##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
data_global
_audit_creation_method     Xtal3.6
_journal_date_recd_electronic     2004-03-24
_journal_date_accepted     2004-05-04
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2004
_journal_volume     60
_journal_issue      7
_journal_page_first     m311
_journal_page_last     m313
_journal_paper_category     FM
_publ_contact_author_name     'Skelton, B. W.'
_publ_contact_author_address
;
   Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email     bws@crystal.uwa.edu.au
_publ_contact_author_fax     '(+61) 08 9380 1118'
_publ_contact_author_phone     '(+61) 08 9380 3481'
_publ_section_title
;
Bis[tris(1-methyl-1H-imidazol-2-yl)phosphine-κ³N³]iron(II)
tetrachloroferrate(II) methanol tetrasolvate (ca 153 K) and
bis[tris(1-methyl-1H-imidazol-2-yl)methanol-κ³N³]iron(III)
bis(tetrachloroferrate(III)) chloride (redetermination, ca 153 K)
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Batten, Michael P.' .
; Department of Chemistry
University of Tasmania
Hobart
Tasmania 7001
Australia
;
    'Canty, Allan J.' .
; Department of Chemistry
University of Tasmania
Hobart
Tasmania 7001
Australia
;
    'Cavell, Kingsley J.'
;
Present address: Department of Chemistry, University of Cardiff, U.K.
;
; Department of Chemistry
University of Tasmania
Hobart
Tasmania 7001
Australia
;
    'Rüther, Thomas'
;
 Present Address: IDT Australia, Boronia, Vic. 3155, Australia
;
; Department of Chemistry
University of Tasmania
Hobart
Tasmania 7001
Australia
;
    'Skelton, Brian W.' .
; Chemistry,
University of Western Australia
35 Stirling Highway
Crawley
WA 6009
Australia
;
    'White, Allan H.' .
; Chemistry
University of Western Australia
35 Stirling Highway
Crawley
WA 6009
Australia
;
data_I
_chemical_name_systematic     ?
_chemical_name_common     ?
_chemical_formula_moiety     'C24 H30 Fe N12 P2 2+, Cl4 Fe 2-, 4C H4 O'
_chemical_formula_sum     'C28 H46 Cl4 Fe2 N12 O4 P2'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac     '[Fe (C12 H15 N6 P1)] [Fe Cl4], 4C H4 O'
_chemical_formula_weight     930.21
_chemical_melting_point     ?
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     P_b_c_n
_symmetry_space_group_name_Hall     -p_2n_2ab
loop_
    _symmetry_equiv_pos_as_xyz
    +x,+y,+z
    1/2-x,1/2-y,1/2+z
    1/2+x,1/2-y,-z
    -x,+y,1/2-z
    -x,-y,-z
    1/2+x,1/2+y,1/2-z
    1/2-x,1/2+y,+z
    +x,-y,1/2+z
_cell_length_a     16.9011(10)
_cell_length_b     12.9824(8)
_cell_length_c     18.3248(11)
_cell_angle_alpha     90.00000
_cell_angle_beta     90.00000
_cell_angle_gamma     90.00000
_cell_volume     4020.8(4)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     6152
_cell_measurement_theta_min     2.6
_cell_measurement_theta_max     37.2
_cell_measurement_temperature     150(2)
_cell_special_details
;      ?
;
_exptl_crystal_description     prism
_exptl_crystal_colour     red
_exptl_crystal_size_max     .2
_exptl_crystal_size_mid     .2
_exptl_crystal_size_min     .15
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     1.537
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1920
_exptl_absorpt_coefficient_mu     1.117
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_absorpt_correction_T_min     .69
_exptl_absorpt_correction_T_max     .83
_exptl_special_details
;      ?
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_radiation_source     'sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     82795
_diffrn_reflns_av_R_equivalents     .051
_diffrn_reflns_av_sigmaI/netI     .116
_diffrn_reflns_theta_min     1.98
_diffrn_reflns_theta_max     37.5
_diffrn_reflns_theta_full     37.5
_diffrn_measured_fraction_theta_max     1.0
_diffrn_measured_fraction_theta_full     1.0
_diffrn_reflns_limit_h_min     -28
_diffrn_reflns_limit_h_max     28
_diffrn_reflns_limit_k_min     -22
_diffrn_reflns_limit_k_max     22
_diffrn_reflns_limit_l_min     -31
_diffrn_reflns_limit_l_max     31
_diffrn_reflns_reduction_process     ?
_diffrn_standards_number     0
_diffrn_standards_decay_%     0
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    ? ? ?
