Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_publication_text

_journal_coden_Cambridge         222
_publ_requested_journal          'Dalton Trans.'
_publ_contact_author_name        'Andrew Whiting'
_publ_contact_author_address     
;Department of Chemistry,
University Science Laboratories,
Durham University,
South Road,
Durham,
DH1 3LE
;
_publ_contact_author_email       andy.whiting@durham.ac.uk
_publ_contact_author_phone       01913342081
_publ_contact_author_fax         01913844737
loop_
_publ_author_name
_publ_author_address
'Whiting, Andrew'
;Department of Chemistry,
University Science Laboratories,
Durham University,
South Road,
Durham,
DH1 3LE
;
'Howard, Judith A. K.'
;Department of Chemistry,
University Science Laboratories,
Durham University,
South Road,
Durham,
DH1 3LE
;
'Ilyashenko, Gennadiy'
;Department of Chemistry,
University Science Laboratories,
Durham University,
South Road,
Durham,
DH1 3LE
;
'Sparkes, Hazel A.'
;Department of Chemistry,
University Science Laboratories,
Durham University,
South Road,
Durham,
DH1 3LE
;

_publ_section_title              
;
Development of new transition metal catalysts for the oxidation
of a hydroxamic acid with in situ Diels-Alder trapping of the
acyl nitroso derivative.
;

data_06srv291
_database_code_depnum_ccdc_archive 'CCDC 642155'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
Di-*\`i\`i*-alkoxo-(1-[(2-Hydroxy-3,5-di-*tert*-butyl-benzylidene)-amino]
-indan-2-ol)iron(III) chloride
;
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C48 H58 Cl2 Fe2 N2 O4, 0.3(C H2 Cl2)'
_chemical_formula_sum            'C48.30 H58.60 Cl2.60 Fe2 N2 O4'
_chemical_formula_weight         935.04
_chemical_absolute_configuration unk

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   12.370(3)
_cell_length_b                   17.427(2)
_cell_length_c                   22.378(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4824.1(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7625
_cell_measurement_theta_min      2.214
_cell_measurement_theta_max      26.101

_exptl_crystal_description       plate
_exptl_crystal_colour            dark_red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1962
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS, (G. Sheldrick, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Bruker SMART 1K CCD Detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            23875
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.36
_reflns_number_total             9356
_reflns_number_gt                7254
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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.
The structure contains disordered CH2Cl2 modelled at 30% occupancy. The
non-hydrogen atoms on the SOlvent were left isotropic due to the low
occupancy.
;

_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^)+(0.0392P)^2^+5.1434P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_number_reflns         9356
_refine_ls_number_parameters     548
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1201
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.075
_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 0.20345(5) 0.66027(4) 0.93816(3) 0.01796(16) Uani 1 1 d . . .
Fe2 Fe 0.26075(5) 0.54645(4) 1.04275(3) 0.01813(16) Uani 1 1 d . . .
Cl1 Cl 0.02538(9) 0.66501(9) 0.93454(7) 0.0356(3) Uani 1 1 d . . .
Cl2 Cl 0.11302(11) 0.51840(8) 1.09458(6) 0.0308(3) Uani 1 1 d . . .
Cl3 Cl 0.8059(5) 0.5230(4) 0.8842(3) 0.0576(15) Uiso 0.30 1 d P . .
Cl4 Cl 0.7269(6) 0.4228(4) 0.9729(3) 0.081(2) Uiso 0.30 1 d P . .
O1 O 0.2445(3) 0.66984(19) 0.85791(13) 0.0217(7) Uani 1 1 d . . .
O2 O 0.2472(3) 0.65545(18) 1.02451(13) 0.0213(7) Uani 1 1 d . . .
O3 O 0.2313(2) 0.55073(18) 0.95387(13) 0.0200(7) Uani 1 1 d . . .
O4 O 0.3813(3) 0.55113(19) 1.09398(14) 0.0212(7) Uani 1 1 d . . .
N1 N 0.2760(3) 0.7664(2) 0.95168(16) 0.0177(9) Uani 1 1 d . . .
N2 N 0.3255(3) 0.4438(2) 1.01074(17) 0.0181(9) Uani 1 1 d . . .
