Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        P.G.Edwards
_publ_contact_author_address     
;
School of Chemistry
Cardiff University
Main Building
Park Place
Cardiff
CF10 3AT
UNITED KINGDOM
;

_publ_contact_author_email       EDWARDSPG@CARDIFF.AC.UK

_publ_section_title              
;
Iron Complexes of Facially Capping triphosphorus Macrocycles
;
loop_
_publ_author_name
P.G.Edwards
'K. M. Abdul Malik'
'Li-ling Ooi.'
'Andrew J. Price'

data_s92
_database_code_depnum_ccdc_archive 'CCDC 277603'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H52 F12 Fe2 P8'
_chemical_formula_weight         976.16

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   'P 2(1)/n'

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

_cell_length_a                   17.011(3)
_cell_length_b                   10.913(2)
_cell_length_c                   22.793(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.65(3)
_cell_angle_gamma                90.00
_cell_volume                     4231.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_process_details   'Walker & Stuart, 1983'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius FAST area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            68181
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         25.03
_reflns_number_total             7394
_reflns_number_gt                6210
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MADNES (Enraf Nonius, 1989)'
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0897P)^2^+16.8622P] 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         7394
_refine_ls_number_parameters     506
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1792
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.002
_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 0.51873(4) 0.26247(6) 0.13645(3) 0.0193(2) Uani 1 1 d . . .
Fe2 Fe 0.50354(4) 0.75591(6) 0.36194(3) 0.01907(19) Uani 1 1 d . . .
P1 P 0.63712(7) 0.33798(12) 0.13624(6) 0.0271(3) Uani 1 1 d . . .
H1A H 0.6712 0.2779 0.1549 0.032 Uiso 1 1 calc R . .
H1B H 0.6530 0.3432 0.0956 0.032 Uiso 1 1 calc R . .
P2 P 0.47887(7) 0.37639(11) 0.06445(5) 0.0234(3) Uani 1 1 d . . .
H2A H 0.4749 0.4599 0.0787 0.028 Uiso 1 1 calc R . .
H2B H 0.5190 0.3754 0.0346 0.028 Uiso 1 1 calc R . .
P3 P 0.55474(7) 0.11796(11) 0.07678(5) 0.0233(3) Uani 1 1 d . . .
H3A H 0.5148 0.0546 0.0774 0.028 Uiso 1 1 calc R . .
H3B H 0.5550 0.1518 0.0374 0.028 Uiso 1 1 calc R . .
P4 P 0.38659(7) 0.83061(12) 0.34635(6) 0.0286(3) Uani 1 1 d . . .
H4A H 0.3625 0.7792 0.3165 0.034 Uiso 1 1 calc R . .
H4B H 0.3575 0.8163 0.3821 0.034 Uiso 1 1 calc R . .
P5 P 0.45361(7) 0.61279(11) 0.41669(5) 0.0237(3) Uani 1 1 d . . .
H5A H 0.4933 0.5498 0.4219 0.028 Uiso 1 1 calc R . .
H5B H 0.4440 0.6480 0.4550 0.028 Uiso 1 1 calc R . .
P6 P 0.52606(7) 0.87278(11) 0.43741(5) 0.0226(3) Uani 1 1 d . . .
H6A H 0.5321 0.9561 0.4234 0.027 Uiso 1 1 calc R . .
H6B H 0.4798 0.8712 0.4619 0.027 Uiso 1 1 calc R . .
P7 P 0.86851(8) 0.76251(12) 0.11562(6) 0.0280(3) Uani 1 1 d . . .
P8 P 0.38292(8) 0.77712(12) 0.12565(6) 0.0291(3) Uani 1 1 d . . .
F1 F 0.8753(2) 0.6302(3) 0.14504(15) 0.0497(9) Uani 1 1 d U . .
F2 F 0.9009(3) 0.7085(4) 0.0565(2) 0.0718(12) Uani 1 1 d U . .
F3 F 0.7812(3) 0.7374(4) 0.0960(2) 0.0700(12) Uani 1 1 d U . .
F4 F 0.8645(2) 0.8956(3) 0.08584(16) 0.0538(9) Uani 1 1 d U . .
F5 F 0.8394(3) 0.8173(4) 0.1755(2) 0.0746(12) Uani 1 1 d U . .
F6 F 0.9560(3) 0.7919(4) 0.13746(19) 0.0676(11) Uani 1 1 d U . .
F7 F 0.3762(2) 0.9079(3) 0.09395(15) 0.0460(8) Uani 1 1 d U . .
F8 F 0.3918(2) 0.6458(3) 0.15621(15) 0.0486(8) Uani 1 1 d U . .
F9 F 0.4157(5) 0.7192(7) 0.0678(3) 0.0365(17) Uani 0.40 1 d PU . .
F9' F 0.4596(8) 0.7503(11) 0.0883(6) 0.052(3) Uani 0.30 1 d PU . .
F9'' F 0.3657(8) 0.7141(10) 0.0638(5) 0.044(3) Uani 0.30 1 d PU . .
F10 F 0.3049(6) 0.7335(8) 0.0954(4) 0.077(2) Uani 0.54 1 d PU . .
F10' F 0.2901(5) 0.7687(8) 0.1273(4) 0.058(2) Uani 0.46 1 d PU . .
F11 F 0.3234(8) 0.8187(12) 0.1746(5) 0.076(3) Uani 0.40 1 d PU . .
F11' F 0.3714(6) 0.8397(8) 0.1883(4) 0.085(2) Uani 0.60 1 d PU . .
F12 F 0.4507(6) 0.8289(10) 0.1681(5) 0.074(3) Uani 0.45 1 d PU . .
F12' F 0.4748(4) 0.8025(7) 0.1368(4) 0.0617(19) Uani 0.55 1 d PU . .
C1 C 0.4702(4) 0.1321(5) 0.1918(2) 0.0436(15) Uani 1 1 d . . .
H1 H 0.4741 0.0478 0.1868 0.052 Uiso 1 1 calc R . .
C2 C 0.5227(4) 0.2049(6) 0.2236(2) 0.0428(14) Uani 1 1 d . . .
H2 H 0.5675 0.1778 0.2434 0.051 Uiso 1 1 calc R . .
C3 C 0.4957(3) 0.3272(6) 0.2203(2) 0.0406(14) Uani 1 1 d . . .
H3 H 0.5197 0.3949 0.2376 0.049 Uiso 1 1 calc R . .
C4 C 0.4264(3) 0.3282(6) 0.1863(2) 0.0433(15) Uani 1 1 d . . .
H4 H 0.3963 0.3966 0.1770 0.052 Uiso 1 1 calc R . .
C5 C 0.4108(3) 0.2063(6) 0.1689(2) 0.0433(15) Uani 1 1 d . . .
H5 H 0.3683 0.1802 0.1461 0.052 Uiso 1 1 calc R . .
C6 C 0.6594(3) 0.4848(5) 0.1698(2) 0.0294(11) Uani 1 1 d . . .
C7 C 0.7075(3) 0.4907(6) 0.2160(3) 0.0412(13) Uani 1 1 d . . .
H7A H 0.7180 0.5658 0.2338 0.049 Uiso 1 1 calc R . .
H7B H 0.7308 0.4197 0.2307 0.049 Uiso 1 1 calc R . .
C8 C 0.6197(4) 0.5945(5) 0.1435(3) 0.0449(14) Uani 1 1 d . . .
H8A H 0.5638 0.5866 0.1475 0.067 Uiso 1 1 calc R . .
H8B H 0.6324 0.6002 0.1027 0.067 Uiso 1 1 calc R . .
H8C H 0.6373 0.6671 0.1635 0.067 Uiso 1 1 calc R . .
C9 C 0.3855(3) 0.3362(5) 0.0296(2) 0.0304(11) Uani 1 1 d . . .
C10 C 0.3248(4) 0.4104(6) 0.0351(3) 0.0502(16) Uani 1 1 d . . .
H10A H 0.2762 0.3887 0.0191 0.060 Uiso 1 1 calc R . .
H10B H 0.3305 0.4843 0.0550 0.060 Uiso 1 1 calc R . .
C11 C 0.3814(3) 0.2161(5) -0.0016(3) 0.0385(13) Uani 1 1 d . . .
H11A H 0.3874 0.1507 0.0262 0.058 Uiso 1 1 calc R . .
H11B H 0.4226 0.2116 -0.0299 0.058 Uiso 1 1 calc R . .
H11C H 0.3313 0.2086 -0.0212 0.058 Uiso 1 1 calc R . .
C12 C 0.6492(3) 0.0455(5) 0.0901(2) 0.0307(11) Uani 1 1 d . . .
C13 C 0.7066(3) 0.0629(5) 0.0530(3) 0.0410(14) Uani 1 1 d . . .
H13A H 0.7561 0.0298 0.0607 0.049 Uiso 1 1 calc R . .
H13B H 0.6979 0.1084 0.0190 0.049 Uiso 1 1 calc R . .
C14 C 0.6570(4) -0.0264(6) 0.1462(3) 0.0508(17) Uani 1 1 d . . .
H14A H 0.6187 -0.0910 0.1463 0.076 Uiso 1 1 calc R . .
H14B H 0.6485 0.0269 0.1790 0.076 Uiso 1 1 calc R . .
H14C H 0.7088 -0.0610 0.1490 0.076 Uiso 1 1 calc R . .
C15 C 0.5460(4) 0.8170(6) 0.2818(2) 0.0420(14) Uani 1 1 d . . .
H15 H 0.5261 0.8834 0.2608 0.050 Uiso 1 1 calc R . .
C16 C 0.5212(3) 0.6932(6) 0.2764(2) 0.0381(13) Uani 1 1 d . . .
H16 H 0.4823 0.6639 0.2511 0.046 Uiso 1 1 calc R . .
C17 C 0.5659(3) 0.6232(5) 0.3158(2) 0.0341(12) Uani 1 1 d . . .
H17 H 0.5614 0.5391 0.3214 0.041 Uiso 1 1 calc R . .
C18 C 0.6186(3) 0.7008(6) 0.3456(2) 0.0373(13) Uani 1 1 d . . .
H18 H 0.6551 0.6772 0.3741 0.045 Uiso 1 1 calc R . .
C19 C 0.6064(3) 0.8208(5) 0.3247(3) 0.0396(14) Uani 1 1 d . . .
H19 H 0.6334 0.8904 0.3371 0.048 Uiso 1 1 calc R . .
C20 C 0.3655(3) 0.9878(5) 0.3249(2) 0.0311(11) Uani 1 1 d . . .
C21 C 0.2846(4) 1.0133(7) 0.3028(4) 0.066(2) Uani 1 1 d . . .
H21A H 0.2471 0.9848 0.3308 0.099 Uiso 1 1 calc R . .
H21B H 0.2763 0.9718 0.2661 0.099 Uiso 1 1 calc R . .
H21C H 0.2782 1.1000 0.2971 0.099 Uiso 1 1 calc R . .
C22 C 0.4200(4) 1.0737(5) 0.3302(3) 0.0413(13) Uani 1 1 d . . .
H22A H 0.4085 1.1542 0.3199 0.050 Uiso 1 1 calc R . .
H22B H 0.4699 1.0535 0.3443 0.050 Uiso 1 1 calc R . .
C23 C 0.3637(3) 0.5382(4) 0.3922(2) 0.0290(11) Uani 1 1 d . . .
C24 C 0.3685(4) 0.4633(6) 0.3370(3) 0.0441(14) Uani 1 1 d . . .
H24A H 0.4094 0.4034 0.3412 0.066 Uiso 1 1 calc R . .
H24B H 0.3798 0.5161 0.3045 0.066 Uiso 1 1 calc R . .
H24C H 0.3192 0.4226 0.3301 0.066 Uiso 1 1 calc R . .
C25 C 0.2981(3) 0.5562(5) 0.4219(3) 0.0448(15) Uani 1 1 d . . .
H25A H 0.2511 0.5214 0.4089 0.054 Uiso 1 1 calc R . .
H25B H 0.2990 0.6036 0.4558 0.054 Uiso 1 1 calc R . .
C26 C 0.6114(3) 0.8365(5) 0.4838(2) 0.0329(12) Uani 1 1 d . . .
C27 C 0.6077(4) 0.7213(6) 0.5190(3) 0.0448(15) Uani 1 1 d . . .
H27A H 0.6073 0.6520 0.4930 0.067 Uiso 1 1 calc R . .
H27B H 0.5607 0.7211 0.5419 0.067 Uiso 1 1 calc R . .
H27C H 0.6528 0.7167 0.5446 0.067 Uiso 1 1 calc R . .
C28 C 0.6738(4) 0.9083(6) 0.4817(3) 0.0550(18) Uani 1 1 d . . .
H28A H 0.7189 0.8881 0.5030 0.066 Uiso 1 1 calc R . .
H28B H 0.6726 0.9790 0.4590 0.066 Uiso 1 1 calc R . .