_reflns_number_total     10596
_reflns_number_gt     6611
_reflns_number_observed     ?
_reflns_threshold_expression     'I>2σ(I)'
_refine_ls_structure_factor_coef     F
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     .08
_refine_ls_R_factor_gt     .04
_refine_ls_wR_factor_all     .049
_refine_ls_wR_factor_ref     .042
_refine_ls_goodness_of_fit_all     .891
_refine_ls_goodness_of_fit_ref     .976
_refine_ls_number_reflns     6611
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_number_constraints     0
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
;
  w = 1/(σ²(F) +  0.0003F²)
;
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     .002
_refine_ls_shift/su_mean     .0002
_refine_diff_density_max     .962
_refine_diff_density_min     -.632
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_extinction_expression     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    C ? .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    H ? 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    Cl ? .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    Fe ? .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    N ? .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    O ? .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    P ? .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1'
_computing_data_collection     'SMART (Siemens, 1995)'
_computing_cell_refinement     'SAINT (Siemens, 1995)'
_computing_data_reduction     'SAINT'
_computing_structure_solution
;
Xtal3.5 (Hall et al., 1995)
;
_computing_structure_refinement     'CRYLSQ in Xtal3.5 '
_computing_molecular_graphics     Xtal3.5
_computing_publication_material     'BONDLA and CIFIO in Xtal3.5 '
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_calc_attached_atom
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Fe1 .00000 .00000 .00000 .01308(11) Uani ? ? 1.00000 ? ?
    Fe2 .00000 .41731(3) .25000 .02327(15) Uani ? ? 1.00000 ? ?
    Cl1 .00511(3) .33017(4) .14210(3) .0377(2) Uani ? ? 1.00000 ? ?
    Cl2 -.11287(4) .52486(5) .24682(3) .0493(3) Uani ? ? 1.00000 ? ?
    P -.14545(2) .18589(3) .01272(2) .01742(16) Uani ? ? 1.00000 ? ?
    N11 .01035(8) .14697(10) -.02833(7) .0167(5) Uani ? ? 1.00000 ? ?
    C12 -.04768(9) .21620(12) -.02228(8) .0168(6) Uani ? ? 1.00000 ? ?
    N13 -.02354(9) .30974(11) -.04555(8) .0207(6) Uani ? ? 1.00000 ? ?
    C131 -.06915(12) .40508(14) -.04378(11) .0286(9) Uani ? ? 1.00000 ? ?
    C14 .05379(11) .30020(14) -.06651(11) .0265(8) Uani ? ? 1.00000 ? ?
    C15 .07426(10) .19997(14) -.05609(10) .0235(8) Uani ? ? 1.00000 ? ?
    N21 -.05468(8) .04385(10) .09007(7) .0161(5) Uani ? ? 1.00000 ? ?
    C22 -.10981(9) .11748(12) .09282(8) .0168(6) Uani ? ? 1.00000 ? ?
    N23 -.13417(8) .13183(11) .16258(7) .0210(6) Uani ? ? 1.00000 ? ?
    C231 -.19012(12) .20871(16) .18929(10) .0306(9) Uani ? ? 1.00000 ? ?
    C24 -.09291(11) .06488(15) .20560(9) .0256(8) Uani ? ? 1.00000 ? ?
    C25 -.04424(10) .01043(14) .16064(8) .0216(7) Uani ? ? 1.00000 ? ?
    N31 -.10427(7) -.00360(10) -.04909(7) .0158(5) Uani ? ? 1.00000 ? ?
    C32 -.15817(9) .07123(12) -.04298(8) .0169(6) Uani ? ? 1.00000 ? ?
    N33 -.22348(8) .04824(11) -.08291(7) .0194(6) Uani ? ? 1.00000 ? ?
    C331 -.29447(10) .11209(16) -.09031(11) .0275(8) Uani ? ? 1.00000 ? ?
    C34 -.21061(10) -.04572(14) -.11506(9) .0217(7) Uani ? ? 1.00000 ? ?
    C35 -.13703(10) -.07748(13) -.09392(9) .0192(7) Uani ? ? 1.00000 ? ?
    O01 -.15888(10) .26858(12) -.17582(9) .0401(8) Uani ? ? 1.00000 ? ?
    C01 -.1291(2) .1884(2) -.21877(15) .0644(18) Uani ? ? 1.00000 ? ?
    O02 .29817(10) -.04606(13) -.09637(10) .0460(9) Uani ? ? 1.00000 ? ?