C1 C 0.2955(4) 0.7194(3) 1.0544(2) 0.0213(11) Uani 1 1 d . . .
H1 H 0.3743 0.7103 1.0614 0.026 Uiso 1 1 calc R . .
C2 C 0.2372(5) 0.7374(3) 1.1130(2) 0.0282(13) Uani 1 1 d . . .
H2A H 0.2046 0.6905 1.1303 0.034 Uiso 1 1 calc R . .
H2B H 0.2875 0.7601 1.1426 0.034 Uiso 1 1 calc R . .
C3 C 0.1516(4) 0.7940(3) 1.0953(2) 0.0209(11) Uani 1 1 d . . .
C4 C 0.0637(4) 0.8211(3) 1.1271(2) 0.0267(13) Uani 1 1 d . . .
H4 H 0.0495 0.8026 1.1662 0.032 Uiso 1 1 calc R . .
C5 C -0.0033(4) 0.8754(3) 1.1014(2) 0.0299(13) Uani 1 1 d . . .
H5 H -0.0640 0.8939 1.1230 0.036 Uiso 1 1 calc R . .
C6 C 0.0172(4) 0.9029(3) 1.0445(2) 0.0282(12) Uani 1 1 d . . .
H6 H -0.0295 0.9403 1.0276 0.034 Uiso 1 1 calc R . .
C7 C 0.1051(4) 0.8765(3) 1.0119(2) 0.0254(12) Uani 1 1 d . . .
H7 H 0.1194 0.8953 0.9728 0.030 Uiso 1 1 calc R . .
C8 C 0.1710(3) 0.8224(3) 1.0378(2) 0.0188(11) Uani 1 1 d . . .
C9 C 0.2778(4) 0.7907(3) 1.0148(2) 0.0193(11) Uani 1 1 d . . .
H9 H 0.3370 0.8288 1.0215 0.023 Uiso 1 1 calc R . .
C10 C 0.3324(4) 0.8050(3) 0.9137(2) 0.0209(11) Uani 1 1 d . . .
H10 H 0.3722 0.8476 0.9285 0.025 Uiso 1 1 calc R . .
C11 C 0.3402(4) 0.7885(3) 0.8500(2) 0.0187(11) Uani 1 1 d . . .
C12 C 0.3991(4) 0.8412(3) 0.8157(2) 0.0239(11) Uani 1 1 d . . .
H12 H 0.4336 0.8835 0.8345 0.029 Uiso 1 1 calc R . .
C13 C 0.4071(4) 0.8317(3) 0.7538(2) 0.0225(11) Uani 1 1 d . . .
C14 C 0.3532(4) 0.7696(3) 0.7289(2) 0.0221(11) Uani 1 1 d . . .
H14 H 0.3562 0.7639 0.6867 0.026 Uiso 1 1 calc R . .
C15 C 0.2947(4) 0.7146(3) 0.7612(2) 0.0197(10) Uani 1 1 d . . .
C16 C 0.2918(4) 0.7232(3) 0.8240(2) 0.0196(11) Uani 1 1 d . . .
C17 C 0.4746(5) 0.8889(3) 0.7165(2) 0.0295(13) Uani 1 1 d . . .
C18 C 0.4336(5) 0.9715(3) 0.7273(3) 0.0417(16) Uani 1 1 d . . .
H18A H 0.4381 0.9836 0.7700 0.063 Uiso 1 1 calc R . .
H18B H 0.3584 0.9757 0.7140 0.063 Uiso 1 1 calc R . .
H18C H 0.4785 1.0077 0.7046 0.063 Uiso 1 1 calc R . .
C19 C 0.5931(4) 0.8841(4) 0.7358(3) 0.0390(15) Uani 1 1 d . . .
H19A H 0.6181 0.8309 0.7325 0.059 Uiso 1 1 calc R . .
H19B H 0.6001 0.9013 0.7773 0.059 Uiso 1 1 calc R . .
H19C H 0.6371 0.9170 0.7099 0.059 Uiso 1 1 calc R . .
C20 C 0.4677(5) 0.8711(4) 0.6494(3) 0.0480(18) Uani 1 1 d . . .
