 O25 78.2(3) . . ?
O28 Fe4 O25 162.7(3) 10_536 . ?
O24 Fe4 O25 102.5(3) . . ?
O23 Fe4 O25 90.2(3) . . ?
O26 Fe4 O27 100.3(3) . 10_536 ?
O28 Fe4 O27 78.8(3) 10_536 10_536 ?
O24 Fe4 O27 161.4(3) . 10_536 ?
O23 Fe4 O27 90.0(3) . 10_536 ?
O25 Fe4 O27 91.9(3) . 10_536 ?
C17 O21 Fe3 117.3(8) . . ?
N21 O22 Fe3 110.1(6) . . ?
C24 O23 Fe4 114.3(7) . . ?
N22 O24 Fe4 110.3(6) . . ?
C25 O25 Fe4 111.1(8) . . ?
N23 O26 Fe4 111.6(6) . . ?
C32 O27 Fe4 111.2(8) . 7_656 ?
N24 O28 Fe4 110.7(6) . 7_656 ?
C17 N21 O22 127.4(11) . . ?
C24 N22 O24 120.1(10) . . ?
O26 N23 C25 119.4(11) . . ?
C32 N24 O28 117.6(10) . . ?
N21 C17 O21 108.3(13) . . ?
N21 C17 C18 131.5(12) . . ?
O21 C17 C18 120.2(12) . . ?
C23 C18 C19 121.7(13) . . ?
C23 C18 C17 116.4(13) . . ?
C19 C18 C17 121.8(12) . . ?
C20 C19 C18 121.9(12) . . ?
C19 C20 C21 118.3(13) . . ?
C19 C20 C24 122.0(13) . . ?
C21 C20 C24 119.4(14) . . ?
C20 C21 C22 120.0(14) . . ?
C23 C22 C21 115.6(15) . . ?
C18 C23 C22 122.4(15) . . ?
O23 C24 N22 115.4(12) . . ?
O23 C24 C20 123.4(12) . . ?
N22 C24 C20 121.0(13) . . ?
O25 C25 N23 118.2(12) . . ?
O25 C25 C26 122.1(12) . . ?
N23 C25 C26 119.7(13) . . ?
C31 C26 C25 126.5(12) . . ?
C31 C26 C27 117.0(12) . . ?
C25 C26 C27 116.5(11) . . ?
C28 C27 C26 117.7(11) . . ?
C29 C28 C27 121.6(11) . . ?
C29 C28 C32 125.7(12) . . ?
C27 C28 C32 112.1(12) . . ?
C28 C29 C30 119.2(12) . . ?
C31 C30 C29 121.3(13) . . ?
C30 C31 C26 123.1(13) . . ?
O27 C32 N24 121.1(12) . . ?
O27 C32 C28 124.4(13) . . ?
N24 C32 C28 114.5(12) . . ?
C33 N31 C35 124.7(16) . . ?
C33 N31 C34 119.3(14) . . ?
C35 N31 C34 115.4(13) . . ?
O31 C33 N31 122.7(18) . . ?
C36 N32 C38 115(2) . . ?
C36 N32 C37 116(2) . . ?
C38 N32 C37 128(2) . . ?
O32 C36 N32 103(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.087