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 0.0227(4) 0.0167(3) 0.0186(4) 0.0001(2) 0.0003(3) 0.0025(3)
Fe2 0.0214(4) 0.0173(3) 0.0185(4) 0.0010(2) 0.0014(3) -0.0017(2)
P1 0.0221(6) 0.0244(7) 0.0347(7) -0.0052(5) 0.0000(5) 0.0021(5)
P2 0.0284(6) 0.0183(6) 0.0236(6) 0.0021(5) -0.0011(5) 0.0045(5)
P3 0.0268(6) 0.0187(6) 0.0242(6) -0.0017(5) -0.0029(5) 0.0055(5)
P4 0.0227(6) 0.0232(7) 0.0396(7) 0.0033(5) -0.0041(5) -0.0023(5)
P5 0.0278(6) 0.0194(6) 0.0238(6) 0.0024(5) 0.0021(5) -0.0047(5)
P6 0.0269(6) 0.0187(6) 0.0224(6) -0.0004(5) 0.0004(5) -0.0039(5)
P7 0.0260(7) 0.0254(7) 0.0326(7) -0.0037(5) -0.0006(5) 0.0069(5)
P8 0.0279(7) 0.0257(7) 0.0338(7) 0.0021(6) 0.0002(5) 0.0041(5)
F1 0.0509(12) 0.0474(12) 0.0509(12) 0.0034(9) 0.0029(9) 0.0002(9)
F2 0.0757(14) 0.0706(14) 0.0694(14) -0.0012(10) 0.0071(10) 0.0034(10)
F3 0.0662(14) 0.0717(15) 0.0721(14) 0.0024(10) -0.0039(10) -0.0025(10)
F4 0.0548(12) 0.0502(12) 0.0563(12) 0.0021(9) -0.0035(9) 0.0028(9)
F5 0.0767(15) 0.0753(15) 0.0718(15) -0.0039(10) 0.0031(10) 0.0048(10)
F6 0.0643(14) 0.0675(14) 0.0710(14) 0.0037(10) -0.0039(9) -0.0005(10)
F7 0.0463(11) 0.0431(11) 0.0484(11) 0.0044(9) -0.0017(9) 0.0022(9)
F8 0.0496(12) 0.0460(12) 0.0502(12) 0.0043(9) 0.0004(9) 0.0003(9)
F9 0.0379(19) 0.0360(19) 0.0358(19) -0.0008(10) 0.0022(10) 0.0006(10)
F9' 0.051(3) 0.052(3) 0.052(3) 0.0016(10) 0.0022(10) 0.0015(10)
F9'' 0.045(3) 0.043(3) 0.043(3) -0.0005(10) -0.0009(10) -0.0002(10)
F10 0.077(3) 0.077(3) 0.077(3) 0.0006(10) -0.0024(10) -0.0017(10)
F10' 0.056(2) 0.058(2) 0.060(2) 0.0020(10) 0.0016(10) 0.0004(10)
F11 0.076(3) 0.076(3) 0.076(3) 0.0005(10) 0.0032(10) 0.0010(10)
F11' 0.087(2) 0.084(2) 0.083(2) -0.0011(10) 0.0011(10) 0.0002(10)
F12 0.075(3) 0.073(3) 0.074(3) 0.0003(10) -0.0025(10) -0.0009(10)
F12' 0.059(2) 0.062(2) 0.064(2) 0.0024(10) 0.0005(10) 0.0001(10)
C1 0.076(4) 0.027(3) 0.028(3) 0.005(2) 0.014(3) -0.009(3)
C2 0.050(3) 0.061(4) 0.018(2) 0.004(3) 0.000(2) 0.010(3)
C3 0.045(3) 0.044(3) 0.033(3) -0.017(3) 0.017(2) -0.010(3)
C4 0.039(3) 0.054(4) 0.038(3) 0.011(3) 0.020(3) 0.017(3)
C5 0.033(3) 0.068(4) 0.029(3) 0.006(3) 0.007(2) -0.021(3)
C6 0.029(3) 0.027(3) 0.033(3) -0.003(2) 0.006(2) -0.006(2)
C7 0.034(3) 0.045(3) 0.045(3) -0.007(3) -0.003(2) -0.006(3)
C8 0.054(4) 0.025(3) 0.056(4) 0.000(3) -0.006(3) -0.005(3)
C9 0.033(3) 0.029(3) 0.029(3) 0.002(2) -0.007(2) 0.005(2)
C10 0.043(3) 0.045(4) 0.062(4) -0.008(3) -0.017(3) 0.014(3)
C11 0.042(3) 0.032(3) 0.041(3) -0.003(2) -0.016(3) 0.003(2)
C12 0.031(3) 0.023(3) 0.038(3) -0.010(2) -0.008(2) 0.012(2)
C13 0.032(3) 0.042(3) 0.048(3) -0.012(3) -0.005(3) 0.013(2)
C14 0.060(4) 0.048(4) 0.044(3) -0.001(3) -0.011(3) 0.031(3)
C15 0.054(4) 0.043(3) 0.030(3) 0.016(3) 0.021(3) 0.009(3)
C16 0.043(3) 0.049(4) 0.022(3) -0.005(2) 0.006(2) 0.001(3)
C17 0.046(3) 0.026(3) 0.032(3) -0.002(2) 0.012(2) 0.007(2)
C18 0.025(3) 0.048(3) 0.039(3) -0.004(3) 0.009(2) 0.009(2)
C19 0.035(3) 0.040(3) 0.044(3) -0.007(3) 0.021(3) -0.013(2)
C20 0.030(3) 0.029(3) 0.034(3) 0.004(2) 0.004(2) 0.005(2)
C21 0.042(4) 0.050(4) 0.106(6) 0.021(4) -0.015(4) 0.010(3)
C22 0.049(3) 0.029(3) 0.046(3) 0.009(3) -0.005(3) -0.002(3)
C23 0.029(3) 0.020(2) 0.038(3) 0.004(2) -0.002(2) -0.006(2)
C24 0.048(3) 0.038(3) 0.047(3) 0.000(3) -0.011(3) -0.013(3)
C25 0.031(3) 0.036(3) 0.067(4) 0.009(3) 0.008(3) -0.011(2)
C26 0.036(3) 0.029(3) 0.034(3) 0.001(2) -0.010(2) -0.004(2)
C27 0.045(3) 0.046(4) 0.043(3) 0.010(3) -0.014(3) -0.006(3)
C28 0.050(4) 0.044(4) 0.071(4) 0.012(3) -0.029(3) -0.015(3)

_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 C4 2.077(5) . ?
Fe1 C3 2.079(5) . ?
Fe1 C5 2.079(5) . ?
Fe1 C1 2.079(5) . ?
Fe1 C2 2.083(5) . ?
Fe1 P2 2.1618(14) . ?
Fe1 P3 2.1751(14) . ?
Fe1 P1 2.1760(14) . ?
Fe2 C19 2.077(5) . ?
Fe2 C15 2.082(5) . ?
Fe2 C18 2.085(5) . ?
Fe2 C17 2.086(5) . ?
Fe2 C16 2.092(5) . ?
Fe2 P6 2.1719(14) . ?
Fe2 P4 2.1755(15) . ?
Fe2 P5 2.1775(14) . ?
P1 C6 1.813(5) . ?
P2 C9 1.821(5) . ?
P3 C12 1.814(5) . ?
P4 C20 1.818(5) . ?
P5 C23 1.815(5) . ?
P6 C26 1.829(5) . ?
P7 F3 1.570(5) . ?
P7 F2 1.576(5) . ?
P7 F5 1.576(5) . ?
P7 F1 1.596(4) . ?
P7 F6 1.597(4) . ?
P7 F4 1.604(4) . ?
P8 F10 1.563(9) . ?
P8 F9 1.570(8) . ?
P8 F11 1.582(12) . ?
P8 F10' 1.582(9) . ?
P8 F9'' 1.593(11) . ?
P8 F9' 1.593(13) . ?
P8 F11' 1.597(9) . ?
P8 F8 1.600(4) . ?
P8 F12 1.600(10) . ?
P8 F7 1.603(4) . ?
P8 F12' 1.604(8) . ?
F9 F9'' 0.857(12) . ?
F9 F9' 0.938(13) . ?
F9' F12' 1.267(15) . ?
F9' F9'' 1.731(17) . ?
F9'' F10 1.285(14) . ?
F10 F10' 0.862(11) . ?
F10' F11 1.329(15) . ?
F11 F11' 0.901(13) . ?
F11' F12 1.436(13) . ?
F12 F12' 0.875(11) . ?
C1 C2 1.391(9) . ?
C1 C5 1.392(9) . ?
C2 C3 1.413(9) . ?
C3 C4 1.403(8) . ?
C4 C5 1.412(9) . ?
C6 C7 1.329(8) . ?
C6 C8 1.496(8) . ?
C9 C10 1.321(8) . ?
C9 C11 1.492(7) . ?
C12 C13 1.313(8) . ?
C12 C14 1.504(8) . ?
C15 C19 1.412(9) . ?
C15 C16 1.420(9) . ?
C16 C17 1.398(8) . ?
C17 C18 1.402(8) . ?
C18 C19 1.408(8) . ?
C20 C22 1.323(8) . ?
C20 C21 1.487(8) . ?
C23 C25 1.326(8) . ?
C23 C24 1.503(8) . ?
C26 C28 1.321(8) . ?
C26 C27 1.493(8) . ?

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
C4 Fe1 C3 39.5(2) . . ?
C4 Fe1 C5 39.7(3) . . ?
C3 Fe1 C5 66.2(2) . . ?
C4 Fe1 C1 66.2(2) . . ?
C3 Fe1 C1 66.0(2) . . ?
C5 Fe1 C1 39.1(3) . . ?
C4 Fe1 C2 66.3(2) . . ?
C3 Fe1 C2 39.7(2) . . ?
C5 Fe1 C2 65.9(2) . . ?
C1 Fe1 C2 39.1(2) . . ?
C4 Fe1 P2 89.11(17) . . ?
C3 Fe1 P2 116.24(18) . . ?
C5 Fe1 P2 99.71(18) . . ?
C1 Fe1 P2 136.98(19) . . ?
C2 Fe1 P2 154.63(17) . . ?
C4 Fe1 P3 144.36(19) . . ?
C3 Fe1 P3 151.44(18) . . ?
C5 Fe1 P3 105.34(19) . . ?
C1 Fe1 P3 90.00(17) . . ?
C2 Fe1 P3 111.78(18) . . ?
P2 Fe1 P3 91.74(5) . . ?
C4 Fe1 P1 125.17(19) . . ?
C3 Fe1 P1 93.28(17) . . ?
C5 Fe1 P1 158.97(17) . . ?
C1 Fe1 P1 129.37(19) . . ?
C2 Fe1 P1 95.54(18) . . ?
P2 Fe1 P1 93.61(6) . . ?
P3 Fe1 P1 90.34(6) . . ?
C19 Fe2 C15 39.7(2) . . ?
C19 Fe2 C18 39.5(2) . . ?
C15 Fe2 C18 66.4(2) . . ?
C19 Fe2 C17 66.1(2) . . ?
C15 Fe2 C17 66.2(2) . . ?
C18 Fe2 C17 39.3(2) . . ?
C19 Fe2 C16 66.4(2) . . ?
C15 Fe2 C16 39.8(2) . . ?
C18 Fe2 C16 66.0(2) . . ?
C17 Fe2 C16 39.1(2) . . ?
C19 Fe2 P6 88.93(16) . . ?
C15 Fe2 P6 116.57(19) . . ?
C18 Fe2 P6 98.82(17) . . ?
C17 Fe2 P6 136.09(16) . . ?
C16 Fe2 P6 154.76(17) . . ?
C19 Fe2 P4 125.34(18) . . ?
C15 Fe2 P4 93.56(18) . . ?
C18 Fe2 P4 159.62(17) . . ?
C17 Fe2 P4 130.32(16) . . ?
C16 Fe2 P4 96.39(17) . . ?
P6 Fe2 P4 93.56(6) . . ?
C19 Fe2 P5 144.50(18) . . ?
C15 Fe2 P5 150.92(18) . . ?
C18 Fe2 P5 105.57(17) . . ?
C17 Fe2 P5 89.69(15) . . ?
C16 Fe2 P5 111.14(17) . . ?
P6 Fe2 P5 91.94(5) . . ?
P4 Fe2 P5 90.03(6) . . ?
C6 P1 Fe1 121.50(17) . . ?
C9 P2 Fe1 117.20(17) . . ?
C12 P3 Fe1 117.82(17) . . ?
C20 P4 Fe2 125.09(17) . . ?
C23 P5 Fe2 118.59(17) . . ?
C26 P6 Fe2 117.54(18) . . ?
F3 P7 F2 91.7(3) . . ?
F3 P7 F5 90.4(2) . . ?
F2 P7 F5 177.9(3) . . ?
F3 P7 F1 91.4(2) . . ?
F2 P7 F1 89.8(2) . . ?
F5 P7 F1 90.1(2) . . ?
F3 P7 F6 177.7(3) . . ?
F2 P7 F6 90.5(2) . . ?
F5 P7 F6 87.4(2) . . ?
F1 P7 F6 89.3(2) . . ?
F3 P7 F4 90.1(2) . . ?
F2 P7 F4 89.4(2) . . ?
F5 P7 F4 90.6(2) . . ?
F1 P7 F4 178.3(2) . . ?
F6 P7 F4 89.1(2) . . ?
F10 P8 F9 79.4(5) . . ?
F10 P8 F11 81.4(6) . . ?
F9 P8 F11 160.8(6) . . ?
F10 P8 F10' 31.8(4) . . ?
F9 P8 F10' 111.2(5) . . ?
F11 P8 F10' 49.7(6) . . ?
F10 P8 F9'' 48.1(5) . . ?
F9 P8 F9'' 31.4(4) . . ?
F11 P8 F9'' 129.5(7) . . ?
F10' P8 F9'' 79.8(6) . . ?
F10 P8 F9' 113.9(6) . . ?
F9 P8 F9' 34.5(5) . . ?
F11 P8 F9' 164.7(7) . . ?
F10' P8 F9' 145.6(6) . . ?
F9'' P8 F9' 65.8(6) . . ?
F10 P8 F11' 114.4(5) . . ?
F9 P8 F11' 166.2(5) . . ?
F11 P8 F11' 32.9(5) . . ?
F10' P8 F11' 82.6(5) . . ?
F9'' P8 F11' 162.4(6) . . ?
F9' P8 F11' 131.8(6) . . ?
F10 P8 F8 89.7(4) . . ?
F9 P8 F8 88.4(3) . . ?
F11 P8 F8 90.5(5) . . ?
F10' P8 F8 91.5(3) . . ?
F9'' P8 F8 90.8(4) . . ?
F9' P8 F8 89.7(5) . . ?
F11' P8 F8 90.3(3) . . ?
F10 P8 F12 167.7(6) . . ?
F9 P8 F12 112.9(5) . . ?
F11 P8 F12 86.3(6) . . ?
F10' P8 F12 136.0(6) . . ?
F9'' P8 F12 144.2(6) . . ?
F9' P8 F12 78.4(6) . . ?
F11' P8 F12 53.4(5) . . ?
F8 P8 F12 89.4(4) . . ?
F10 P8 F7 91.0(4) . . ?
F9 P8 F7 90.2(3) . . ?
F11 P8 F7 91.1(5) . . ?
F10' P8 F7 89.8(3) . . ?
F9'' P8 F7 88.5(4) . . ?
F9' P8 F7 88.7(5) . . ?
F11' P8 F7 90.8(3) . . ?
F8 P8 F7 178.4(2) . . ?
F12 P8 F7 90.3(4) . . ?
F10 P8 F12' 160.6(5) . . ?
F9 P8 F12' 81.2(5) . . ?
F11 P8 F12' 118.0(6) . . ?
F10' P8 F12' 167.6(5) . . ?
F9'' P8 F12' 112.5(6) . . ?
F9' P8 F12' 46.7(6) . . ?
F11' P8 F12' 85.0(5) . . ?
F8 P8 F12' 89.9(3) . . ?
F12 P8 F12' 31.7(4) . . ?
F7 P8 F12' 89.0(3) . . ?
F9'' F9 F9' 149.3(16) . . ?
F9'' F9 P8 75.7(10) . . ?
F9' F9 P8 74.1(9) . . ?
F9 F9' F12' 138.5(14) . . ?
F9 F9' P8 71.4(9) . . ?
F12' F9' P8 67.1(7) . . ?
F9 F9' F9'' 14.7(8) . . ?
F12' F9' F9'' 124.2(10) . . ?
P8 F9' F9'' 57.1(6) . . ?
F9 F9'' F10 137.2(14) . . ?
F9 F9'' P8 72.8(10) . . ?
F10 F9'' P8 64.7(6) . . ?
F9 F9'' F9' 16.1(8) . . ?
F10 F9'' F9' 121.8(10) . . ?
P8 F9'' F9' 57.1(6) . . ?
F10' F10 F9'' 142.3(13) . . ?
F10' F10 P8 75.4(9) . . ?
F9'' F10 P8 67.2(7) . . ?
F10 F10' F11 137.8(13) . . ?
F10 F10' P8 72.8(9) . . ?
F11 F10' P8 65.1(7) . . ?
F11' F11 F10' 139.6(15) . . ?
F11' F11 P8 74.5(10) . . ?
F10' F11 P8 65.2(7) . . ?
F11 F11' F12 136.0(13) . . ?
F11 F11' P8 72.6(10) . . ?
F12 F11' P8 63.4(6) . . ?
F12' F12 F11' 137.6(13) . . ?
F12' F12 P8 74.4(9) . . ?
F11' F12 P8 63.2(6) . . ?
F12 F12' F9' 140.1(13) . . ?
F12 F12' P8 73.9(9) . . ?
F9' F12' P8 66.2(7) . . ?
C2 C1 C5 108.8(5) . . ?
C2 C1 Fe1 70.6(3) . . ?
C5 C1 Fe1 70.4(3) . . ?
C1 C2 C3 107.8(5) . . ?
C1 C2 Fe1 70.3(3) . . ?
C3 C2 Fe1 70.0(3) . . ?
C4 C3 C2 107.8(5) . . ?
C4 C3 Fe1 70.2(3) . . ?
C2 C3 Fe1 70.3(3) . . ?
C3 C4 C5 107.6(5) . . ?
C3 C4 Fe1 70.4(3) . . ?
C5 C4 Fe1 70.2(3) . . ?
C1 C5 C4 108.0(5) . . ?
C1 C5 Fe1 70.4(3) . . ?
C4 C5 Fe1 70.0(3) . . ?
C7 C6 C8 123.4(5) . . ?
C7 C6 P1 120.0(4) . . ?
C8 C6 P1 116.6(4) . . ?
C10 C9 C11 123.4(5) . . ?
C10 C9 P2 119.4(4) . . ?
C11 C9 P2 117.2(4) . . ?
C13 C12 C14 124.3(5) . . ?
C13 C12 P3 119.6(4) . . ?
C14 C12 P3 116.0(4) . . ?
C19 C15 C16 107.5(5) . . ?
C19 C15 Fe2 69.9(3) . . ?
C16 C15 Fe2 70.5(3) . . ?
C17 C16 C15 107.8(5) . . ?
C17 C16 Fe2 70.2(3) . . ?
C15 C16 Fe2 69.7(3) . . ?
C16 C17 C18 108.8(5) . . ?
C16 C17 Fe2 70.7(3) . . ?
C18 C17 Fe2 70.3(3) . . ?
C17 C18 C19 107.9(5) . . ?
C17 C18 Fe2 70.4(3) . . ?
C19 C18 Fe2 69.9(3) . . ?
C18 C19 C15 108.1(5) . . ?
C18 C19 Fe2 70.5(3) . . ?
C15 C19 Fe2 70.4(3) . . ?
C22 C20 C21 122.9(5) . . ?
C22 C20 P4 120.5(4) . . ?
C21 C20 P4 116.6(4) . . ?
C25 C23 C24 124.2(5) . . ?
C25 C23 P5 119.2(4) . . ?
C24 C23 P5 116.6(4) . . ?
C28 C26 C27 123.9(5) . . ?
C28 C26 P6 118.9(4) . . ?
C27 C26 P6 117.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.625
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.113