    C02 .26807(15) .05456(18) -.09151(13) .0404(12) Uani ? ? 1.00000 ? ?
    H131a -.06544 .43526 .00351 .04300 Uiso ? ? 1.00000 ? ?
    H131b -.04860 .45125 -.07902 .04400 Uiso ? ? 1.00000 ? ?
    H131c -.12286 .38983 -.05488 .03900 Uiso ? ? 1.00000 ? ?
    H14 .08699 .35333 -.08479 .03500 Uiso ? ? 1.00000 ? ?
    H15 .12477 .16900 -.06618 .02600 Uiso ? ? 1.00000 ? ?
    H231a -.22221 .17892 .22630 .05900 Uiso ? ? 1.00000 ? ?
    H231b -.16207 .26554 .20892 .03600 Uiso ? ? 1.00000 ? ?
    H231c -.22280 .23133 .15025 .05100 Uiso ? ? 1.00000 ? ?
    H24 -.09724 .05769 .25698 .03400 Uiso ? ? 1.00000 ? ?
    H25 -.00874 -.04210 .17559 .01700 Uiso ? ? 1.00000 ? ?
    H331a -.27948 .18105 -.10069 .03300 Uiso ? ? 1.00000 ? ?
    H331b -.32359 .11004 -.04586 .04800 Uiso ? ? 1.00000 ? ?
    H331c -.32622 .08611 -.12877 .04500 Uiso ? ? 1.00000 ? ?
    H34 -.24605 -.08189 -.14597 .02700 Uiso ? ? 1.00000 ? ?
    H35 -.11246 -.14021 -.10791 .01700 Uiso ? ? 1.00000 ? ?
    H01 -.14028 .32871 -.19600 .05000 Uiso ? ? 1.00000 ? ?
    H01a -.15017 .12460 -.20234 .12300 Uiso ? ? 1.00000 ? ?
    H01b -.07335 .18711 -.21599 .07300 Uiso ? ? 1.00000 ? ?
    H01c -.14485 .19900 -.26841 .07500 Uiso ? ? 1.00000 ? ?
    H02 .31802 -.05066 -.14337 .06900 Uiso ? ? 1.00000 ? ?
    H02a .24304 .06362 -.04561 .06700 Uiso ? ? 1.00000 ? ?
    H02b .23032 .06555 -.12944 .04400 Uiso ? ? 1.00000 ? ?
    H02c .30992 .10276 -.09654 .08000 Uiso ? ? 1.00000 ? ?
_geom_special_details     ?
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Fe1 N11 . . 1.9851(13) yes
    Fe1 N21 . . 1.9755(13) yes
    Fe1 N31 . . 1.9792(12) yes
    Fe1 N11 . 5 1.9851(13) ?
    Fe1 N21 . 5 1.9755(13) ?
    Fe1 N31 . 5 1.9792(12) ?
    Fe2 Cl1 . . 2.2797(5) ?
    Fe2 Cl2 . . 2.3648(7) ?
    Fe2 Cl1 . 4 2.2797(5) ?
    Fe2 Cl2 . 4 2.3648(7) ?
    P C12 . . 1.8158(16) ?
    P C22 . . 1.8182(16) ?
    P C32 . . 1.8177(16) ?
    N11 C12 . . 1.335(2) ?
    N11 C15 . . 1.378(2) ?
    C12 N13 . . 1.350(2) ?
    N13 C131 . . 1.459(2) ?
    N13 C14 . . 1.368(2) ?
    C131 H131a . . .953 ?
    C131 H131b . . .947 ?
    C131 H131c . . .951 ?
    C14 C15 . . 1.360(3) ?
    C14 H14 . . .9501 ?
    C15 H15 . . .9616 ?
    N21 C22 . . 1.336(2) ?
    N21 C25 . . 1.375(2) ?
    C22 N23 . . 1.356(2) ?
    N23 C231 . . 1.459(3) ?
    N23 C24 . . 1.365(2) ?
    C231 H231a . . .951 ?
    C231 H231b . . .948 ?
    C231 H231c . . .950 ?
    C24 C25 . . 1.362(2) ?
    C24 H24 . . .9490 ?
    C25 H25 . . .9487 ?
    N31 C32 . . 1.336(2) ?
    N31 C35 . . 1.379(2) ?
    C32 N33 . . 1.358(2) ?
    N33 C331 . . 1.465(2) ?
    N33 C34 . . 1.372(2) ?
    C331 H331a . . .950 ?
    C331 H331b . . .952 ?
    C331 H331c . . .9478 ?
    C34 C35 . . 1.366(2) ?