H20A H 0.5127 0.9075 0.6272 0.072 Uiso 1 1 calc R . .
H20B H 0.3925 0.8756 0.6361 0.072 Uiso 1 1 calc R . .
H20C H 0.4935 0.8187 0.6422 0.072 Uiso 1 1 calc R . .
C21 C 0.2384(4) 0.6477(3) 0.7296(2) 0.0220(11) Uani 1 1 d . . .
C22 C 0.1166(4) 0.6472(3) 0.7451(2) 0.0276(12) Uani 1 1 d . . .
H22A H 0.0824 0.6021 0.7269 0.041 Uiso 1 1 calc R . .
H22B H 0.0826 0.6939 0.7295 0.041 Uiso 1 1 calc R . .
H22C H 0.1075 0.6452 0.7885 0.041 Uiso 1 1 calc R . .
C23 C 0.2924(5) 0.5729(3) 0.7474(2) 0.0255(12) Uani 1 1 d . . .
H23A H 0.3699 0.5758 0.7387 0.038 Uiso 1 1 calc R . .
H23B H 0.2602 0.5305 0.7248 0.038 Uiso 1 1 calc R . .
H23C H 0.2819 0.5641 0.7903 0.038 Uiso 1 1 calc R . .
C24 C 0.2485(5) 0.6530(3) 0.6611(2) 0.0286(12) Uani 1 1 d . . .
H24A H 0.3251 0.6542 0.6499 0.043 Uiso 1 1 calc R . .
H24B H 0.2130 0.7000 0.6470 0.043 Uiso 1 1 calc R . .
H24C H 0.2137 0.6083 0.6427 0.043 Uiso 1 1 calc R . .
C25 C 0.2444(5) 0.4857(3) 0.9162(2) 0.0311(6) Uani 1 1 d U . .
H25 H 0.3030 0.4944 0.8862 0.037 Uiso 1 1 calc R . .
C26 C 0.1379(4) 0.4639(3) 0.8855(2) 0.0328(6) Uani 1 1 d U . .
H26A H 0.0913 0.5096 0.8800 0.039 Uiso 1 1 calc R . .
H26B H 0.1516 0.4402 0.8460 0.039 Uiso 1 1 calc R . .
C27 C 0.0868(5) 0.4079(3) 0.9270(2) 0.0351(6) Uani 1 1 d U . .
C28 C -0.0182(5) 0.3802(3) 0.9280(3) 0.0387(6) Uani 1 1 d U . .
H28 H -0.0698 0.3977 0.8997 0.046 Uiso 1 1 calc R . .
C29 C -0.0475(5) 0.3256(4) 0.9717(2) 0.0405(7) Uani 1 1 d U . .
H29 H -0.1192 0.3060 0.9725 0.049 Uiso 1 1 calc R . .
C30 C 0.0266(5) 0.3004(4) 1.0132(3) 0.0396(7) Uani 1 1 d U . .
H30 H 0.0049 0.2650 1.0432 0.047 Uiso 1 1 calc R . .
C31 C 0.1336(5) 0.3264(3) 1.0116(2) 0.0365(6) Uani 1 1 d U . .
H31 H 0.1856 0.3076 1.0391 0.044 Uiso 1 1 calc R . .
C32 C 0.1619(5) 0.3806(3) 0.9685(2) 0.0339(6) Uani 1 1 d U . .
C33 C 0.2708(4) 0.4152(3) 0.9572(2) 0.0315(6) Uani 1 1 d U . .
H33 H 0.3181 0.3779 0.9355 0.038 Uiso 1 1 calc R . .
C34 C 0.4113(4) 0.4108(3) 1.0296(2) 0.0214(11) Uani 1 1 d . . .
H34 H 0.4331 0.3659 1.0088 0.026 Uiso 1 1 calc R . .
C35 C 0.4784(4) 0.4341(3) 1.0788(2) 0.0196(11) Uani 1 1 d . . .
C36 C 0.5645(4) 0.3854(3) 1.0950(2) 0.0257(12) Uani 1 1 d . . .
H36 H 0.5743 0.3388 1.0736 0.031 Uiso 1 1 calc R . .