data_98pge013
_database_code_depnum_ccdc_archive 'CCDC 277604'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H42 Fe N3 P3, B2 F8'
_chemical_formula_sum            'C21 H42 B2 F8 Fe N3 P3'
_chemical_formula_weight         658.96

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   10.296(2)
_cell_length_b                   15.901(3)
_cell_length_c                   18.784(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.23(3)
_cell_angle_gamma                90.00
_cell_volume                     3072.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9311
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      25.02

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.7886
_exptl_absorpt_correction_T_max  0.8707
_exptl_absorpt_process_details   'Walker & Stuart, 1983'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius FAST area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9317
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1311
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4358
_reflns_number_gt                2377
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MADNES (Enraf Nonius, 1989)'
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
All F atoms were restrained using ISOR due to prolate ellipsoids.

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^)+(0.0232P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4358
_refine_ls_number_parameters     412
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1094
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_restrained_S_all      0.988
_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 0.21210(8) 0.24442(4) 0.13054(4) 0.0423(2) Uani 1 1 d . A .
P1 P 0.34887(17) 0.34695(9) 0.16097(8) 0.0529(5) Uani 1 1 d . . .
P2 P 0.24226(15) 0.26366(8) 0.01500(7) 0.0465(4) Uani 1 1 d D . .
P3 P 0.04399(17) 0.33178(9) 0.13190(8) 0.0572(5) Uani 1 1 d . . .
C1 C 0.3982(8) 0.4178(4) 0.0896(3) 0.104(3) Uani 1 1 d . A .
H1A H 0.3223 0.4486 0.0720 0.124 Uiso 1 1 calc R . .
H1B H 0.4595 0.4583 0.1098 0.124 Uiso 1 1 calc R . .
C2 C 0.4588(6) 0.3758(4) 0.0276(3) 0.075(2) Uani 1 1 d D . .
H2A H 0.4669 0.4175 -0.0095 0.090 Uiso 1 1 d . . .
H2B H 0.5456 0.3588 0.0427 0.090 Uiso 1 1 d . . .
C3 C 0.4126(7) 0.2915(4) 0.0002(5) 0.052(3) Uani 0.65 1 d PD A 1
H3A H 0.4676 0.2485 0.0222 0.062 Uiso 0.65 1 calc PR A 1
H3B H 0.4256 0.2896 -0.0506 0.062 Uiso 0.65 1 calc PR A 1
C3' C 0.3478(14) 0.3434(10) -0.0204(6) 0.077(7) Uani 0.35 1 d PD A 2
H3'1 H 0.3848 0.3209 -0.0632 0.093 Uiso 0.35 1 calc PR A 2
H3'2 H 0.2942 0.3911 -0.0348 0.093 Uiso 0.35 1 calc PR A 2
C4A C 0.1502(7) 0.3413(5) -0.0368(4) 0.063(3) Uani 0.65 1 d PD A 3
H4A H 0.1953 0.3947 -0.0325 0.076 Uiso 0.65 1 calc PR A 3
H4B H 0.1505 0.3249 -0.0866 0.076 Uiso 0.65 1 calc PR A 3
C5A C 0.0104(6) 0.3547(4) -0.0171(3) 0.081(2) Uani 0.65 1 d PD A 3
H5A H -0.0349 0.3888 -0.0529 0.097 Uiso 0.65 1 calc PR A 3
H5B H -0.0340 0.3011 -0.0142 0.097 Uiso 0.65 1 calc PR A 3
C4B C 0.0891(12) 0.2776(8) -0.0346(7) 0.070(6) Uani 0.35 1 d PD A 4
H4C H 0.1069 0.2795 -0.0849 0.084 Uiso 0.35 1 calc PR A 4
H4D H 0.0358 0.2284 -0.0270 0.084 Uiso 0.35 1 calc PR A 4
C5B C 0.0104(6) 0.3547(4) -0.0171(3) 0.081(2) Uani 0.35 1 d PD A 4
H5C H 0.0333 0.3973 -0.0514 0.097 Uiso 0.35 1 calc PR A 4
H5D H -0.0796 0.3401 -0.0282 0.097 Uiso 0.35 1 calc PR A 4
C6 C 0.0113(7) 0.3985(4) 0.0541(3) 0.093(2) Uani 1 1 d . A .
H6A H -0.0725 0.4253 0.0592 0.112 Uiso 1 1 calc R B 3
H6B H 0.0764 0.4426 0.0541 0.112 Uiso 1 1 calc R B 3
C7 C 0.0491(7) 0.4085(4) 0.2046(3) 0.081(2) Uani 1 1 d . A .
H7A H -0.0291 0.4425 0.2008 0.097 Uiso 1 1 calc R . .
H7B H 0.0479 0.3783 0.2495 0.097 Uiso 1 1 calc R . .
C8 C 0.1667(7) 0.4671(4) 0.2067(4) 0.080(2) Uani 1 1 d . . .
H8A H 0.1533 0.5112 0.2413 0.096 Uiso 1 1 calc R A .
H8B H 0.1733 0.4936 0.1604 0.096 Uiso 1 1 calc R . .
C9 C 0.2949(7) 0.4219(4) 0.2260(3) 0.091(2) Uani 1 1 d . A .
H9A H 0.2855 0.3928 0.2708 0.109 Uiso 1 1 calc R . .
H9B H 0.3623 0.4640 0.2334 0.109 Uiso 1 1 calc R . .
C10 C 0.5053(7) 0.3159(4) 0.1995(4) 0.097(2) Uani 1 1 d . . .
H10A H 0.5492 0.2816 0.1651 0.116 Uiso 1 1 calc R . .
H10B H 0.5574 0.3660 0.2079 0.116 Uiso 1 1 calc R . .
C11 C 0.4998(7) 0.2656(4) 0.2710(3) 0.096(2) Uani 1 1 d . . .
H11A H 0.5866 0.2574 0.2902 0.143 Uiso 1 1 d . . .
H11B H 0.4599 0.2120 0.2616 0.143 Uiso 1 1 d . . .
H11C H 0.4500 0.2965 0.3040 0.143 Uiso 1 1 d . . .
C12A C 0.2205(11) 0.1676(6) -0.0385(4) 0.062(4) Uani 0.65 1 d PD A 1
H12A H 0.2493 0.1203 -0.0094 0.074 Uiso 0.65 1 calc PR A 1
H12B H 0.1282 0.1603 -0.0490 0.074 Uiso 0.65 1 calc PR A 1
C13A C 0.2898(7) 0.1633(4) -0.1084(2) 0.079(2) Uani 0.65 1 d PD A 1
H13A H 0.2366 0.1890 -0.1454 0.119 Uiso 0.65 1 calc PR A 1
H13B H 0.3053 0.1055 -0.1203 0.119 Uiso 0.65 1 calc PR A 1
H13C H 0.3712 0.1926 -0.1035 0.119 Uiso 0.65 1 calc PR A 1
C12B C 0.304(2) 0.1691(10) -0.0277(4) 0.093(11) Uani 0.35 1 d PD A 2
H12C H 0.3955 0.1639 -0.0144 0.112 Uiso 0.35 1 calc PR A 2
H12D H 0.2601 0.1210 -0.0079 0.112 Uiso 0.35 1 calc PR A 2
C13B C 0.2898(7) 0.1633(4) -0.1084(2) 0.079(2) Uani 0.35 1 d PD A 2
H13D H 0.2134 0.1308 -0.1214 0.119 Uiso 0.35 1 d P C 2
H13E H 0.3647 0.1367 -0.1267 0.119 Uiso 0.35 1 d P D 2
H13F H 0.2803 0.2188 -0.1282 0.119 Uiso 0.35 1 d P E 2
C14 C -0.1193(7) 0.2831(4) 0.1357(4) 0.115(3) Uani 1 1 d . A .
H14A H -0.1850 0.3264 0.1285 0.139 Uiso 1 1 calc R . .
H14B H -0.1303 0.2428 0.0971 0.139 Uiso 1 1 calc R . .
C15 C -0.1391(8) 0.2415(5) 0.2017(4) 0.126(3) Uani 1 1 d . . .
H15A H -0.2253 0.2185 0.2013 0.189 Uiso 1 1 calc R A .
H15B H -0.1285 0.2811 0.2401 0.189 Uiso 1 1 calc R . .
H15C H -0.0768 0.1970 0.2081 0.189 Uiso 1 1 calc R . .
N1 N 0.3553(5) 0.1621(3) 0.1316(2) 0.0464(12) Uani 1 1 d . . .
C16 C 0.4320(6) 0.1125(3) 0.1299(3) 0.0491(16) Uani 1 1 d . A .
C17 C 0.5355(6) 0.0488(3) 0.1283(3) 0.075(2) Uani 1 1 d . . .
H17A H 0.5800 0.0536 0.0845 0.113 Uiso 1 1 calc R A .
H17B H 0.4981 -0.0063 0.1315 0.113 Uiso 1 1 calc R . .
H17C H 0.5961 0.0575 0.1678 0.113 Uiso 1 1 calc R . .
N2 N 0.1892(4) 0.2189(3) 0.2312(2) 0.0507(13) Uani 1 1 d . . .
C18 C 0.1760(6) 0.1986(3) 0.2881(3) 0.0552(17) Uani 1 1 d . A .
C19 C 0.1567(7) 0.1723(4) 0.3610(3) 0.081(2) Uani 1 1 d . . .
H19A H 0.1055 0.2135 0.3845 0.121 Uiso 1 1 calc R A .
H19B H 0.2396 0.1667 0.3858 0.121 Uiso 1 1 calc R . .
H19C H 0.1124 0.1191 0.3608 0.121 Uiso 1 1 calc R . .
N3 N 0.0970(4) 0.1486(3) 0.1100(2) 0.0463(12) Uani 1 1 d . . .
C20 C 0.0378(6) 0.0896(4) 0.1060(3) 0.0529(16) Uani 1 1 d . A .
C21 C -0.0436(6) 0.0137(3) 0.1032(3) 0.079(2) Uani 1 1 d . . .
H21A H 0.0097 -0.0346 0.0947 0.118 Uiso 1 1 calc R A .
H21B H -0.1086 0.0190 0.0655 0.118 Uiso 1 1 calc R . .
H21C H -0.0850 0.0069 0.1478 0.118 Uiso 1 1 calc R . .
B1 B 0.7082(11) 0.5377(6) 0.1898(5) 0.073(3) Uani 1 1 d . . .
F1 F 0.5949(9) 0.5713(6) 0.1830(5) 0.161(3) Uani 0.80 1 d PU . .
F2 F 0.8094(8) 0.5905(4) 0.1956(4) 0.137(3) Uani 0.80 1 d PU . .
F1' F 0.659(3) 0.6229(12) 0.1653(11) 0.088(7) Uani 0.20 1 d PU . .
F2' F 0.789(4) 0.553(3) 0.2306(19) 0.151(13) Uani 0.20 1 d PU . .
F3 F 0.7215(5) 0.4892(3) 0.1310(2) 0.1244(16) Uani 1 1 d U . .
F4 F 0.7153(8) 0.4840(4) 0.2453(3) 0.137(2) Uani 0.80 1 d PU . .
F4' F 0.589(3) 0.5252(15) 0.2273(11) 0.084(7) Uani 0.20 1 d PU . .
B2 B -0.2669(11) 0.1188(6) -0.0513(7) 0.087(3) Uani 1 1 d . . .
F5 F -0.1595(5) 0.1507(4) -0.0633(3) 0.178(2) Uani 1 1 d U . .
F6 F -0.2672(5) 0.0391(3) -0.0333(3) 0.161(2) Uani 1 1 d U . .
F7 F -0.3155(9) 0.1665(4) 0.0022(3) 0.168(3) Uani 0.80 1 d PU . .
F8 F -0.3417(8) 0.1286(4) -0.1136(3) 0.137(2) Uani 0.80 1 d PU . .
F8' F -0.385(3) 0.1359(14) -0.0463(15) 0.244(10) Uani 0.40 1 d PU . .