    C34 H34 . . .9487 ?
    C35 H35 . . .9494 ?
    O01 C01 . . 1.398(3) ?
    O01 H01 . . .9192 ?
    C01 H01a . . .950 ?
    C01 H01b . . .944 ?
    C01 H01c . . .958 ?
    O02 C02 . . 1.405(3) ?
    O02 H02 . . .9263 ?
    C02 H02a . . .949 ?
    C02 H02b . . .954 ?
    C02 H02c . . .949 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N11 Fe1 N21 . . . 89.01(5) yes
    N11 Fe1 N31 . . . 88.99(5) yes
    N11 Fe1 N11 . . 5 180.0000 ?
    N11 Fe1 N21 . . 5 90.99(5) ?
    N11 Fe1 N31 . . 5 91.01(5) ?
    N21 Fe1 N31 . . . 88.28(5) yes
    N21 Fe1 N11 . . 5 90.99(5) ?
    N21 Fe1 N21 . . 5 180.0000 ?
    N21 Fe1 N31 . . 5 91.72(5) ?
    N31 Fe1 N11 . . 5 91.01(5) ?
    N31 Fe1 N21 . . 5 91.72(5) ?
    N31 Fe1 N31 . . 5 180.0000 ?
    N11 Fe1 N21 5 . 5 89.01(5) ?
    N11 Fe1 N31 5 . 5 88.99(5) ?
    N21 Fe1 N31 5 . 5 88.28(5) ?
    Cl1 Fe2 Cl2 . . . 107.59(2) ?
    Cl1 Fe2 Cl1 . . 4 120.49(2) ?
    Cl1 Fe2 Cl2 . . 4 106.49(2) ?
    Cl2 Fe2 Cl1 . . 4 106.49(2) ?
    Cl2 Fe2 Cl2 . . 4 107.62(3) ?
    Cl1 Fe2 Cl2 4 . 4 107.59(2) ?
    C12 P C22 . . . 95.14(7) ?
    C12 P C32 . . . 94.98(7) ?
    C22 P C32 . . . 95.31(7) ?
    Fe1 N11 C12 . . . 124.10(10) ?
    Fe1 N11 C15 . . . 130.21(11) ?
    C12 N11 C15 . . . 105.68(13) ?
    P C12 N11 . . . 123.51(12) ?
    P C12 N13 . . . 125.56(12) ?
    N11 C12 N13 . . . 110.94(14) ?
    C12 N13 C131 . . . 126.62(15) ?
    C12 N13 C14 . . . 107.22(14) ?
    C131 N13 C14 . . . 126.02(15) ?
    N13 C131 H131a . . . 109.53 ?
    N13 C131 H131b . . . 109.16 ?
    N13 C131 H131c . . . 108.85 ?
    H131a C131 H131b . . . 109.61 ?
    H131a C131 H131c . . . 110.0 ?
    H131b C131 H131c . . . 109.6 ?
    N13 C14 C15 . . . 106.87(16) ?
    N13 C14 H14 . . . 126.69 ?
    C15 C14 H14 . . . 126.44 ?
    N11 C15 C14 . . . 109.29(15) ?
    N11 C15 H15 . . . 123.92 ?
    C14 C15 H15 . . . 126.79 ?
    Fe1 N21 C22 . . . 124.34(10) ?
    Fe1 N21 C25 . . . 129.39(11) ?
    C22 N21 C25 . . . 106.25(13) ?
    P C22 N21 . . . 123.38(11) ?
    P C22 N23 . . . 126.40(12) ?
    N21 C22 N23 . . . 110.22(13) ?
    C22 N23 C231 . . . 127.37(14) ?
    C22 N23 C24 . . . 107.58(14) ?
    C231 N23 C24 . . . 124.94(14) ?
    N23 C231 H231a . . . 109.31 ?
    N23 C231 H231b . . . 109.60 ?
    N23 C231 H231c . . . 109.60 ?
    H231a C231 H231b . . . 109.3 ?
    H231a C231 H231c . . . 109.3 ?
    H231b C231 H231c . . . 109.6 ?
    N23 C24 C25 . . . 106.84(14) ?
    N23 C24 H24 . . . 126.61 ?
    C25 C24 H24 . . . 126.56 ?
    N21 C25 C24 . . . 109.12(15) ?
    N21 C25 H25 . . . 125.41 ?
    C24 C25 H25 . . . 125.48 ?
    Fe1 N31 C32 . . . 123.48(11) ?
    Fe1 N31 C35 . . . 130.15(11) ?