C37 C 0.6345(4) 0.4028(3) 1.1402(2) 0.0284(13) Uani 1 1 d . . .
C38 C 0.6154(4) 0.4726(3) 1.1708(2) 0.0228(11) Uani 1 1 d . . .
H38 H 0.6633 0.4856 1.2024 0.027 Uiso 1 1 calc R . .
C39 C 0.5328(4) 0.5232(3) 1.1583(2) 0.0201(11) Uani 1 1 d . . .
C40 C 0.4612(4) 0.5038(3) 1.1099(2) 0.0181(11) Uani 1 1 d . . .
C41 C 0.7281(6) 0.3504(4) 1.1595(3) 0.0541(11) Uani 1 1 d U . .
C42 C 0.7273(6) 0.2744(4) 1.1274(3) 0.0556(13) Uani 1 1 d U . .
H42A H 0.6565 0.2499 1.1324 0.083 Uiso 1 1 calc R . .
H42B H 0.7835 0.2411 1.1441 0.083 Uiso 1 1 calc R . .
H42C H 0.7413 0.2826 1.0848 0.083 Uiso 1 1 calc R . .
C43 C 0.7254(6) 0.3373(4) 1.2275(3) 0.0563(13) Uani 1 1 d U . .
H43A H 0.7338 0.3865 1.2481 0.085 Uiso 1 1 calc R . .
H43B H 0.7846 0.3029 1.2389 0.085 Uiso 1 1 calc R . .
H43C H 0.6562 0.3141 1.2387 0.085 Uiso 1 1 calc R . .
C44 C 0.8348(5) 0.3918(4) 1.1443(3) 0.0563(13) Uani 1 1 d U . .
H44A H 0.8379 0.4018 1.1013 0.084 Uiso 1 1 calc R . .
H44B H 0.8960 0.3594 1.1559 0.084 Uiso 1 1 calc R . .
H44C H 0.8382 0.4405 1.1661 0.084 Uiso 1 1 calc R . .
C45 C 0.5170(4) 0.5977(3) 1.1949(2) 0.0249(8) Uani 1 1 d U . .
C46 C 0.5954(4) 0.6027(3) 1.2480(2) 0.0286(10) Uani 1 1 d U . .
H46A H 0.6700 0.6023 1.2333 0.043 Uiso 1 1 calc R . .
H46B H 0.5840 0.5586 1.2745 0.043 Uiso 1 1 calc R . .
H46C H 0.5821 0.6503 1.2702 0.043 Uiso 1 1 calc R . .
C47 C 0.5386(4) 0.6676(3) 1.1546(2) 0.0243(9) Uani 1 1 d U . .
H47A H 0.6146 0.6676 1.1421 0.037 Uiso 1 1 calc R . .
H47B H 0.5230 0.7148 1.1767 0.037 Uiso 1 1 calc R . .
H47C H 0.4920 0.6649 1.1192 0.037 Uiso 1 1 calc R . .
C48 C 0.4011(4) 0.6022(3) 1.2202(2) 0.0261(9) Uani 1 1 d U . .
H48A H 0.3928 0.6496 1.2432 0.039 Uiso 1 1 calc R . .
H48B H 0.3879 0.5579 1.2462 0.039 Uiso 1 1 calc R . .
H48C H 0.3491 0.6018 1.1872 0.039 Uiso 1 1 calc R . .
C49 C 0.8130(19) 0.5013(14) 0.9577(11) 0.058(6) Uiso 0.30 1 d P . .
H49A H 0.7907 0.5462 0.9818 0.069 Uiso 0.30 1 calc PR . .
H49B H 0.8883 0.4881 0.9686 0.069 Uiso 0.30 1 calc PR . .