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 0.0436(5) 0.0398(4) 0.0439(4) -0.0014(4) 0.0062(3) -0.0018(4)
P1 0.0545(12) 0.0503(9) 0.0541(10) -0.0082(8) 0.0058(8) -0.0091(8)
P2 0.0505(11) 0.0444(9) 0.0450(8) -0.0013(7) 0.0061(7) -0.0029(8)
P3 0.0525(12) 0.0498(9) 0.0698(11) -0.0043(9) 0.0079(9) 0.0062(9)
C1 0.129(8) 0.088(5) 0.095(5) -0.001(4) 0.028(5) -0.060(5)
C2 0.077(6) 0.089(5) 0.060(4) -0.005(4) 0.023(4) -0.021(4)
C3 0.064(7) 0.045(5) 0.048(6) 0.007(5) 0.018(5) -0.011(5)
C3' 0.14(2) 0.047(11) 0.051(12) 0.009(10) 0.025(13) -0.040(13)
C4A 0.081(9) 0.047(6) 0.061(6) 0.008(5) -0.006(6) 0.000(6)
C5A 0.081(6) 0.071(5) 0.088(5) 0.002(4) -0.013(4) 0.011(4)
C4B 0.092(17) 0.075(13) 0.043(10) 0.008(10) 0.000(10) 0.004(12)
C5B 0.081(6) 0.071(5) 0.088(5) 0.002(4) -0.013(4) 0.011(4)
C6 0.119(7) 0.081(5) 0.078(5) 0.012(4) -0.015(4) 0.038(5)
C7 0.079(6) 0.075(4) 0.089(5) -0.023(4) 0.013(4) 0.023(4)
C8 0.081(6) 0.054(4) 0.106(5) -0.023(4) 0.017(5) 0.000(4)
C9 0.088(6) 0.094(5) 0.091(5) -0.044(4) 0.016(5) -0.022(5)
C10 0.080(6) 0.089(5) 0.120(6) -0.016(5) -0.003(5) -0.020(5)
C11 0.080(6) 0.141(6) 0.064(4) 0.006(5) -0.017(4) -0.012(5)
C12A 0.106(12) 0.040(6) 0.040(6) -0.011(5) -0.002(6) -0.020(6)
C13A 0.118(7) 0.069(4) 0.052(4) -0.010(3) 0.010(4) 0.007(4)
C12B 0.17(3) 0.080(16) 0.031(12) 0.015(11) -0.032(14) 0.012(19)
C13B 0.118(7) 0.069(4) 0.052(4) -0.010(3) 0.010(4) 0.007(4)
C14 0.087(7) 0.111(6) 0.152(7) 0.042(6) 0.043(6) 0.036(5)
C15 0.099(7) 0.147(7) 0.135(7) -0.006(6) 0.038(6) 0.012(6)
N1 0.040(3) 0.046(3) 0.053(3) 0.001(2) 0.008(3) 0.002(2)
C16 0.053(5) 0.053(4) 0.042(3) 0.002(3) 0.008(3) -0.003(3)
C17 0.063(5) 0.073(4) 0.090(5) 0.011(4) 0.012(4) 0.029(4)
N2 0.052(3) 0.056(3) 0.045(3) 0.000(3) 0.010(3) -0.003(2)
C18 0.062(5) 0.048(4) 0.057(4) -0.004(3) 0.012(4) -0.002(3)
C19 0.117(7) 0.081(4) 0.045(4) 0.000(3) 0.019(4) -0.022(4)
N3 0.045(3) 0.042(3) 0.051(3) 0.001(2) 0.000(2) -0.007(2)
C20 0.054(4) 0.055(4) 0.050(4) 0.001(3) 0.011(3) 0.001(3)
C21 0.084(6) 0.058(4) 0.095(5) -0.009(4) 0.012(4) -0.031(4)
B1 0.085(8) 0.069(6) 0.065(6) -0.011(6) -0.014(6) -0.001(6)
F1 0.127(6) 0.149(6) 0.203(7) -0.035(6) -0.044(6) 0.053(6)
F2 0.139(6) 0.133(5) 0.138(5) 0.011(4) -0.012(4) -0.083(5)
F1' 0.102(12) 0.077(10) 0.087(10) 0.031(8) 0.014(9) 0.008(9)
F2' 0.144(16) 0.154(16) 0.152(16) -0.012(10) -0.017(10) -0.002(10)
F3 0.136(4) 0.120(3) 0.118(3) -0.021(3) 0.016(3) -0.008(3)
F4 0.174(7) 0.131(5) 0.106(4) 0.048(4) 0.014(4) -0.020(5)
F4' 0.082(11) 0.093(10) 0.080(10) 0.002(8) 0.020(9) -0.027(9)
B2 0.073(8) 0.066(6) 0.126(9) 0.019(6) 0.034(7) -0.001(6)
F5 0.114(5) 0.163(5) 0.260(6) -0.017(4) 0.043(5) -0.036(4)
F6 0.174(5) 0.091(3) 0.215(5) 0.030(3) -0.035(4) 0.008(3)
F7 0.217(7) 0.165(5) 0.125(5) -0.037(4) 0.050(5) 0.012(5)
F8 0.179(6) 0.141(4) 0.088(4) 0.024(4) -0.035(4) -0.024(4)
F8' 0.240(14) 0.233(13) 0.258(14) -0.005(10) 0.007(10) 0.017(10)