    C32 N31 C35 . . . 106.37(13) ?
    P C32 N31 . . . 124.17(11) ?
    P C32 N33 . . . 125.38(12) ?
    N31 C32 N33 . . . 110.44(13) ?
    C32 N33 C331 . . . 126.27(14) ?
    C32 N33 C34 . . . 107.34(13) ?
    C331 N33 C34 . . . 126.39(14) ?
    N33 C331 H331a . . . 109.49 ?
    N33 C331 H331b . . . 109.17 ?
    N33 C331 H331c . . . 109.35 ?
    H331a C331 H331b . . . 109.6 ?
    H331a C331 H331c . . . 109.7 ?
    H331b C331 H331c . . . 109.48 ?
    N33 C34 C35 . . . 106.91(14) ?
    N33 C34 H34 . . . 126.61 ?
    C35 C34 H34 . . . 126.48 ?
    N31 C35 C34 . . . 108.94(14) ?
    N31 C35 H35 . . . 125.58 ?
    C34 C35 H35 . . . 125.48 ?
    C01 O01 H01 . . . 106.43 ?
    O01 C01 H01a . . . 109.6 ?
    O01 C01 H01b . . . 110.0 ?
    O01 C01 H01c . . . 109.1 ?
    H01a C01 H01b . . . 109.9 ?
    H01a C01 H01c . . . 108.8 ?
    H01b C01 H01c . . . 109.3 ?
    C02 O02 H02 . . . 104.48 ?
    O02 C02 H02a . . . 109.5 ?
    O02 C02 H02b . . . 109.6 ?
    O02 C02 H02c . . . 109.7 ?
    H02a C02 H02b . . . 109.2 ?
    H02a C02 H02c . . . 109.7 ?
    H02b C02 H02c . . . 109.2 ?
data_II
_chemical_name_systematic     ?
_chemical_name_common     ?
_chemical_formula_moiety     'C26 H32 Fe N12 O2 3+, 2Cl4 Fe -, Cl 1-'
_chemical_formula_sum     'C26 H32 Cl9 Fe3 N12 O2'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac     '[Fe (C13 H16 N6 O)2] [Fe Cl4]2 Cl'
_chemical_formula_weight     1031.24
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     -p_2ybc
loop_
    _symmetry_equiv_pos_as_xyz
    +x,+y,+z
    -x,1/2+y,1/2-z
    -x,-y,-z
    +x,1/2-y,1/2+z
_cell_length_a     9.7792(9)
_cell_length_b     14.8534(10)
_cell_length_c     13.3529(17)
_cell_angle_alpha     90.00000
_cell_angle_beta     93.835(2)
_cell_angle_gamma     90.00000
_cell_volume     1935.2(3)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     7062
_cell_measurement_theta_min     2.4
_cell_measurement_theta_max     26.8
_cell_measurement_temperature     150(2)
_cell_special_details
;      ?
;
_exptl_crystal_description     cuboid
_exptl_crystal_colour     'dark red'
_exptl_crystal_size_max     .45
_exptl_crystal_size_mid     .45
_exptl_crystal_size_min     .4
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     1.77
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1038
_exptl_absorpt_coefficient_mu     1.777
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
 (SADABS; Sheldrick, 1996)
;
_exptl_absorpt_correction_T_min     .68
_exptl_absorpt_correction_T_max     .80
_exptl_special_details
;      ?
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_radiation_source     'sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     38960
_diffrn_reflns_av_R_equivalents     .033
_diffrn_reflns_av_sigmaI/netI     .055
_diffrn_reflns_theta_min     2.05
_diffrn_reflns_theta_max     37.7
_diffrn_reflns_theta_full     37.5
_diffrn_measured_fraction_theta_max     .98
_diffrn_measured_fraction_theta_full     1.0
_diffrn_reflns_limit_h_min     -16
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_k_min     -25
_diffrn_reflns_limit_k_max     25
_diffrn_reflns_limit_l_min     -22
_diffrn_reflns_limit_l_max     22
_diffrn_reflns_reduction_process     ?
_diffrn_standards_number     0
_diffrn_standards_decay_%     0
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    ? ? ?
_reflns_number_total     10066
_reflns_number_gt     7754
_reflns_number_observed     ?