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 0.0191(3) 0.0182(4) 0.0166(3) 0.0006(3) 0.0001(3) -0.0002(3)
Fe2 0.0228(4) 0.0175(4) 0.0141(3) -0.0003(3) 0.0013(3) 0.0013(3)
Cl1 0.0194(6) 0.0371(8) 0.0503(8) 0.0100(8) 0.0038(6) 0.0048(6)
Cl2 0.0295(7) 0.0344(8) 0.0284(7) 0.0038(6) 0.0096(6) -0.0017(6)
O1 0.0232(17) 0.0233(19) 0.0187(16) 0.0004(14) 0.0008(15) -0.0059(16)
O2 0.0317(18) 0.0165(18) 0.0157(15) -0.0036(13) -0.0052(14) 0.0058(16)
O3 0.0269(17) 0.0157(17) 0.0174(15) 0.0014(14) 0.0012(14) 0.0008(14)
O4 0.0254(17) 0.0165(18) 0.0217(17) -0.0032(15) 0.0022(15) 0.0043(16)
N1 0.019(2) 0.019(2) 0.0154(19) -0.0035(17) 0.0002(16) 0.0022(16)
N2 0.022(2) 0.016(2) 0.016(2) 0.0007(18) 0.0001(16) 0.0019(17)
C1 0.027(2) 0.016(3) 0.021(3) -0.003(2) -0.006(2) 0.000(2)
C2 0.056(4) 0.016(3) 0.013(2) 0.000(2) -0.002(2) 0.009(3)
C3 0.031(3) 0.015(3) 0.017(3) -0.001(2) -0.003(2) -0.003(2)
C4 0.031(3) 0.030(3) 0.019(3) -0.003(2) 0.000(2) -0.003(2)
C5 0.020(3) 0.040(4) 0.030(3) -0.011(3) 0.002(2) 0.005(2)
C6 0.027(3) 0.027(3) 0.031(3) -0.003(3) -0.004(2) 0.002(2)
C7 0.029(3) 0.022(3) 0.025(3) 0.003(2) -0.001(2) 0.003(2)
C8 0.018(2) 0.019(3) 0.019(2) -0.008(2) -0.003(2) -0.0061(19)
C9 0.020(3) 0.022(3) 0.015(2) -0.004(2) -0.0031(19) 0.005(2)
C10 0.017(2) 0.018(3) 0.028(3) -0.004(2) -0.002(2) -0.002(2)
C11 0.020(2) 0.019(3) 0.017(2) 0.000(2) 0.001(2) 0.002(2)
C12 0.019(2) 0.023(3) 0.029(3) -0.003(2) 0.001(2) -0.004(2)
C13 0.025(3) 0.020(3) 0.023(3) 0.000(2) 0.003(2) 0.000(2)
C14 0.026(3) 0.022(3) 0.019(3) -0.002(2) 0.004(2) 0.000(2)
C15 0.022(2) 0.016(3) 0.021(2) -0.002(2) 0.000(2) -0.001(2)
C16 0.016(2) 0.022(3) 0.021(2) 0.002(2) 0.001(2) 0.004(2)
C17 0.040(3) 0.020(3) 0.029(3) -0.003(2) 0.011(3) -0.003(3)
C18 0.046(4) 0.026(4) 0.053(4) 0.011(3) 0.019(3) -0.003(3)
C19 0.032(3) 0.036(4) 0.049(4) -0.005(3) 0.017(3) -0.011(3)
C20 0.052(4) 0.059(5) 0.033(3) 0.002(3) 0.015(3) -0.023(3)
C21 0.032(3) 0.017(3) 0.017(2) -0.001(2) -0.001(2) -0.002(2)
C22 0.027(3) 0.026(3) 0.030(3) -0.006(2) -0.009(2) -0.003(2)
C23 0.036(3) 0.019(3) 0.021(3) -0.003(2) -0.002(2) 0.002(2)
C24 0.043(3) 0.023(3) 0.019(2) 0.004(2) -0.008(2) -0.006(3)
C25 0.0448(15) 0.0297(14) 0.0187(12) -0.0035(11) -0.0007(12) -0.0123(12)
C26 0.0463(14) 0.0317(14) 0.0203(12) -0.0028(11) -0.0012(11) -0.0133(12)
C27 0.0484(14) 0.0340(13) 0.0229(11) -0.0026(10) -0.0017(10) -0.0157(11)
C28 0.0512(15) 0.0381(14) 0.0267(12) -0.0017(11) -0.0026(12) -0.0181(12)
C29 0.0535(15) 0.0395(15) 0.0285(13) -0.0018(12) -0.0016(12) -0.0196(12)
C30 0.0538(15) 0.0381(14) 0.0269(13) -0.0024(12) -0.0004(12) -0.0193(12)