_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 N2 1.956(4) . ?
Fe1 N3 1.960(4) . ?
Fe1 N1 1.971(5) . ?
Fe1 P1 2.2147(17) . ?
Fe1 P3 2.2202(18) . ?
Fe1 P2 2.2254(15) . ?
P1 C10 1.809(7) . ?
P1 C9 1.809(6) . ?
P1 C1 1.838(6) . ?
P2 C3' 1.813(9) . ?
P2 C4B 1.814(9) . ?
P2 C4A 1.816(7) . ?
P2 C12B 1.829(10) . ?
P2 C12A 1.837(7) . ?
P2 C3 1.840(7) . ?
P3 C6 1.826(6) . ?
P3 C7 1.831(6) . ?
P3 C14 1.855(8) . ?
C1 C2 1.498(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.507(5) . ?
C2 C3' 1.519(5) . ?
C2 H2A 0.9682 . ?
C2 H2B 0.9659 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3' H3'1 0.9700 . ?
C3' H3'2 0.9700 . ?
C4A C5A 1.516(5) . ?
C4A H4A 0.9700 . ?
C4A H4B 0.9700 . ?
C5A C6 1.508(8) . ?
C5A H5A 0.9700 . ?
C5A H5B 0.9700 . ?
C4B H4C 0.9700 . ?
C4B H4D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.527(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.534(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.567(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9590 . ?
C11 H11B 0.9608 . ?
C11 H11C 0.9545 . ?
C12A C13A 1.519(5) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C13A H13A 0.9600 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9600 . ?
C13A H13D 0.9647 . ?
C13A H13E 0.9557 . ?
C13A H13F 0.9618 . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C14 C15 1.427(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N1 C16 1.117(6) . ?
C16 C17 1.473(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
N2 C18 1.131(6) . ?
C18 C19 1.452(7) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
N3 C20 1.120(6) . ?
C20 C21 1.469(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
B1 F2' 1.13(4) . ?
B1 F1 1.285(11) . ?
B1 F2 1.339(11) . ?
B1 F4 1.347(11) . ?
B1 F3 1.359(8) . ?
B1 F4' 1.45(2) . ?
B1 F1' 1.51(2) . ?
F1 F4' 1.11(2) . ?
F1 F1' 1.115(19) . ?
F2 F2' 0.92(4) . ?
F2 F1' 1.70(3) . ?
F2' F4 1.37(4) . ?
F4 F4' 1.49(3) . ?
B2 F5 1.245(10) . ?
B2 F8' 1.25(2) . ?
B2 F6 1.312(9) . ?
B2 F7 1.369(11) . ?
B2 F8 1.384(13) . ?
F7 F8' 1.24(2) . ?
F8 F8' 1.36(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
N2 Fe1 N3 86.22(18) . . ?
N2 Fe1 N1 88.33(18) . . ?
N3 Fe1 N1 86.09(18) . . ?
N2 Fe1 P1 90.14(14) . . ?
N3 Fe1 P1 175.43(14) . . ?
N1 Fe1 P1 91.05(14) . . ?
N2 Fe1 P3 89.72(14) . . ?
N3 Fe1 P3 91.33(14) . . ?
N1 Fe1 P3 176.86(14) . . ?
P1 Fe1 P3 91.41(7) . . ?
N2 Fe1 P2 175.82(13) . . ?
N3 Fe1 P2 91.23(13) . . ?
N1 Fe1 P2 88.19(13) . . ?
P1 Fe1 P2 92.24(6) . . ?
P3 Fe1 P2 93.65(7) . . ?
C10 P1 C9 101.7(3) . . ?
C10 P1 C1 101.1(3) . . ?
C9 P1 C1 100.9(3) . . ?
C10 P1 Fe1 116.7(2) . . ?
C9 P1 Fe1 116.8(2) . . ?
C1 P1 Fe1 117.0(2) . . ?
C3' P2 C4B 104.3(7) . . ?
C3' P2 C4A 68.6(5) . . ?
C4B P2 C4A 38.4(5) . . ?
C3' P2 C12B 101.0(10) . . ?
C4B P2 C12B 100.6(7) . . ?
C4A P2 C12B 120.4(4) . . ?
C3' P2 C12A 116.3(6) . . ?
C4B P2 C12A 74.7(5) . . ?
C4A P2 C12A 102.8(5) . . ?
C12B P2 C12A 27.6(8) . . ?
C3' P2 C3 35.7(5) . . ?
C4B P2 C3 135.0(6) . . ?
C4A P2 C3 103.6(4) . . ?
C12B P2 C3 77.5(9) . . ?
C12A P2 C3 102.4(4) . . ?
C3' P2 Fe1 124.2(4) . . ?
C4B P2 Fe1 111.5(5) . . ?
C4A P2 Fe1 121.8(3) . . ?
C12B P2 Fe1 112.3(4) . . ?
C12A P2 Fe1 113.6(3) . . ?
C3 P2 Fe1 110.5(3) . . ?
C6 P3 C7 102.0(3) . . ?
C6 P3 C14 97.7(3) . . ?
C7 P3 C14 104.5(3) . . ?
C6 P3 Fe1 118.3(2) . . ?
C7 P3 Fe1 115.2(2) . . ?
C14 P3 Fe1 116.6(2) . . ?
C2 C1 P1 115.4(4) . . ?
C2 C1 H1A 108.4 . . ?
P1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
P1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 C3 121.7(5) . . ?
C1 C2 C3' 106.6(9) . . ?
C3 C2 C3' 43.5(7) . . ?
C1 C2 H2A 107.7 . . ?
C3 C2 H2A 113.5 . . ?
C3' C2 H2A 83.6 . . ?
C1 C2 H2B 107.8 . . ?
C3 C2 H2B 97.3 . . ?
C3' C2 H2B 138.2 . . ?
H2A C2 H2B 107.4 . . ?
C2 C3 P2 116.9(5) . . ?
C2 C3 H3A 108.1 . . ?
P2 C3 H3A 108.1 . . ?
C2 C3 H3B 108.1 . . ?
P2 C3 H3B 108.1 . . ?
H3A C3 H3B 107.3 . . ?
C2 C3' P2 117.8(7) . . ?
C2 C3' H3'1 107.8 . . ?
P2 C3' H3'1 107.8 . . ?
C2 C3' H3'2 107.8 . . ?
P2 C3' H3'2 107.8 . . ?
H3'1 C3' H3'2 107.2 . . ?
C5A C4A P2 116.4(5) . . ?
C5A C4A H4A 108.2 . . ?
P2 C4A H4A 108.2 . . ?
C5A C4A H4B 108.2 . . ?
P2 C4A H4B 108.2 . . ?
H4A C4A H4B 107.3 . . ?
C6 C5A C4A 108.0(6) . . ?
C6 C5A H5A 110.1 . . ?
C4A C5A H5A 110.1 . . ?
C6 C5A H5B 110.1 . . ?
C4A C5A H5B 110.1 . . ?
H5A C5A H5B 108.4 . . ?
P2 C4B H4C 108.1 . . ?
P2 C4B H4D 108.1 . . ?
H4C C4B H4D 107.3 . . ?
C5A C6 P3 115.9(4) . . ?
C5A C6 H6A 108.3 . . ?
P3 C6 H6A 108.3 . . ?
C5A C6 H6B 108.3 . . ?
P3 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
C8 C7 P3 115.2(5) . . ?
C8 C7 H7A 108.5 . . ?
P3 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
P3 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 C9 113.2(5) . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 P1 115.7(5) . . ?
C8 C9 H9A 108.4 . . ?
P1 C9 H9A 108.4 . . ?
C8 C9 H9B 108.4 . . ?
P1 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C11 C10 P1 114.9(5) . . ?
C11 C10 H10A 108.5 . . ?
P1 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
P1 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 110.0 . . ?
H11B C11 H11C 109.9 . . ?
C13A C12A P2 117.3(5) . . ?
C13A C12A H12A 108.0 . . ?
P2 C12A H12A 108.0 . . ?
C13A C12A H12B 108.0 . . ?
P2 C12A H12B 108.0 . . ?
H12A C12A H12B 107.2 . . ?
C12A C13A H13D 80.7 . . ?
H13A C13A H13D 66.9 . . ?
H13B C13A H13D 64.5 . . ?
H13C C13A H13D 169.7 . . ?
C12A C13A H13E 138.1 . . ?
H13A C13A H13E 111.8 . . ?
H13B C13A H13E 49.4 . . ?
H13C C13A H13E 62.2 . . ?
H13D C13A H13E 109.4 . . ?
C12A C13A H13F 104.4 . . ?
H13A C13A H13F 44.1 . . ?
H13B C13A H13F 143.4 . . ?
H13C C13A H13F 70.5 . . ?
H13D C13A H13F 108.9 . . ?
H13E C13A H13F 109.7 . . ?
P2 C12B H12C 107.9 . . ?
P2 C12B H12D 107.9 . . ?
H12C C12B H12D 107.2 . . ?
C15 C14 P3 112.7(6) . . ?
C15 C14 H14A 109.0 . . ?
P3 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
P3 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 N1 Fe1 176.0(5) . . ?
N1 C16 C17 178.5(7) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 N2 Fe1 175.4(5) . . ?
N2 C18 C19 179.0(7) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 N3 Fe1 171.3(5) . . ?
N3 C20 C21 177.4(6) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
F2' B1 F1 128(2) . . ?
F2' B1 F2 43(2) . . ?
F1 B1 F2 116.6(9) . . ?
F2' B1 F4 66(2) . . ?
F1 B1 F4 111.3(10) . . ?
F2 B1 F4 108.4(9) . . ?
F2' B1 F3 125(2) . . ?
F1 B1 F3 105.9(8) . . ?
F2 B1 F3 108.6(9) . . ?
F4 B1 F3 105.4(8) . . ?
F2' B1 F4' 108(2) . . ?
F1 B1 F4' 47.4(11) . . ?
F2 B1 F4' 135.8(11) . . ?
F4 B1 F4' 63.9(12) . . ?
F3 B1 F4' 115.5(11) . . ?
F2' B1 F1' 104(2) . . ?
F1 B1 F1' 46.1(10) . . ?
F2 B1 F1' 73.2(11) . . ?
F4 B1 F1' 144.3(11) . . ?
F3 B1 F1' 107.7(11) . . ?
F4' B1 F1' 89.6(15) . . ?
F4' F1 F1' 140(2) . . ?
F4' F1 B1 74.3(15) . . ?
F1' F1 B1 77.7(15) . . ?
F2' F2 B1 57(3) . . ?
F2' F2 F1' 102(3) . . ?
B1 F2 F1' 58.1(8) . . ?
F1 F1' B1 56.2(10) . . ?
F1 F1' F2 102.7(15) . . ?
B1 F1' F2 48.7(8) . . ?
F2 F2' B1 81(3) . . ?
F2 F2' F4 144(4) . . ?
B1 F2' F4 64(2) . . ?
B1 F4 F2' 49.3(15) . . ?
B1 F4 F4' 61.5(9) . . ?
F2' F4 F4' 95.0(18) . . ?
F1 F4' B1 58.3(11) . . ?
F1 F4' F4 112.7(19) . . ?
B1 F4' F4 54.5(11) . . ?
F5 B2 F8' 142.8(15) . . ?
F5 B2 F6 116.8(10) . . ?
F8' B2 F6 100.3(13) . . ?
F5 B2 F7 105.0(10) . . ?
F8' B2 F7 56.1(12) . . ?
F6 B2 F7 109.9(8) . . ?
F5 B2 F8 105.7(9) . . ?
F8' B2 F8 62.0(14) . . ?
F6 B2 F8 108.7(9) . . ?
F7 B2 F8 110.6(9) . . ?
F8' F7 B2 57.1(12) . . ?
F8' F8 B2 54.2(11) . . ?
F7 F8' B2 66.8(16) . . ?
F7 F8' F8 121(2) . . ?
B2 F8' F8 63.9(15) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Fe1 P1 C10 70.0(3) . . . . ?
N3 Fe1 P1 C10 32.8(18) . . . . ?
N1 Fe1 P1 C10 -18.3(3) . . . . ?
P3 Fe1 P1 C10 159.7(3) . . . . ?
P2 Fe1 P1 C10 -106.5(3) . . . . ?
N2 Fe1 P1 C9 -50.5(3) . . . . ?
N3 Fe1 P1 C9 -87.7(18) . . . . ?
N1 Fe1 P1 C9 -138.8(3) . . . . ?
P3 Fe1 P1 C9 39.2(3) . . . . ?
P2 Fe1 P1 C9 133.0(3) . . . . ?
N2 Fe1 P1 C1 -170.1(3) . . . . ?
N3 Fe1 P1 C1 152.7(17) . . . . ?
N1 Fe1 P1 C1 101.5(3) . . . . ?
P3 Fe1 P1 C1 -80.4(3) . . . . ?
P2 Fe1 P1 C1 13.3(3) . . . . ?
N2 Fe1 P2 C3' -126(2) . . . . ?
N3 Fe1 P2 C3' -177.9(8) . . . . ?
N1 Fe1 P2 C3' -91.9(8) . . . . ?
P1 Fe1 P2 C3' -0.9(8) . . . . ?
P3 Fe1 P2 C3' 90.7(8) . . . . ?
N2 Fe1 P2 C4B 108(2) . . . . ?
N3 Fe1 P2 C4B 56.0(4) . . . . ?
N1 Fe1 P2 C4B 142.0(4) . . . . ?
P1 Fe1 P2 C4B -127.0(4) . . . . ?
P3 Fe1 P2 C4B -35.4(4) . . . . ?
N2 Fe1 P2 C4A 150(2) . . . . ?
N3 Fe1 P2 C4A 97.7(4) . . . . ?
N1 Fe1 P2 C4A -176.3(4) . . . . ?
P1 Fe1 P2 C4A -85.3(3) . . . . ?
P3 Fe1 P2 C4A 6.2(3) . . . . ?
N2 Fe1 P2 C12B -4(2) . . . . ?
N3 Fe1 P2 C12B -56.1(9) . . . . ?
N1 Fe1 P2 C12B 30.0(9) . . . . ?
P1 Fe1 P2 C12B 121.0(9) . . . . ?
P3 Fe1 P2 C12B -147.5(9) . . . . ?
N2 Fe1 P2 C12A 26(2) . . . . ?
N3 Fe1 P2 C12A -26.1(4) . . . . ?
N1 Fe1 P2 C12A 59.9(4) . . . . ?
P1 Fe1 P2 C12A 150.9(4) . . . . ?
P3 Fe1 P2 C12A -117.5(4) . . . . ?
N2 Fe1 P2 C3 -88(2) . . . . ?
N3 Fe1 P2 C3 -140.5(3) . . . . ?
N1 Fe1 P2 C3 -54.4(3) . . . . ?
P1 Fe1 P2 C3 36.5(3) . . . . ?
P3 Fe1 P2 C3 128.1(3) . . . . ?
N2 Fe1 P3 C6 171.2(3) . . . . ?
N3 Fe1 P3 C6 -102.6(3) . . . . ?
N1 Fe1 P3 C6 -137(3) . . . . ?
P1 Fe1 P3 C6 81.0(3) . . . . ?
P2 Fe1 P3 C6 -11.3(3) . . . . ?
N2 Fe1 P3 C7 50.2(3) . . . . ?
N3 Fe1 P3 C7 136.4(3) . . . . ?
N1 Fe1 P3 C7 102(3) . . . . ?
P1 Fe1 P3 C7 -40.0(2) . . . . ?
P2 Fe1 P3 C7 -132.3(2) . . . . ?
N2 Fe1 P3 C14 -72.8(3) . . . . ?
N3 Fe1 P3 C14 13.4(3) . . . . ?
N1 Fe1 P3 C14 -21(3) . . . . ?
P1 Fe1 P3 C14 -162.9(3) . . . . ?
P2 Fe1 P3 C14 104.7(3) . . . . ?
C10 P1 C1 C2 71.3(6) . . . . ?
C9 P1 C1 C2 175.6(6) . . . . ?
Fe1 P1 C1 C2 -56.6(6) . . . . ?
P1 C1 C2 C3 36.9(10) . . . . ?
P1 C1 C2 C3' 82.0(8) . . . . ?
C1 C2 C3 P2 26.9(11) . . . . ?
C3' C2 C3 P2 -53.7(8) . . . . ?
C3' P2 C3 C2 52.8(7) . . . . ?
C4B P2 C3 C2 90.3(8) . . . . ?
C4A P2 C3 C2 64.2(8) . . . . ?
C12B P2 C3 C2 -177.2(8) . . . . ?
C12A P2 C3 C2 170.9(7) . . . . ?
Fe1 P2 C3 C2 -67.8(7) . . . . ?
C1 C2 C3' P2 -63.3(14) . . . . ?
C3 C2 C3' P2 55.6(8) . . . . ?
C4B P2 C3' C2 153.6(12) . . . . ?
C4A P2 C3' C2 139.2(16) . . . . ?
C12B P2 C3' C2 -102.3(14) . . . . ?
C12A P2 C3' C2 -126.7(12) . . . . ?
C3 P2 C3' C2 -52.8(7) . . . . ?
Fe1 P2 C3' C2 24.5(17) . . . . ?
C3' P2 C4A C5A -152.9(10) . . . . ?
C4B P2 C4A C5A 50.0(6) . . . . ?
C12B P2 C4A C5A 116.7(12) . . . . ?
C12A P2 C4A C5A 93.6(7) . . . . ?
C3 P2 C4A C5A -160.0(6) . . . . ?
Fe1 P2 C4A C5A -35.0(8) . . . . ?
P2 C4A C5A C6 70.5(8) . . . . ?
C4A C5A C6 P3 -78.7(7) . . . . ?
C7 P3 C6 C5A 175.8(5) . . . . ?
C14 P3 C6 C5A -77.6(6) . . . . ?
Fe1 P3 C6 C5A 48.2(6) . . . . ?
C6 P3 C7 C8 -70.1(6) . . . . ?
C14 P3 C7 C8 -171.4(5) . . . . ?
Fe1 P3 C7 C8 59.4(5) . . . . ?
P3 C7 C8 C9 -68.5(7) . . . . ?
C7 C8 C9 P1 66.8(7) . . . . ?
C10 P1 C9 C8 175.3(5) . . . . ?
C1 P1 C9 C8 71.4(6) . . . . ?
Fe1 P1 C9 C8 -56.5(6) . . . . ?
C9 P1 C10 C11 66.8(5) . . . . ?
C1 P1 C10 C11 170.5(5) . . . . ?
Fe1 P1 C10 C11 -61.5(5) . . . . ?
C3' P2 C12A C13A -1.2(11) . . . . ?
C4B P2 C12A C13A 97.5(10) . . . . ?
C4A P2 C12A C13A 71.1(9) . . . . ?
C12B P2 C12A C13A -62.2(11) . . . . ?
C3 P2 C12A C13A -36.3(9) . . . . ?
Fe1 P2 C12A C13A -155.4(7) . . . . ?
C6 P3 C14 C15 -165.4(6) . . . . ?
C7 P3 C14 C15 -60.8(6) . . . . ?
Fe1 P3 C14 C15 67.5(6) . . . . ?
N2 Fe1 N1 C16 109(7) . . . . ?
N3 Fe1 N1 C16 22(7) . . . . ?
P1 Fe1 N1 C16 -161(7) . . . . ?
P3 Fe1 N1 C16 57(8) . . . . ?
P2 Fe1 N1 C16 -69(7) . . . . ?
Fe1 N1 C16 C17 163(19) . . . . ?
N3 Fe1 N2 C18 37(6) . . . . ?
N1 Fe1 N2 C18 -49(6) . . . . ?
P1 Fe1 N2 C18 -140(6) . . . . ?
P3 Fe1 N2 C18 128(6) . . . . ?
P2 Fe1 N2 C18 -15(8) . . . . ?
Fe1 N2 C18 C19 -77(37) . . . . ?
N2 Fe1 N3 C20 -32(3) . . . . ?
N1 Fe1 N3 C20 57(3) . . . . ?
P1 Fe1 N3 C20 6(5) . . . . ?
P3 Fe1 N3 C20 -121(3) . . . . ?
P2 Fe1 N3 C20 145(3) . . . . ?
Fe1 N3 C20 C21 75(17) . . . . ?
F2' B1 F1 F4' -80(4) . . . . ?
F2 B1 F1 F4' -128.9(15) . . . . ?
F4 B1 F1 F4' -3.9(14) . . . . ?
F3 B1 F1 F4' 110.2(14) . . . . ?
F1' B1 F1 F4' -150.4(19) . . . . ?
F2' B1 F1 F1' 71(4) . . . . ?
F2 B1 F1 F1' 21.5(16) . . . . ?
F4 B1 F1 F1' 146.5(15) . . . . ?
F3 B1 F1 F1' -99.4(14) . . . . ?
F4' B1 F1 F1' 150.4(19) . . . . ?
F1 B1 F2 F2' 118(3) . . . . ?
F4 B1 F2 F2' -8(3) . . . . ?
F3 B1 F2 F2' -122(3) . . . . ?
F4' B1 F2 F2' 63(4) . . . . ?
F1' B1 F2 F2' 134(3) . . . . ?
F2' B1 F2 F1' -134(3) . . . . ?
F1 B1 F2 F1' -16.0(12) . . . . ?
F4 B1 F2 F1' -142.5(11) . . . . ?
F3 B1 F2 F1' 103.5(11) . . . . ?
F4' B1 F2 F1' -71(2) . . . . ?
F4' F1 F1' B1 47(3) . . . . ?
F4' F1 F1' F2 32(3) . . . . ?
B1 F1 F1' F2 -15.3(11) . . . . ?
F2' B1 F1' F1 -130(2) . . . . ?
F2 B1 F1' F1 -160.0(15) . . . . ?
F4 B1 F1' F1 -62(3) . . . . ?
F3 B1 F1' F1 95.3(12) . . . . ?
F4' B1 F1' F1 -21.3(14) . . . . ?
F2' B1 F1' F2 30(2) . . . . ?
F1 B1 F1' F2 160.0(15) . . . . ?
F4 B1 F1' F2 98(2) . . . . ?
F3 B1 F1' F2 -104.6(10) . . . . ?
F4' B1 F1' F2 138.7(12) . . . . ?
F2' F2 F1' F1 -21(3) . . . . ?
B1 F2 F1' F1 16.9(12) . . . . ?
F2' F2 F1' B1 -38(2) . . . . ?
F1' F2 F2' B1 38(2) . . . . ?
B1 F2 F2' F4 13(5) . . . . ?
F1' F2 F2' F4 52(6) . . . . ?
F1 B1 F2' F2 -89(3) . . . . ?
F4 B1 F2' F2 171(3) . . . . ?
F3 B1 F2' F2 79(3) . . . . ?
F4' B1 F2' F2 -139(2) . . . . ?
F1' B1 F2' F2 -45(3) . . . . ?
F1 B1 F2' F4 99(2) . . . . ?
F2 B1 F2' F4 -171(3) . . . . ?
F3 B1 F2' F4 -93(2) . . . . ?
F4' B1 F2' F4 49.4(17) . . . . ?
F1' B1 F2' F4 143.6(13) . . . . ?
F1 B1 F4 F2' -123(2) . . . . ?
F2 B1 F4 F2' 6(2) . . . . ?
F3 B1 F4 F2' 122(2) . . . . ?
F4' B1 F4 F2' -127(2) . . . . ?
F1' B1 F4 F2' -81(3) . . . . ?
F2' B1 F4 F4' 127(2) . . . . ?
F1 B1 F4 F4' 3.2(12) . . . . ?
F2 B1 F4 F4' 132.7(12) . . . . ?
F3 B1 F4 F4' -111.2(12) . . . . ?
F1' B1 F4 F4' 46(2) . . . . ?
F2 F2' F4 B1 -15(5) . . . . ?
F2 F2' F4 F4' -60(6) . . . . ?
B1 F2' F4 F4' -45.1(17) . . . . ?
F1' F1 F4' B1 -48(3) . . . . ?
F1' F1 F4' F4 -44(3) . . . . ?
B1 F1 F4' F4 3.5(13) . . . . ?
F2' B1 F4' F1 125(3) . . . . ?
F2 B1 F4' F1 86(2) . . . . ?
F4 B1 F4' F1 176.0(15) . . . . ?
F3 B1 F4' F1 -88.5(14) . . . . ?
F1' B1 F4' F1 20.9(14) . . . . ?
F2' B1 F4' F4 -51(2) . . . . ?
F1 B1 F4' F4 -176.0(15) . . . . ?
F2 B1 F4' F4 -90(2) . . . . ?
F3 B1 F4' F4 95.5(12) . . . . ?
F1' B1 F4' F4 -155.1(12) . . . . ?
B1 F4 F4' F1 -3.7(13) . . . . ?
F2' F4 F4' F1 34(2) . . . . ?
F2' F4 F4' B1 37.7(15) . . . . ?
F5 B2 F7 F8' 144.4(18) . . . . ?
F6 B2 F7 F8' -89.2(16) . . . . ?
F8 B2 F7 F8' 30.9(15) . . . . ?
F5 B2 F8 F8' -142.0(16) . . . . ?
F6 B2 F8 F8' 92.0(15) . . . . ?
F7 B2 F8 F8' -28.8(13) . . . . ?
B2 F7 F8' F8 -34.9(16) . . . . ?
F5 B2 F8' F7 -68(3) . . . . ?
F6 B2 F8' F7 107.2(12) . . . . ?
F8 B2 F8' F7 -147.0(14) . . . . ?
F5 B2 F8' F8 79(3) . . . . ?
F6 B2 F8' F8 -105.8(11) . . . . ?
F7 B2 F8' F8 147.0(14) . . . . ?
B2 F8 F8' F7 35.8(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.803
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.803
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.069

data_s92_3
_database_code_depnum_ccdc_archive 'CCDC 277605'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H48 Fe P3, B F4'
_chemical_formula_sum            'C25 H48 B F4 Fe P3'
_chemical_formula_weight         584.20