_reflns_threshold_expression     'I>2σ(I)'
_refine_ls_structure_factor_coef     F
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     .056
_refine_ls_R_factor_gt     .037
_refine_ls_wR_factor_all     .075
_refine_ls_wR_factor_ref     .067
_refine_ls_goodness_of_fit_all     .993
_refine_ls_goodness_of_fit_ref     1.022
_refine_ls_number_reflns     7754
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_number_constraints     0
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
;
 w = 1/(σ²(F) +  0.003F²)
;
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     .007
_refine_ls_shift/su_mean     .001
_refine_diff_density_max     1.435
_refine_diff_density_min     -.78
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_extinction_expression     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    C ? .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    H ? 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    Cl ? .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    Fe ? .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    N ? .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
    O ? .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
_computing_data_collection     'SMART (Siemens, 1995)'
_computing_cell_refinement     'SAINT (Siemens, 1995)'
_computing_data_reduction     'SAINT'
_computing_structure_solution
;
Xtal3.5 (Hall et al., 1995)
;
_computing_structure_refinement     'CRYLSQ in Xtal3.5'
_computing_molecular_graphics     Xtal3.5
_computing_publication_material     'BONDLA and CIFIO in Xtal3.5'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_calc_attached_atom
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Fe1 .50000 .00000 .50000 .01067(12) Uani ? ? 1.00000 ? ?
    Fe2 -.01174(3) .243653(17) .05474(2) .01686(11) Uani ? ? 1.00000 ? ?
    Cl1 -.10083(5) .11291(3) .09375(4) .0242(2) Uani ? ? 1.00000 ? ?
    Cl2 -.04784(5) .26675(3) -.10715(3) .0252(2) Uani ? ? 1.00000 ? ?
    Cl3 -.11127(5) .34894(3) .13991(3) .02262(18) Uani ? ? 1.00000 ? ?
    Cl4 .21135(5) .24393(3) .09358(4) .0273(2) Uani ? ? 1.00000 ? ?
    Cl5 .50000 .00000 .00000 .0232(3) Uani ? ? 1.00000 ? ?
    N11 .62699(13) -.03232(9) .61310(9) .0133(5) Uani ? ? 1.00000 ? ?
    C12 .62985(15) .01385(10) .69855(11) .0120(5) Uani ? ? 1.00000 ? ?
    N13 .73653(14) -.01272(9) .76064(10) .0136(5) Uani ? ? 1.00000 ? ?
    C131 .78867(18) .02546(13) .85791(12) .0193(7) Uani ? ? 1.00000 ? ?
    C14 .80304(17) -.08037(11) .71146(12) .0158(6) Uani ? ? 1.00000 ? ?
    C15 .73508(16) -.09234(11) .62065(12) .0155(6) Uani ? ? 1.00000 ? ?
    N21 .36069(14) .00358(9) .59830(10) .0140(5) Uani ? ? 1.00000 ? ?
    C22 .38249(15) .04811(10) .68493(11) .0123(5) Uani ? ? 1.00000 ? ?
    N23 .26671(14) .05260(9) .73365(10) .0151(5) Uani ? ? 1.00000 ? ?
    C231 .2374(2) .10247(13) .82517(14) .0216(7) Uani ? ? 1.00000 ? ?
    C24 .16680(17) .00700(12) .67607(13) .0184(7) Uani ? ? 1.00000 ? ?
    C25 .22509(16) -.02286(11) .59217(12) .0168(6) Uani ? ? 1.00000 ? ?
    N31 .53876(14) .12525(9) .53419(9) .0134(5) Uani ? ? 1.00000 ? ?
    C32 .54526(15) .15562(10) .62863(11) .0121(5) Uani ? ? 1.00000 ? ?
    N33 .56937(16) .24470(9) .62978(11) .0149(5) Uani ? ? 1.00000 ? ?
    C331 .5831(2) .30693(12) .71463(13) .0233(8) Uani ? ? 1.00000 ? ?
    C34 .5799(2) .27209(11) .53229(12) .0183(7) Uani ? ? 1.00000 ? ?
    C35 .5607(2) .19764(11) .47343(12) .0179(6) Uani ? ? 1.00000 ? ?
    C0 .52416(15) .08866(10) .71221(10) .0119(5) Uani ? ? 1.00000 ? ?
    O0 .53582(13) .13007(8) .80603(8) .0149(4) Uani ? ? 1.00000 ? ?
    H131a .87414 -.00238 .87705 .02700 Uiso ? ? 1.00000 ? ?
    H131b .80099 .08836 .85142 .04000 Uiso ? ? 1.00000 ? ?
    H131c .72493 .01232 .90639 .03000 Uiso ? ? 1.00000 ? ?
    H14 .88175 -.11256 .73719 .01700 Uiso ? ? 1.00000 ? ?
    H15 .75827 -.13418 .57076 .01400 Uiso ? ? 1.00000 ? ?