C31 0.0513(15) 0.0348(14) 0.0235(12) -0.0032(11) -0.0004(11) -0.0169(12)
C32 0.0480(14) 0.0323(13) 0.0214(11) -0.0034(10) -0.0007(10) -0.0152(11)
C33 0.0454(14) 0.0301(14) 0.0190(12) -0.0036(11) -0.0004(11) -0.0126(12)
C34 0.031(3) 0.014(3) 0.019(3) -0.002(2) 0.003(2) 0.000(2)
C35 0.027(3) 0.010(3) 0.021(3) 0.003(2) 0.003(2) -0.0008(19)
C36 0.030(3) 0.021(3) 0.026(3) -0.006(2) 0.002(2) 0.004(2)
C37 0.024(3) 0.029(3) 0.032(3) 0.000(2) -0.007(2) 0.007(2)
C38 0.027(3) 0.019(3) 0.023(3) 0.002(2) -0.004(2) 0.004(2)
C39 0.026(3) 0.014(3) 0.021(3) -0.001(2) 0.004(2) -0.006(2)
C40 0.020(2) 0.018(3) 0.015(2) 0.002(2) 0.0011(19) 0.000(2)
C41 0.058(2) 0.048(2) 0.056(2) -0.018(2) -0.026(2) 0.024(2)
C42 0.060(3) 0.048(3) 0.059(3) -0.017(2) -0.027(2) 0.026(2)
C43 0.063(3) 0.049(3) 0.056(3) -0.013(2) -0.027(2) 0.025(2)
C44 0.056(3) 0.053(3) 0.059(3) -0.019(2) -0.023(2) 0.023(2)
C45 0.0323(17) 0.0215(17) 0.0209(16) -0.0024(14) -0.0020(14) -0.0027(14)
C46 0.035(2) 0.025(2) 0.025(2) -0.0028(18) -0.0060(18) -0.0008(18)
C47 0.032(2) 0.020(2) 0.0213(19) -0.0016(18) -0.0018(17) -0.0044(17)
C48 0.034(2) 0.022(2) 0.0216(19) -0.0041(17) 0.0031(18) -0.0035(18)

_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 O1 1.874(3) . ?
Fe1 O3 1.971(3) . ?
Fe1 O2 2.008(3) . ?
Fe1 N1 2.078(4) . ?
Fe1 Cl1 2.2056(14) . ?
Fe2 O4 1.882(3) . ?
Fe2 O2 1.950(3) . ?
Fe2 O3 2.023(3) . ?
Fe2 N2 2.086(4) . ?
Fe2 Cl2 2.2189(15) . ?
Cl3 C49 1.69(2) . ?
Cl4 C49 1.77(2) . ?
O1 C16 1.335(6) . ?
O2 C1 1.431(5) . ?
O3 C25 1.422(6) . ?
O4 C40 1.336(6) . ?
N1 C10 1.289(6) . ?
N1 C9 1.475(6) . ?
N2 C34 1.279(6) . ?
N2 C33 1.464(6) . ?
C1 C2 1.530(7) . ?
C1 C9 1.541(7) . ?
C1 H1 1.0000 . ?
C2 C3 1.500(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.383(7) . ?
C3 C8 1.399(7) . ?
C4 C5 1.382(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.375(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.521(6) . ?
C9 H9 1.0000 . ?
C10 C11 1.458(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(7) . ?
C11 C16 1.412(7) . ?
C12 C13 1.399(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(7) . ?
C13 C17 1.545(7) . ?
C14 C15 1.402(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.413(7) . ?
C15 C21 1.531(7) . ?
C17 C19 1.531(8) . ?
C17 C20 1.536(8) . ?
C17 C18 1.545(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.519(7) . ?
C21 C24 1.541(6) . ?
C21 C22 1.546(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.532(7) . ?
C25 C33 1.568(7) . ?
C25 H25 1.0000 . ?
C26 C27 1.489(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.386(8) . ?