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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 bca'

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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.3920(1)
_cell_length_b                   13.1650(1)
_cell_length_c                   27.211(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5513.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25.03

_exptl_crystal_description       plate-like
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7504
_exptl_absorpt_correction_T_max  0.9629
_exptl_absorpt_process_details   'Walker & Stuart, 1983'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius FAST area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17175
_diffrn_reflns_av_R_equivalents  0.1618
_diffrn_reflns_av_sigmaI/netI    0.4550
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.62
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4244
_reflns_number_gt                1164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MADNES (Enraf Nonius, 1989)'
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;

ISOR restraints were used on the following due to high mean square
displacement parameters C13 C12 C15 C9 C10 C14 C16 C22 C23 C25
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^)+(0.0395P)^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_number_reflns         4244
_refine_ls_number_parameters     293
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.2166
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.1668
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      0.709
_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 0.02447(9) 0.27495(9) 0.39704(5) 0.0274(4) Uani 1 1 d . . .
P1 P -0.0374(2) 0.34134(17) 0.33100(11) 0.0338(8) Uani 1 1 d . . .
P2 P 0.14082(17) 0.2387(2) 0.35323(11) 0.0357(8) Uani 1 1 d . . .
P3 P -0.0289(2) 0.1227(2) 0.38033(11) 0.0557(11) Uani 1 1 d . . .
C1 C 0.0123(8) 0.4155(8) 0.4367(4) 0.036(3) Uani 1 1 d . . .
C2 C -0.0520(8) 0.3438(8) 0.4534(4) 0.036(3) Uani 1 1 d . . .
C3 C -0.0047(7) 0.2619(8) 0.4746(4) 0.039(3) Uani 1 1 d . . .
C4 C 0.0846(8) 0.2805(10) 0.4682(4) 0.048(3) Uani 1 1 d . . .
C5 C 0.0947(9) 0.3735(10) 0.4442(4) 0.053(4) Uani 1 1 d . . .
C6 C -0.0066(8) 0.5244(6) 0.4227(4) 0.075(5) Uani 1 1 d . . .
H6A H -0.0655 0.5292 0.4092 0.113 Uiso 1 1 calc R . .
H6B H 0.0354 0.5470 0.3980 0.113 Uiso 1 1 calc R . .
H6C H -0.0020 0.5676 0.4520 0.113 Uiso 1 1 calc R . .
C7 C -0.1453(7) 0.3647(7) 0.4604(4) 0.054(4) Uani 1 1 d . . .
H7A H -0.1614 0.3501 0.4946 0.081 Uiso 1 1 calc R . .
H7B H -0.1794 0.3215 0.4383 0.081 Uiso 1 1 calc R . .
H7C H -0.1571 0.4362 0.4531 0.081 Uiso 1 1 calc R . .
C8 C -0.0428(8) 0.1859(7) 0.5090(4) 0.067(4) Uani 1 1 d . . .
H8A H -0.0213 0.1180 0.5006 0.101 Uiso 1 1 calc R . .
H8B H -0.1063 0.1872 0.5063 0.101 Uiso 1 1 calc R . .
H8C H -0.0258 0.2026 0.5428 0.101 Uiso 1 1 calc R . .
C9 C 0.1509(9) 0.2173(8) 0.4936(5) 0.092(5) Uani 1 1 d U . .
H9A H 0.2076 0.2511 0.4918 0.138 Uiso 1 1 calc R . .
H9B H 0.1546 0.1507 0.4776 0.138 Uiso 1 1 calc R . .
H9C H 0.1344 0.2084 0.5281 0.138 Uiso 1 1 calc R . .
C10 C 0.1742(8) 0.4367(8) 0.4411(5) 0.083(4) Uani 1 1 d U . .
H10A H 0.2254 0.3941 0.4471 0.125 Uiso 1 1 calc R . .
H10B H 0.1716 0.4906 0.4659 0.125 Uiso 1 1 calc R . .
H10C H 0.1783 0.4670 0.4083 0.125 Uiso 1 1 calc R . .
C11 C 0.0277(7) 0.4344(6) 0.2968(3) 0.042(3) Uani 1 1 d . . .
H11A H 0.0040 0.4409 0.2632 0.051 Uiso 1 1 calc R . .
H11B H 0.0224 0.5015 0.3130 0.051 Uiso 1 1 calc R . .
C12 C 0.1165(11) 0.4081(10) 0.2938(6) 0.114(6) Uani 1 1 d U . .
H12A H 0.1301 0.4211 0.2588 0.136 Uiso 1 1 calc R . .
H12B H 0.1451 0.4641 0.3120 0.136 Uiso 1 1 calc R . .
C13 C 0.1667(11) 0.3295(11) 0.3041(6) 0.136(6) Uani 1 1 d U . .
H13A H 0.2251 0.3570 0.3115 0.164 Uiso 1 1 calc R . .
H13B H 0.1723 0.2896 0.2735 0.164 Uiso 1 1 calc R . .
C14 C 0.1429(10) 0.1272(9) 0.3157(5) 0.108(5) Uani 1 1 d U . .
H14A H 0.0975 0.1322 0.2901 0.129 Uiso 1 1 calc R . .
H14B H 0.2000 0.1218 0.2991 0.129 Uiso 1 1 calc R . .
C15 C 0.1277(10) 0.0349(10) 0.3461(6) 0.118(6) Uani 1 1 d U . .
H15A H 0.1150 -0.0204 0.3225 0.141 Uiso 1 1 calc R . .
H15B H 0.1846 0.0182 0.3611 0.141 Uiso 1 1 calc R . .
C16 C 0.0629(8) 0.0238(7) 0.3861(5) 0.073(4) Uani 1 1 d U . .
H16A H 0.0921 0.0321 0.4182 0.087 Uiso 1 1 calc R . .
H16B H 0.0376 -0.0453 0.3849 0.087 Uiso 1 1 calc R . .
C17 C -0.0728(7) 0.0876(7) 0.3190(4) 0.050(4) Uani 1 1 d . . .
H17A H -0.0236 0.0692 0.2973 0.060 Uiso 1 1 calc R . .
H17B H -0.1096 0.0263 0.3228 0.060 Uiso 1 1 calc R . .
C18 C -0.1251(7) 0.1680(7) 0.2941(4) 0.046(3) Uani 1 1 d . . .
H18A H -0.1713 0.1920 0.3167 0.055 Uiso 1 1 calc R . .
H18B H -0.1534 0.1392 0.2646 0.055 Uiso 1 1 calc R . .
C19 C -0.0681(7) 0.2573(6) 0.2792(4) 0.044(3) Uani 1 1 d . . .
H19A H -0.0993 0.2980 0.2542 0.053 Uiso 1 1 calc R . .
H19B H -0.0145 0.2308 0.2637 0.053 Uiso 1 1 calc R . .
C20 C -0.1403(7) 0.4081(7) 0.3401(4) 0.045(3) Uani 1 1 d . . .
H20A H -0.1835 0.3582 0.3521 0.055 Uiso 1 1 calc R . .
H20B H -0.1317 0.4586 0.3667 0.055 Uiso 1 1 calc R . .
C21 C -0.1799(7) 0.4636(7) 0.2958(4) 0.067(4) Uani 1 1 d . . .
H21A H -0.1342 0.5005 0.2782 0.100 Uiso 1 1 calc R . .
H21B H -0.2242 0.5116 0.3072 0.100 Uiso 1 1 calc R . .
H21C H -0.2067 0.4139 0.2736 0.100 Uiso 1 1 calc R . .
C22 C 0.2468(7) 0.2263(8) 0.3846(5) 0.071(4) Uani 1 1 d U . .
H22A H 0.2576 0.2899 0.4030 0.085 Uiso 1 1 calc R . .
H22B H 0.2418 0.1710 0.4091 0.085 Uiso 1 1 calc R . .
C23 C 0.3261(9) 0.2049(8) 0.3531(5) 0.093(5) Uani 1 1 d U . .
H23A H 0.3785 0.2098 0.3734 0.140 Uiso 1 1 calc R . .
H23B H 0.3291 0.2548 0.3265 0.140 Uiso 1 1 calc R . .
H23C H 0.3217 0.1365 0.3392 0.140 Uiso 1 1 calc R . .
C24 C -0.1053(14) 0.0324(14) 0.4181(8) 0.195(9) Uiso 1 1 d . . .
H24A H -0.1167 -0.0325 0.4010 0.234 Uiso 1 1 calc R . .
H24B H -0.0830 0.0191 0.4516 0.234 Uiso 1 1 calc R . .
C25 C -0.1740(13) 0.0936(13) 0.4182(7) 0.187(9) Uiso 1 1 d . . .
H25A H -0.1826 0.1216 0.3851 0.281 Uiso 1 1 calc R . .
H25B H -0.1645 0.1492 0.4415 0.281 Uiso 1 1 calc R . .
H25C H -0.2257 0.0551 0.4279 0.281 Uiso 1 1 calc R . .
B1 B 0.0986(12) 0.2496(10) 0.1517(7) 0.108(7) Uiso 1 1 d D . .
F1 F 0.0664(5) 0.1794(4) 0.1830(3) 0.081(2) Uiso 1 1 d D A .
F2A F 0.0366(11) 0.2724(10) 0.1187(5) 0.071(6) Uiso 0.488(17) 1 d P A 1
F3A F 0.1555(11) 0.1932(10) 0.1255(6) 0.096(8) Uiso 0.488(17) 1 d PD A 1
F4A F 0.1280(13) 0.3343(12) 0.1755(6) 0.096(7) Uiso 0.488(17) 1 d P A 1
F2B F 0.0453(13) 0.3257(11) 0.1658(7) 0.130(9) Uiso 0.512(17) 1 d PD A 2
F3B F 0.1761(17) 0.2736(15) 0.1644(8) 0.160(10) Uiso 0.512(17) 1 d P A 2
F4B F 0.086(2) 0.249(2) 0.1072(14) 0.256(15) Uiso 0.512(17) 1 d P A 2