    H231a .26772 .16283 .81993 .03000 Uiso ? ? 1.00000 ? ?
    H231b .14158 .10073 .83280 .04400 Uiso ? ? 1.00000 ? ?
    H231c .28447 .07436 .88145 .04000 Uiso ? ? 1.00000 ? ?
    H24 .07448 -.00201 .69121 .03100 Uiso ? ? 1.00000 ? ?
    H25 .18029 -.05605 .53863 .02000 Uiso ? ? 1.00000 ? ?
    H331a .50035 .30814 .74760 .02200 Uiso ? ? 1.00000 ? ?
    H331b .65575 .28698 .76049 .02500 Uiso ? ? 1.00000 ? ?
    H331c .60353 .36539 .69136 .05000 Uiso ? ? 1.00000 ? ?
    H34 .59744 .33144 .50966 .02200 Uiso ? ? 1.00000 ? ?
    H35 .56216 .19604 .40243 .02300 Uiso ? ? 1.00000 ? ?
    H0 .52932 .08841 .85637 .04300 Uiso ? ? 1.00000 ? ?
_geom_special_details     ?
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Fe1 N11 . . 1.9500(13) yes
    Fe1 N21 . . 1.9547(14) yes
    Fe1 N31 . . 1.9468(13) yes
    Fe1 N11 . '3 656' 1.9500(13) ?
    Fe1 N21 . '3 656' 1.9547(14) ?
    Fe1 N31 . '3 656' 1.9468(13) ?
    Fe2 Cl1 . . 2.2051(5) ?
    Fe2 Cl2 . . 2.1939(6) ?
    Fe2 Cl3 . . 2.1987(5) ?
    Fe2 Cl4 . . 2.2085(6) ?
    N11 C12 . . 1.330(2) ?
    N11 C15 . . 1.381(2) ?
    C12 N13 . . 1.348(2) ?
    C12 C0 . . 1.537(2) ?
    N13 C131 . . 1.477(2) ?
    N13 C14 . . 1.386(2) ?
    C131 H131a . . .9520 ?
    C131 H131b . . .9467 ?
    C131 H131c . . .9485 ?
    C14 C15 . . 1.355(2) ?
    C14 H14 . . .9506 ?
    C15 H15 . . .9496 ?
    N21 C22 . . 1.337(2) ?
    N21 C25 . . 1.380(2) ?
    C22 N23 . . 1.345(2) ?
    C22 C0 . . 1.532(2) ?
    N23 C231 . . 1.474(2) ?
    N23 C24 . . 1.380(2) ?
    C231 H231a . . .949 ?
    C231 H231b . . .9492 ?
    C231 H231c . . .9513 ?
    C24 C25 . . 1.365(2) ?
    C24 H24 . . .9478 ?
    C25 H25 . . .9509 ?
    N31 C32 . . 1.337(2) ?
    N31 C35 . . 1.373(2) ?
    C32 N33 . . 1.344(2) ?
    C32 C0 . . 1.519(2) ?
    N33 C331 . . 1.461(2) ?
    N33 C34 . . 1.374(2) ?
    C331 H331a . . .947 ?
    C331 H331b . . .953 ?
    C331 H331c . . .9480 ?
    C34 C35 . . 1.362(2) ?
    C34 H34 . . .9512 ?
    C35 H35 . . .9494 ?
    C0 O0 . . 1.3935(18) ?
    O0 H0 . . .9189 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N11 Fe1 N21 . . . 85.59(6) yes
    N11 Fe1 N31 . . . 87.12(5) yes
    N11 Fe1 N11 . . '3 656' 180.0000 ?
    N11 Fe1 N21 . . '3 656' 94.41(6) ?
    N11 Fe1 N31 . . '3 656' 92.88(5) ?
    N21 Fe1 N31 . . . 87.13(6) yes
    N21 Fe1 N11 . . '3 656' 94.41(6) ?
    N21 Fe1 N21 . . '3 656' 180.0000 ?
    N21 Fe1 N31 . . '3 656' 92.87(6) ?
    N31 Fe1 N11 . . '3 656' 92.88(5) ?
    N31 Fe1 N21 . . '3 656' 92.87(6) ?
    N31 Fe1 N31 . . '3 656' 180.0000 ?
    N11 Fe1 N21 '3 656' . '3 656' 85.59(6) ?
    N11 Fe1 N31 '3 656' . '3 656' 87.12(5) ?
    N21 Fe1 N31 '3 656' . '3 656' 87.13(6) ?