C27 C32 1.397(8) . ?
C28 C29 1.412(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.399(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.394(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.497(8) . ?
C33 H33 1.0000 . ?
C34 C35 1.437(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.409(7) . ?
C35 C40 1.417(7) . ?
C36 C37 1.365(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.417(7) . ?
C37 C41 1.537(8) . ?
C38 C39 1.378(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.439(7) . ?
C39 C45 1.547(7) . ?
C41 C42 1.508(9) . ?
C41 C43 1.539(9) . ?
C41 C44 1.541(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.537(7) . ?
C45 C47 1.539(7) . ?
C45 C48 1.544(7) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?

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 Fe1 O3 102.11(14) . . ?
O1 Fe1 O2 148.54(13) . . ?
O3 Fe1 O2 74.98(13) . . ?
O1 Fe1 N1 86.76(15) . . ?
O3 Fe1 N1 139.53(14) . . ?
O2 Fe1 N1 77.34(14) . . ?
O1 Fe1 Cl1 103.41(11) . . ?
O3 Fe1 Cl1 102.54(10) . . ?
O2 Fe1 Cl1 107.81(11) . . ?
N1 Fe1 Cl1 113.77(11) . . ?
O4 Fe2 O2 98.83(14) . . ?
O4 Fe2 O3 137.72(14) . . ?
O2 Fe2 O3 75.11(12) . . ?
O4 Fe2 N2 86.68(15) . . ?
O2 Fe2 N2 142.77(14) . . ?
O3 Fe2 N2 76.31(14) . . ?
O4 Fe2 Cl2 110.08(11) . . ?
O2 Fe2 Cl2 104.66(11) . . ?
O3 Fe2 Cl2 111.93(10) . . ?
N2 Fe2 Cl2 107.86(12) . . ?
C16 O1 Fe1 136.5(3) . . ?
C1 O2 Fe2 128.7(3) . . ?
C1 O2 Fe1 122.0(3) . . ?
Fe2 O2 Fe1 105.38(14) . . ?
C25 O3 Fe1 133.3(3) . . ?
C25 O3 Fe2 122.2(3) . . ?
Fe1 O3 Fe2 104.03(14) . . ?
C40 O4 Fe2 136.2(3) . . ?
C10 N1 C9 118.2(4) . . ?
C10 N1 Fe1 127.1(3) . . ?
C9 N1 Fe1 113.7(3) . . ?
C34 N2 C33 120.1(4) . . ?
C34 N2 Fe2 126.2(3) . . ?
C33 N2 Fe2 113.3(3) . . ?
O2 C1 C2 111.3(4) . . ?
O2 C1 C9 107.5(4) . . ?
C2 C1 C9 105.1(4) . . ?
O2 C1 H1 110.9 . . ?
C2 C1 H1 110.9 . . ?
C9 C1 H1 110.9 . . ?
C3 C2 C1 103.9(4) . . ?
C3 C2 H2A 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C3 C2 H2B 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C4 C3 C8 119.1(5) . . ?
C4 C3 C2 130.0(5) . . ?
C8 C3 C2 110.8(4) . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 120.9(5) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 118.0(5) . . ?
C8 C7 H7 121.0 . . ?
C6 C7 H7 121.0 . . ?
C7 C8 C3 121.9(5) . . ?
C7 C8 C9 128.4(5) . . ?
C3 C8 C9 109.3(4) . . ?
N1 C9 C8 114.5(4) . . ?
N1 C9 C1 108.7(4) . . ?
C8 C9 C1 102.9(4) . . ?
N1 C9 H9 110.2 . . ?
C8 C9 H9 110.2 . . ?
C1 C9 H9 110.2 . . ?
N1 C10 C11 125.2(5) . . ?
N1 C10 H10 117.4 . . ?
C11 C10 H10 117.4 . . ?
C12 C11 C16 121.5(4) . . ?
C12 C11 C10 116.1(5) . . ?
C16 C11 C10 122.4(4) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 117.2(5) . . ?
C14 C13 C17 123.1(4) . . ?
C12 C13 C17 119.8(5) . . ?
C13 C14 C15 124.9(5) . . ?