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 0.0273(8) 0.0370(8) 0.0180(8) -0.0033(7) -0.0025(10) 0.0007(8)
P1 0.035(2) 0.0347(15) 0.032(2) -0.0034(13) -0.0077(18) 0.0087(15)
P2 0.0288(17) 0.0432(17) 0.0350(18) 0.0035(13) 0.0043(18) 0.0031(16)
P3 0.066(3) 0.0644(19) 0.037(2) 0.0109(15) -0.010(2) -0.036(2)
C1 0.036(9) 0.051(8) 0.020(7) -0.011(5) 0.002(6) 0.009(6)
C2 0.025(8) 0.065(8) 0.017(7) -0.005(6) 0.004(6) 0.011(6)
C3 0.042(9) 0.056(7) 0.020(6) -0.010(5) 0.003(6) 0.015(6)
C4 0.038(9) 0.083(9) 0.024(7) -0.005(7) -0.007(7) 0.024(8)
C5 0.043(10) 0.072(9) 0.042(9) -0.029(7) 0.011(8) -0.010(8)
C6 0.133(15) 0.039(6) 0.053(9) -0.009(6) 0.019(9) 0.000(7)
C7 0.056(10) 0.067(8) 0.040(9) 0.004(6) 0.000(8) 0.017(7)
C8 0.115(13) 0.066(7) 0.021(7) 0.013(6) -0.010(8) -0.022(8)
C9 0.089(6) 0.106(6) 0.080(6) 0.006(5) -0.002(5) 0.006(5)
C10 0.083(6) 0.086(5) 0.080(6) -0.018(4) -0.002(5) -0.005(5)
C11 0.035(8) 0.065(7) 0.026(7) 0.011(5) -0.007(7) -0.003(7)
C12 0.114(6) 0.113(6) 0.114(6) 0.0010(10) 0.0008(10) 0.0003(10)
C13 0.136(6) 0.137(6) 0.136(6) 0.0010(10) 0.0005(10) 0.0004(10)
C14 0.102(7) 0.113(6) 0.108(7) -0.013(5) 0.005(5) 0.002(5)
C15 0.117(6) 0.117(6) 0.118(6) -0.0001(10) -0.0001(10) 0.0004(10)
C16 0.095(6) 0.051(5) 0.072(6) 0.010(4) -0.006(5) 0.002(4)
C17 0.054(9) 0.043(7) 0.052(9) -0.016(6) -0.008(7) -0.013(6)
C18 0.068(10) 0.035(7) 0.035(8) -0.012(6) -0.017(7) 0.004(7)
C19 0.065(9) 0.039(6) 0.027(7) -0.005(5) -0.012(6) 0.005(6)
C20 0.038(8) 0.044(7) 0.054(9) -0.005(6) -0.010(7) 0.011(6)
C21 0.045(9) 0.081(9) 0.074(11) -0.006(7) -0.024(8) 0.020(7)
C22 0.060(5) 0.077(5) 0.074(6) -0.002(4) 0.000(4) 0.006(4)
C23 0.086(6) 0.096(6) 0.098(6) 0.002(5) 0.002(5) 0.004(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C5 2.121(11) . ?
Fe1 C2 2.135(10) . ?
Fe1 C4 2.147(11) . ?
Fe1 C1 2.150(10) . ?
Fe1 C3 2.165(10) . ?
Fe1 P2 2.204(3) . ?
Fe1 P3 2.213(3) . ?
Fe1 P1 2.214(3) . ?
P1 C20 1.828(10) . ?
P1 C11 1.836(9) . ?
P1 C19 1.853(9) . ?
P2 C14 1.788(11) . ?
P2 C13 1.836(15) . ?
P2 C22 1.849(12) . ?
P3 C17 1.860(10) . ?
P3 C16 1.928(11) . ?
P3 C24 1.963(19) . ?
C1 C5 1.398(14) . ?
C1 C2 1.441(13) . ?
C1 C6 1.512(11) . ?
C2 C3 1.424(12) . ?
C2 C7 1.474(13) . ?
C3 C4 1.407(14) . ?
C3 C8 1.490(12) . ?
C4 C5 1.396(14) . ?
C4 C9 1.487(14) . ?
C5 C10 1.483(14) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.413(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.322(16) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.488(14) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.484(16) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.492(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.536(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.517(14) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.33(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
B1 F4B 1.22(4) . ?
B1 F3B 1.28(3) . ?
B1 F2A 1.34(2) . ?
B1 F1 1.3502(10) . ?
B1 F3A 1.3506(10) . ?
B1 F2B 1.3507(10) . ?
B1 F4A 1.37(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
C5 Fe1 C2 65.6(4) . . ?
C5 Fe1 C4 38.2(4) . . ?
C2 Fe1 C4 64.9(4) . . ?
C5 Fe1 C1 38.2(4) . . ?
C2 Fe1 C1 39.3(4) . . ?
C4 Fe1 C1 63.6(4) . . ?
C5 Fe1 C3 64.2(4) . . ?
C2 Fe1 C3 38.7(3) . . ?
C4 Fe1 C3 38.1(4) . . ?
C1 Fe1 C3 63.9(4) . . ?
C5 Fe1 P2 92.6(3) . . ?
C2 Fe1 P2 158.2(3) . . ?
C4 Fe1 P2 98.3(3) . . ?
C1 Fe1 P2 121.9(3) . . ?
C3 Fe1 P2 132.8(3) . . ?
C5 Fe1 P3 150.1(4) . . ?
C2 Fe1 P3 109.1(3) . . ?
C4 Fe1 P3 112.1(4) . . ?
C1 Fe1 P3 148.2(3) . . ?
C3 Fe1 P3 92.9(3) . . ?
P2 Fe1 P3 89.67(12) . . ?
C5 Fe1 P1 118.0(4) . . ?
C2 Fe1 P1 100.2(3) . . ?
C4 Fe1 P1 154.7(4) . . ?
C1 Fe1 P1 91.7(3) . . ?
C3 Fe1 P1 137.2(3) . . ?
P2 Fe1 P1 89.78(12) . . ?
P3 Fe1 P1 91.78(11) . . ?
C20 P1 C11 102.7(5) . . ?
C20 P1 C19 99.8(5) . . ?
C11 P1 C19 98.8(5) . . ?
C20 P1 Fe1 116.9(4) . . ?
C11 P1 Fe1 116.1(4) . . ?
C19 P1 Fe1 119.4(3) . . ?
C14 P2 C13 96.6(7) . . ?
C14 P2 C22 100.1(6) . . ?
C13 P2 C22 101.7(7) . . ?
C14 P2 Fe1 120.1(5) . . ?
C13 P2 Fe1 115.4(5) . . ?
C22 P2 Fe1 119.1(4) . . ?
C17 P3 C16 99.9(5) . . ?
C17 P3 C24 95.8(7) . . ?
C16 P3 C24 89.2(7) . . ?
C17 P3 Fe1 123.0(3) . . ?
C16 P3 Fe1 108.9(4) . . ?
C24 P3 Fe1 131.5(6) . . ?
C5 C1 C2 108.5(9) . . ?
C5 C1 C6 125.9(12) . . ?
C2 C1 C6 124.6(11) . . ?
C5 C1 Fe1 69.8(6) . . ?
C2 C1 Fe1 69.8(6) . . ?
C6 C1 Fe1 135.0(7) . . ?
C3 C2 C1 105.8(10) . . ?
C3 C2 C7 125.8(10) . . ?
C1 C2 C7 126.0(10) . . ?
C3 C2 Fe1 71.8(6) . . ?
C1 C2 Fe1 70.9(6) . . ?
C7 C2 Fe1 135.2(8) . . ?
C4 C3 C2 108.5(10) . . ?
C4 C3 C8 125.3(11) . . ?
C2 C3 C8 124.3(10) . . ?
C4 C3 Fe1 70.3(6) . . ?
C2 C3 Fe1 69.5(6) . . ?
C8 C3 Fe1 138.4(7) . . ?
C5 C4 C3 108.6(11) . . ?
C5 C4 C9 129.1(13) . . ?
C3 C4 C9 121.1(12) . . ?
C5 C4 Fe1 69.9(7) . . ?
C3 C4 Fe1 71.6(7) . . ?
C9 C4 Fe1 134.1(8) . . ?
C4 C5 C1 108.3(11) . . ?
C4 C5 C10 127.6(13) . . ?
C1 C5 C10 121.2(12) . . ?
C4 C5 Fe1 71.9(7) . . ?
C1 C5 Fe1 72.0(7) . . ?
C10 C5 Fe1 136.8(9) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 113.2(8) . . ?
C12 C11 H11A 108.9 . . ?
P1 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
P1 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 C11 138.1(15) . . ?
C13 C12 H12A 102.6 . . ?
C11 C12 H12A 102.6 . . ?
C13 C12 H12B 102.6 . . ?
C11 C12 H12B 102.6 . . ?
H12A C12 H12B 104.9 . . ?
C12 C13 P2 122.6(14) . . ?
C12 C13 H13A 106.7 . . ?
P2 C13 H13A 106.7 . . ?
C12 C13 H13B 106.7 . . ?
P2 C13 H13B 106.7 . . ?
H13A C13 H13B 106.6 . . ?
C15 C14 P2 110.5(10) . . ?
C15 C14 H14A 109.5 . . ?
P2 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
P2 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C14 126.4(12) . . ?
C16 C15 H15A 105.7 . . ?
C14 C15 H15A 105.7 . . ?
C16 C15 H15B 105.7 . . ?
C14 C15 H15B 105.7 . . ?
H15A C15 H15B 106.2 . . ?
C15 C16 P3 111.5(9) . . ?
C15 C16 H16A 109.3 . . ?
P3 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
P3 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 P3 115.2(7) . . ?
C18 C17 H17A 108.5 . . ?
P3 C17 H17A 108.5 . . ?
C18 C17 H17B 108.5 . . ?
P3 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.0(9) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 P1 113.9(7) . . ?
C18 C19 H19A 108.8 . . ?
P1 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
P1 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 P1 117.8(8) . . ?
C21 C20 H20A 107.9 . . ?
P1 C20 H20A 107.9 . . ?
C21 C20 H20B 107.9 . . ?
P1 C20 H20B 107.9 . . ?
H20A C20 H20B 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 P2 117.7(10) . . ?
C23 C22 H22A 107.9 . . ?
P2 C22 H22A 107.9 . . ?
C23 C22 H22B 107.9 . . ?
P2 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 P3 96.3(14) . . ?
C25 C24 H24A 112.5 . . ?
P3 C24 H24A 112.5 . . ?
C25 C24 H24B 112.5 . . ?
P3 C24 H24B 112.5 . . ?
H24A C24 H24B 110.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
F4B B1 F3B 114.6(19) . . ?
F4B B1 F2A 39.6(18) . . ?
F3B B1 F2A 141.9(12) . . ?
F4B B1 F1 124(2) . . ?
F3B B1 F1 109.8(17) . . ?
F2A B1 F1 108.3(15) . . ?
F4B B1 F3A 65.1(17) . . ?
F3B B1 F3A 71.0(13) . . ?
F2A B1 F3A 103.4(18) . . ?
F1 B1 F3A 101.2(11) . . ?
F4B B1 F2B 101(2) . . ?
F3B B1 F2B 108(2) . . ?
F2A B1 F2B 66.1(13) . . ?
F1 B1 F2B 96.0(10) . . ?
F3A B1 F2B 162.1(13) . . ?
F4B B1 F4A 121.7(16) . . ?
F3B B1 F4A 50.4(13) . . ?
F2A B1 F4A 111.7(13) . . ?
F1 B1 F4A 112.4(16) . . ?
F3A B1 F4A 118.9(17) . . ?
F2B B1 F4A 57.3(12) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 Fe1 P1 C20 -79.2(5) . . . . ?
C2 Fe1 P1 C20 -11.5(5) . . . . ?
C4 Fe1 P1 C20 -62.7(9) . . . . ?
C1 Fe1 P1 C20 -50.2(5) . . . . ?
C3 Fe1 P1 C20 2.0(6) . . . . ?
P2 Fe1 P1 C20 -172.1(4) . . . . ?
P3 Fe1 P1 C20 98.3(4) . . . . ?
C5 Fe1 P1 C11 42.4(5) . . . . ?
C2 Fe1 P1 C11 110.0(5) . . . . ?
C4 Fe1 P1 C11 58.8(9) . . . . ?
C1 Fe1 P1 C11 71.4(5) . . . . ?
C3 Fe1 P1 C11 123.6(5) . . . . ?
P2 Fe1 P1 C11 -50.5(4) . . . . ?
P3 Fe1 P1 C11 -140.2(4) . . . . ?
C5 Fe1 P1 C19 160.5(6) . . . . ?
C2 Fe1 P1 C19 -131.8(5) . . . . ?
C4 Fe1 P1 C19 177.0(9) . . . . ?
C1 Fe1 P1 C19 -170.5(5) . . . . ?
C3 Fe1 P1 C19 -118.3(6) . . . . ?
P2 Fe1 P1 C19 67.6(4) . . . . ?
P3 Fe1 P1 C19 -22.0(4) . . . . ?
C5 Fe1 P2 C14 160.6(7) . . . . ?
C2 Fe1 P2 C14 160.6(10) . . . . ?
C4 Fe1 P2 C14 122.7(7) . . . . ?
C1 Fe1 P2 C14 -173.3(6) . . . . ?
C3 Fe1 P2 C14 104.1(7) . . . . ?
P3 Fe1 P2 C14 10.4(6) . . . . ?
P1 Fe1 P2 C14 -81.4(6) . . . . ?
C5 Fe1 P2 C13 -84.4(7) . . . . ?
C2 Fe1 P2 C13 -84.4(10) . . . . ?
C4 Fe1 P2 C13 -122.4(7) . . . . ?
C1 Fe1 P2 C13 -58.3(7) . . . . ?
C3 Fe1 P2 C13 -140.9(7) . . . . ?
P3 Fe1 P2 C13 125.4(6) . . . . ?
P1 Fe1 P2 C13 33.6(6) . . . . ?
C5 Fe1 P2 C22 36.9(6) . . . . ?
C2 Fe1 P2 C22 36.9(10) . . . . ?
C4 Fe1 P2 C22 -1.0(6) . . . . ?
C1 Fe1 P2 C22 63.0(5) . . . . ?
C3 Fe1 P2 C22 -19.6(6) . . . . ?
P3 Fe1 P2 C22 -113.3(4) . . . . ?
P1 Fe1 P2 C22 154.9(4) . . . . ?
C5 Fe1 P3 C17 -168.0(8) . . . . ?
C2 Fe1 P3 C17 117.9(6) . . . . ?
C4 Fe1 P3 C17 -172.2(6) . . . . ?
C1 Fe1 P3 C17 112.7(7) . . . . ?
C3 Fe1 P3 C17 153.9(5) . . . . ?
P2 Fe1 P3 C17 -73.3(5) . . . . ?
P1 Fe1 P3 C17 16.5(5) . . . . ?
C5 Fe1 P3 C16 -52.1(8) . . . . ?
C2 Fe1 P3 C16 -126.1(5) . . . . ?
C4 Fe1 P3 C16 -56.2(5) . . . . ?
C1 Fe1 P3 C16 -131.4(7) . . . . ?
C3 Fe1 P3 C16 -90.1(5) . . . . ?
P2 Fe1 P3 C16 42.7(4) . . . . ?
P1 Fe1 P3 C16 132.4(4) . . . . ?
C5 Fe1 P3 C24 54.4(12) . . . . ?
C2 Fe1 P3 C24 -19.6(10) . . . . ?
C4 Fe1 P3 C24 50.3(10) . . . . ?
C1 Fe1 P3 C24 -24.9(11) . . . . ?
C3 Fe1 P3 C24 16.4(9) . . . . ?
P2 Fe1 P3 C24 149.2(9) . . . . ?
P1 Fe1 P3 C24 -121.1(9) . . . . ?
C2 Fe1 C1 C5 119.8(9) . . . . ?
C4 Fe1 C1 C5 37.9(7) . . . . ?
C3 Fe1 C1 C5 80.6(7) . . . . ?
P2 Fe1 C1 C5 -45.3(8) . . . . ?
P3 Fe1 C1 C5 127.7(8) . . . . ?
P1 Fe1 C1 C5 -136.1(7) . . . . ?
C5 Fe1 C1 C2 -119.8(9) . . . . ?
C4 Fe1 C1 C2 -81.9(7) . . . . ?
C3 Fe1 C1 C2 -39.2(6) . . . . ?
P2 Fe1 C1 C2 -165.1(5) . . . . ?
P3 Fe1 C1 C2 7.9(10) . . . . ?
P1 Fe1 C1 C2 104.1(6) . . . . ?
C5 Fe1 C1 C6 121.1(16) . . . . ?
C2 Fe1 C1 C6 -119.1(15) . . . . ?
C4 Fe1 C1 C6 159.0(14) . . . . ?
C3 Fe1 C1 C6 -158.3(14) . . . . ?
P2 Fe1 C1 C6 75.8(13) . . . . ?
P3 Fe1 C1 C6 -111.2(11) . . . . ?
P1 Fe1 C1 C6 -15.0(12) . . . . ?
C5 C1 C2 C3 4.6(11) . . . . ?
C6 C1 C2 C3 -164.8(9) . . . . ?
Fe1 C1 C2 C3 63.8(7) . . . . ?
C5 C1 C2 C7 168.2(10) . . . . ?
C6 C1 C2 C7 -1.3(17) . . . . ?
Fe1 C1 C2 C7 -132.6(11) . . . . ?
C5 C1 C2 Fe1 -59.2(7) . . . . ?
C6 C1 C2 Fe1 131.4(10) . . . . ?
C5 Fe1 C2 C3 -78.5(7) . . . . ?
C4 Fe1 C2 C3 -36.3(6) . . . . ?
C1 Fe1 C2 C3 -114.7(9) . . . . ?
P2 Fe1 C2 C3 -78.5(11) . . . . ?
P3 Fe1 C2 C3 69.7(7) . . . . ?
P1 Fe1 C2 C3 165.3(6) . . . . ?
C5 Fe1 C2 C1 36.1(6) . . . . ?
C4 Fe1 C2 C1 78.3(7) . . . . ?
C3 Fe1 C2 C1 114.7(9) . . . . ?
P2 Fe1 C2 C1 36.1(12) . . . . ?
P3 Fe1 C2 C1 -175.6(6) . . . . ?
P1 Fe1 C2 C1 -80.1(6) . . . . ?
C5 Fe1 C2 C7 158.5(13) . . . . ?
C4 Fe1 C2 C7 -159.3(13) . . . . ?
C1 Fe1 C2 C7 122.4(14) . . . . ?
C3 Fe1 C2 C7 -123.0(14) . . . . ?
P2 Fe1 C2 C7 158.5(7) . . . . ?
P3 Fe1 C2 C7 -53.2(11) . . . . ?
P1 Fe1 C2 C7 42.3(11) . . . . ?
C1 C2 C3 C4 -3.5(11) . . . . ?
C7 C2 C3 C4 -167.1(10) . . . . ?
Fe1 C2 C3 C4 59.7(8) . . . . ?
C1 C2 C3 C8 161.4(9) . . . . ?
C7 C2 C3 C8 -2.1(16) . . . . ?
Fe1 C2 C3 C8 -135.3(9) . . . . ?
C1 C2 C3 Fe1 -63.2(7) . . . . ?
C7 C2 C3 Fe1 133.2(11) . . . . ?
C5 Fe1 C3 C4 -37.0(6) . . . . ?
C2 Fe1 C3 C4 -119.6(10) . . . . ?
C1 Fe1 C3 C4 -79.7(7) . . . . ?
P2 Fe1 C3 C4 30.7(8) . . . . ?
P3 Fe1 C3 C4 123.0(7) . . . . ?
P1 Fe1 C3 C4 -141.2(6) . . . . ?
C5 Fe1 C3 C2 82.5(7) . . . . ?
C4 Fe1 C3 C2 119.6(10) . . . . ?
C1 Fe1 C3 C2 39.8(6) . . . . ?
P2 Fe1 C3 C2 150.3(6) . . . . ?
P3 Fe1 C3 C2 -117.4(6) . . . . ?
P1 Fe1 C3 C2 -21.6(8) . . . . ?
C5 Fe1 C3 C8 -158.5(14) . . . . ?
C2 Fe1 C3 C8 119.0(15) . . . . ?
C4 Fe1 C3 C8 -121.5(16) . . . . ?
C1 Fe1 C3 C8 158.8(14) . . . . ?
P2 Fe1 C3 C8 -90.7(13) . . . . ?
P3 Fe1 C3 C8 1.5(12) . . . . ?
P1 Fe1 C3 C8 97.3(12) . . . . ?
C2 C3 C4 C5 1.2(13) . . . . ?
C8 C3 C4 C5 -163.6(9) . . . . ?
Fe1 C3 C4 C5 60.4(8) . . . . ?
C2 C3 C4 C9 169.8(10) . . . . ?
C8 C3 C4 C9 5.0(17) . . . . ?
Fe1 C3 C4 C9 -131.0(11) . . . . ?
C2 C3 C4 Fe1 -59.2(7) . . . . ?
C8 C3 C4 Fe1 136.0(10) . . . . ?
C2 Fe1 C4 C5 -81.8(7) . . . . ?
C1 Fe1 C4 C5 -38.0(7) . . . . ?
C3 Fe1 C4 C5 -118.7(10) . . . . ?
P2 Fe1 C4 C5 83.6(7) . . . . ?
P3 Fe1 C4 C5 176.7(6) . . . . ?
P1 Fe1 C4 C5 -23.9(13) . . . . ?
C5 Fe1 C4 C3 118.7(10) . . . . ?
C2 Fe1 C4 C3 36.9(6) . . . . ?
C1 Fe1 C4 C3 80.7(7) . . . . ?
P2 Fe1 C4 C3 -157.7(6) . . . . ?
P3 Fe1 C4 C3 -64.7(7) . . . . ?
P1 Fe1 C4 C3 94.8(10) . . . . ?
C5 Fe1 C4 C9 -125.5(17) . . . . ?
C2 Fe1 C4 C9 152.7(15) . . . . ?
C1 Fe1 C4 C9 -163.5(15) . . . . ?
C3 Fe1 C4 C9 115.8(16) . . . . ?
P2 Fe1 C4 C9 -41.9(13) . . . . ?
P3 Fe1 C4 C9 51.2(14) . . . . ?
P1 Fe1 C4 C9 -149.4(9) . . . . ?
C3 C4 C5 C1 1.8(13) . . . . ?
C9 C4 C5 C1 -165.7(11) . . . . ?
Fe1 C4 C5 C1 63.3(8) . . . . ?
C3 C4 C5 C10 162.7(11) . . . . ?
C9 C4 C5 C10 -5(2) . . . . ?
Fe1 C4 C5 C10 -135.8(12) . . . . ?
C3 C4 C5 Fe1 -61.5(8) . . . . ?
C9 C4 C5 Fe1 131.1(12) . . . . ?
C2 C1 C5 C4 -4.0(12) . . . . ?
C6 C1 C5 C4 165.2(9) . . . . ?
Fe1 C1 C5 C4 -63.2(8) . . . . ?
C2 C1 C5 C10 -166.4(11) . . . . ?
C6 C1 C5 C10 2.9(17) . . . . ?
Fe1 C1 C5 C10 134.4(12) . . . . ?
C2 C1 C5 Fe1 59.2(7) . . . . ?
C6 C1 C5 Fe1 -131.6(10) . . . . ?
C2 Fe1 C5 C4 79.8(7) . . . . ?
C1 Fe1 C5 C4 117.0(10) . . . . ?
C3 Fe1 C5 C4 37.0(7) . . . . ?
P2 Fe1 C5 C4 -100.2(7) . . . . ?
P3 Fe1 C5 C4 -6.2(12) . . . . ?
P1 Fe1 C5 C4 168.7(6) . . . . ?
C2 Fe1 C5 C1 -37.1(6) . . . . ?
C4 Fe1 C5 C1 -117.0(10) . . . . ?
C3 Fe1 C5 C1 -80.0(7) . . . . ?
P2 Fe1 C5 C1 142.9(7) . . . . ?
P3 Fe1 C5 C1 -123.2(8) . . . . ?
P1 Fe1 C5 C1 51.7(8) . . . . ?
C2 Fe1 C5 C10 -153.9(16) . . . . ?
C4 Fe1 C5 C10 126.3(18) . . . . ?
C1 Fe1 C5 C10 -116.8(18) . . . . ?
C3 Fe1 C5 C10 163.2(16) . . . . ?
P2 Fe1 C5 C10 26.1(15) . . . . ?
P3 Fe1 C5 C10 120.0(13) . . . . ?
P1 Fe1 C5 C10 -65.1(15) . . . . ?
C20 P1 C11 C12 168.1(10) . . . . ?
C19 P1 C11 C12 -89.7(10) . . . . ?
Fe1 P1 C11 C12 39.3(10) . . . . ?
P1 C11 C12 C13 9(3) . . . . ?
C11 C12 C13 P2 -29(3) . . . . ?
C14 P2 C13 C12 124.2(16) . . . . ?
C22 P2 C13 C12 -134.0(15) . . . . ?
Fe1 P2 C13 C12 -3.7(17) . . . . ?
C13 P2 C14 C15 177.3(12) . . . . ?
C22 P2 C14 C15 74.2(12) . . . . ?
Fe1 P2 C14 C15 -58.2(13) . . . . ?
P2 C14 C15 C16 42(2) . . . . ?
C14 C15 C16 P3 21(2) . . . . ?
C17 P3 C16 C15 60.4(11) . . . . ?
C24 P3 C16 C15 156.2(11) . . . . ?
Fe1 P3 C16 C15 -69.6(10) . . . . ?
C16 P3 C17 C18 -160.2(8) . . . . ?
C24 P3 C17 C18 109.5(10) . . . . ?
Fe1 P3 C17 C18 -39.9(10) . . . . ?
P3 C17 C18 C19 68.1(10) . . . . ?
C17 C18 C19 P1 -76.2(9) . . . . ?
C20 P1 C19 C18 -75.0(8) . . . . ?
C11 P1 C19 C18 -179.7(8) . . . . ?
Fe1 P1 C19 C18 53.6(8) . . . . ?
C11 P1 C20 C21 45.9(9) . . . . ?
C19 P1 C20 C21 -55.5(8) . . . . ?
Fe1 P1 C20 C21 174.2(6) . . . . ?
C14 P2 C22 C23 49.1(10) . . . . ?
C13 P2 C22 C23 -49.9(10) . . . . ?
Fe1 P2 C22 C23 -177.9(7) . . . . ?
C17 P3 C24 C25 -81.3(14) . . . . ?
C16 P3 C24 C25 178.8(14) . . . . ?
Fe1 P3 C24 C25 64.0(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.872
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.872
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.090