    Cl1 Fe2 Cl2 . . . 109.29(2) ?
    Cl1 Fe2 Cl3 . . . 107.98(2) ?
    Cl1 Fe2 Cl4 . . . 110.23(2) ?
    Cl2 Fe2 Cl3 . . . 110.54(2) ?
    Cl2 Fe2 Cl4 . . . 108.81(2) ?
    Cl3 Fe2 Cl4 . . . 109.98(2) ?
    Fe1 N11 C12 . . . 120.88(10) ?
    Fe1 N11 C15 . . . 131.30(11) ?
    C12 N11 C15 . . . 107.34(12) ?
    N11 C12 N13 . . . 110.35(13) ?
    N11 C12 C0 . . . 119.93(12) ?
    N13 C12 C0 . . . 129.65(13) ?
    C12 N13 C131 . . . 129.51(14) ?
    C12 N13 C14 . . . 106.82(13) ?
    C131 N13 C14 . . . 123.36(13) ?
    N13 C131 H131a . . . 108.33 ?
    N13 C131 H131b . . . 109.70 ?
    N13 C131 H131c . . . 108.50 ?
    H131a C131 H131b . . . 109.78 ?
    H131a C131 H131c . . . 109.43 ?
    H131b C131 H131c . . . 111.05 ?
    N13 C14 C15 . . . 107.55(14) ?
    N13 C14 H14 . . . 125.99 ?
    C15 C14 H14 . . . 126.46 ?
    N11 C15 C14 . . . 107.93(14) ?
    N11 C15 H15 . . . 126.07 ?
    C14 C15 H15 . . . 126.00 ?
    Fe1 N21 C22 . . . 121.09(11) ?
    Fe1 N21 C25 . . . 131.49(11) ?
    C22 N21 C25 . . . 106.80(13) ?
    N21 C22 N23 . . . 110.63(13) ?
    N21 C22 C0 . . . 119.31(13) ?
    N23 C22 C0 . . . 129.99(13) ?
    C22 N23 C231 . . . 130.03(14) ?
    C22 N23 C24 . . . 107.08(13) ?
    C231 N23 C24 . . . 122.61(14) ?
    N23 C231 H231a . . . 109.55 ?
    N23 C231 H231b . . . 108.89 ?
    N23 C231 H231c . . . 108.88 ?
    H231a C231 H231b . . . 110.5 ?
    H231a C231 H231c . . . 109.61 ?
    H231b C231 H231c . . . 109.42 ?
    N23 C24 C25 . . . 107.33(14) ?
    N23 C24 H24 . . . 126.83 ?
    C25 C24 H24 . . . 125.83 ?
    N21 C25 C24 . . . 108.14(14) ?
    N21 C25 H25 . . . 125.78 ?
    C24 C25 H25 . . . 126.09 ?
    Fe1 N31 C32 . . . 122.68(10) ?
    Fe1 N31 C35 . . . 130.22(11) ?
    C32 N31 C35 . . . 107.09(13) ?
    N31 C32 N33 . . . 109.89(13) ?
    N31 C32 C0 . . . 118.15(12) ?
    N33 C32 C0 . . . 131.96(13) ?
    C32 N33 C331 . . . 129.68(14) ?
    C32 N33 C34 . . . 107.75(13) ?
    C331 N33 C34 . . . 122.56(14) ?
    N33 C331 H331a . . . 109.58 ?
    N33 C331 H331b . . . 109.10 ?
    N33 C331 H331c . . . 109.61 ?
    H331a C331 H331b . . . 109.30 ?
    H331a C331 H331c . . . 109.9 ?
    H331b C331 H331c . . . 109.3 ?
    N33 C34 C35 . . . 106.86(14) ?
    N33 C34 H34 . . . 127.00 ?
    C35 C34 H34 . . . 126.14 ?
    N31 C35 C34 . . . 108.41(14) ?
    N31 C35 H35 . . . 125.74 ?
    C34 C35 H35 . . . 125.86 ?
    C12 C0 C22 . . . 106.99(12) ?
    C12 C0 C32 . . . 105.11(12) ?
    C12 C0 O0 . . . 114.24(12) ?
    C22 C0 C32 . . . 104.35(11) ?
    C22 C0 O0 . . . 113.93(12) ?
    C32 C0 O0 . . . 111.37(12) ?
    C0 O0 H0 . . . 110.79 ?
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    ? ? ? ? ? ? ? ? ? ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_D
    _geom_hbond_site_symmetry_H
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    ? ? ? ? ? ? ? ? ? ? ?