C13 C14 H14 117.5 . . ?
C15 C14 H14 117.5 . . ?
C14 C15 C16 117.0(5) . . ?
C14 C15 C21 121.1(4) . . ?
C16 C15 C21 121.8(4) . . ?
O1 C16 C11 120.8(4) . . ?
O1 C16 C15 120.2(4) . . ?
C11 C16 C15 119.0(4) . . ?
C19 C17 C20 108.5(5) . . ?
C19 C17 C18 108.8(5) . . ?
C20 C17 C18 108.8(5) . . ?
C19 C17 C13 109.3(5) . . ?
C20 C17 C13 111.5(5) . . ?
C18 C17 C13 110.0(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C21 C15 109.4(4) . . ?
C23 C21 C24 106.1(4) . . ?
C15 C21 C24 112.1(4) . . ?
C23 C21 C22 111.4(4) . . ?
C15 C21 C22 110.2(4) . . ?
C24 C21 C22 107.6(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 C26 111.4(5) . . ?
O3 C25 C33 107.5(4) . . ?
C26 C25 C33 104.3(4) . . ?
O3 C25 H25 111.1 . . ?
C26 C25 H25 111.1 . . ?
C33 C25 H25 111.1 . . ?
C27 C26 C25 104.4(4) . . ?
C27 C26 H26A 110.9 . . ?
C25 C26 H26A 110.9 . . ?
C27 C26 H26B 110.9 . . ?
C25 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
C28 C27 C32 119.6(5) . . ?
C28 C27 C26 129.6(5) . . ?
C32 C27 C26 110.8(5) . . ?
C27 C28 C29 119.1(6) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 120.7(6) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 120.5(6) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C32 C31 C30 118.4(6) . . ?
C32 C31 H31 120.8 . . ?
C30 C31 H31 120.8 . . ?
C31 C32 C27 121.5(5) . . ?
C31 C32 C33 128.1(5) . . ?
C27 C32 C33 110.4(5) . . ?
N2 C33 C32 114.5(4) . . ?
N2 C33 C25 108.0(4) . . ?
C32 C33 C25 103.2(5) . . ?
N2 C33 H33 110.3 . . ?
C32 C33 H33 110.3 . . ?
C25 C33 H33 110.3 . . ?
N2 C34 C35 127.3(5) . . ?
N2 C34 H34 116.4 . . ?
C35 C34 H34 116.4 . . ?
C36 C35 C40 120.2(5) . . ?
C36 C35 C34 117.6(4) . . ?
C40 C35 C34 122.1(4) . . ?
C37 C36 C35 122.4(5) . . ?
C37 C36 H36 118.8 . . ?
C35 C36 H36 118.8 . . ?
C36 C37 C38 116.3(5) . . ?
C36 C37 C41 123.7(5) . . ?
C38 C37 C41 120.0(5) . . ?
C39 C38 C37 125.1(5) . . ?
C39 C38 H38 117.5 . . ?
C37 C38 H38 117.5 . . ?
C38 C39 C40 117.3(4) . . ?
C38 C39 C45 121.5(4) . . ?
C40 C39 C45 121.2(4) . . ?
O4 C40 C35 120.6(4) . . ?
O4 C40 C39 120.8(4) . . ?
C35 C40 C39 118.6(4) . . ?
C42 C41 C37 112.5(5) . . ?
C42 C41 C43 109.9(6) . . ?
C37 C41 C43 110.5(5) . . ?
C42 C41 C44 108.2(6) . . ?
C37 C41 C44 107.8(5) . . ?
C43 C41 C44 107.8(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C47 107.4(4) . . ?
C46 C45 C48 107.4(4) . . ?
C47 C45 C48 109.6(4) . . ?
C46 C45 C39 112.2(4) . . ?
C47 C45 C39 109.4(4) . . ?
C48 C45 C39 110.7(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Cl3 C49 Cl4 109.2(14) . . ?
Cl3 C49 H49A 109.8 . . ?
Cl4 C49 H49A 109.8 . . ?
Cl3 C49 H49B 109.8 . . ?
Cl4 C49 H49B 109.8 . . ?
H49A C49 H49B 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.083