data_s92_4
_database_code_depnum_ccdc_archive 'CCDC 277606'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H38 Fe P3, B F4, C4 H10 O'
_chemical_formula_sum            'C24 H48 B F4 Fe O P3'
_chemical_formula_weight         588.19

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.075(1)
_cell_length_b                   19.277(2)
_cell_length_c                   17.852(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.19(1)
_cell_angle_gamma                90.00
_cell_volume                     2776.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      25.03

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.7770
_exptl_absorpt_correction_T_max  0.8630
_exptl_absorpt_process_details   'Walker & Stuart, 1983'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius FAST area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9165
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.04
_reflns_number_total             3964
_reflns_number_gt                2403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MADNES (Enraf Nonius, 1989)'
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;

Most F atoms and disordered C01 and C01'
were restrained using ISOR due to high MSDAs.

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^)+(0.0180P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3781
_refine_ls_number_parameters     357
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1155
_refine_ls_wR_factor_gt          0.1105
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.003
_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 0.36763(8) 0.35224(4) 0.69541(4) 0.0193(2) Uani 1 1 d . . .
P1 P 0.23901(16) 0.26659(8) 0.74870(8) 0.0226(4) Uani 1 1 d . . .
P2 P 0.18811(15) 0.34840(8) 0.59881(7) 0.0206(4) Uani 1 1 d . . .
P3 P 0.23169(16) 0.42949(8) 0.75801(8) 0.0218(4) Uani 1 1 d . . .
C1 C 0.5727(6) 0.4155(3) 0.6743(3) 0.0321(16) Uani 1 1 d . . .
H1 H 0.5656 0.4621 0.6612 0.039 Uiso 1 1 calc R . .
C2 C 0.5879(6) 0.3879(4) 0.7483(3) 0.0319(16) Uani 1 1 d . . .
H2 H 0.5941 0.4136 0.7924 0.038 Uiso 1 1 calc R . .
C3 C 0.5919(6) 0.3171(4) 0.7435(4) 0.0334(16) Uani 1 1 d . . .
H3 H 0.6004 0.2868 0.7840 0.040 Uiso 1 1 calc R . .
C4 C 0.5811(6) 0.2973(3) 0.6667(4) 0.0346(17) Uani 1 1 d . . .
H4 H 0.5812 0.2523 0.6479 0.041 Uiso 1 1 calc R . .
C5 C 0.5703(6) 0.3587(4) 0.6247(3) 0.0334(16) Uani 1 1 d . . .
H5 H 0.5628 0.3614 0.5727 0.040 Uiso 1 1 calc R . .
C6 C 0.0240(6) 0.2500(3) 0.7153(3) 0.0255(15) Uani 1 1 d . . .
H6A H -0.0233 0.2149 0.7469 0.031 Uiso 1 1 calc R . .
H6B H -0.0398 0.2922 0.7209 0.031 Uiso 1 1 calc R . .
C7 C 0.0061(6) 0.2264(3) 0.6345(3) 0.0296(15) Uani 1 1 d . . .
H7A H -0.1079 0.2343 0.6175 0.036 Uiso 1 1 calc R . .
H7B H 0.0246 0.1767 0.6335 0.036 Uiso 1 1 calc R . .
C8 C 0.1190(6) 0.2598(3) 0.5770(3) 0.0260(15) Uani 1 1 d . . .
H8A H 0.0603 0.2602 0.5286 0.031 Uiso 1 1 calc R . .
H8B H 0.2162 0.2307 0.5725 0.031 Uiso 1 1 calc R . .
C9 C -0.0100(6) 0.3960(3) 0.6011(3) 0.0246(14) Uani 1 1 d . . .
H9A H -0.0455 0.4070 0.5499 0.030 Uiso 1 1 calc R . .
H9B H -0.0925 0.3653 0.6212 0.030 Uiso 1 1 calc R . .
C10 C -0.0084(6) 0.4621(3) 0.6458(3) 0.0278(15) Uani 1 1 d . . .
H10A H -0.1126 0.4862 0.6367 0.033 Uiso 1 1 calc R . .
H10B H 0.0798 0.4918 0.6291 0.033 Uiso 1 1 calc R . .
C11 C 0.0167(6) 0.4491(3) 0.7293(3) 0.0237(14) Uani 1 1 d . . .
H11A H -0.0531 0.4107 0.7435 0.028 Uiso 1 1 calc R . .
H11B H -0.0187 0.4899 0.7563 0.028 Uiso 1 1 calc R . .
C12 C 0.2144(6) 0.4088(3) 0.8579(3) 0.0315(15) Uani 1 1 d . . .
H12A H 0.3249 0.4077 0.8811 0.038 Uiso 1 1 calc R . .
H12B H 0.1541 0.4460 0.8814 0.038 Uiso 1 1 calc R . .
C13 C 0.1290(7) 0.3408(3) 0.8743(3) 0.0352(16) Uani 1 1 d . . .
H13A H 0.0199 0.3413 0.8496 0.042 Uiso 1 1 calc R . .
H13B H 0.1136 0.3379 0.9278 0.042 Uiso 1 1 calc R . .
C14 C 0.2202(7) 0.2756(3) 0.8496(3) 0.0344(16) Uani 1 1 d . . .
H14A H 0.1624 0.2353 0.8680 0.041 Uiso 1 1 calc R . .
H14B H 0.3305 0.2757 0.8731 0.041 Uiso 1 1 calc R . .
C15 C 0.3329(6) 0.1810(3) 0.7400(3) 0.0271(15) Uani 1 1 d . . .
H15A H 0.3340 0.1694 0.6871 0.033 Uiso 1 1 calc R . .
H15B H 0.4474 0.1841 0.7582 0.033 Uiso 1 1 calc R . .
C16 C 0.2517(7) 0.1208(3) 0.7807(3) 0.0409(17) Uani 1 1 d . . .
H16A H 0.2968 0.0777 0.7639 0.061 Uiso 1 1 calc R . .
H16B H 0.1343 0.1215 0.7700 0.061 Uiso 1 1 calc R . .
H16C H 0.2730 0.1255 0.8338 0.061 Uiso 1 1 calc R . .
C17 C 0.2564(7) 0.3736(3) 0.5054(3) 0.0339(17) Uani 1 1 d . . .
H17A H 0.3498 0.3448 0.4929 0.041 Uiso 1 1 calc R . .
H17B H 0.1672 0.3643 0.4688 0.041 Uiso 1 1 calc R . .
C18 C 0.3061(7) 0.4487(3) 0.4993(3) 0.0418(17) Uani 1 1 d . . .
H18A H 0.3536 0.4566 0.4515 0.063 Uiso 1 1 calc R . .
H18B H 0.3862 0.4597 0.5386 0.063 Uiso 1 1 calc R . .
H18C H 0.2102 0.4776 0.5038 0.063 Uiso 1 1 calc R . .
C19 C 0.3240(6) 0.5159(3) 0.7610(3) 0.0312(15) Uani 1 1 d . . .
H19A H 0.4391 0.5108 0.7776 0.037 Uiso 1 1 calc R . .
H19B H 0.3231 0.5334 0.7101 0.037 Uiso 1 1 calc R . .
C20 C 0.2464(7) 0.5715(4) 0.8101(4) 0.058(2) Uani 1 1 d . . .
H20A H 0.3060 0.6143 0.8055 0.087 Uiso 1 1 calc R . .
H20B H 0.2518 0.5567 0.8615 0.087 Uiso 1 1 calc R . .
H20C H 0.1327 0.5783 0.7942 0.087 Uiso 1 1 calc R . .
B1 B 0.2482(11) 0.6649(6) 0.5915(5) 0.052(3) Uani 1 1 d . . .
F1A F 0.2234(13) 0.6943(5) 0.5249(5) 0.092(4) Uani 0.576(11) 1 d P A 5
F2A F 0.4082(12) 0.6953(6) 0.5954(7) 0.119(5) Uani 0.576(11) 1 d PU A 5
F3A F 0.2297(16) 0.6709(7) 0.6690(7) 0.139(5) Uani 0.576(11) 1 d PU A 5
F1B F 0.344(2) 0.6908(9) 0.6424(11) 0.120(6) Uani 0.424(11) 1 d PU A 6
F2B F 0.1399(16) 0.7089(8) 0.5787(9) 0.103(5) Uani 0.424(11) 1 d PU A 6
F3B F 0.359(2) 0.6073(9) 0.5846(9) 0.113(6) Uani 0.424(11) 1 d PU A 6
F4A F 0.1113(13) 0.6311(6) 0.6139(7) 0.126(6) Uani 0.553(13) 1 d PU A 1
F4B F 0.2696(17) 0.6013(7) 0.5683(7) 0.084(5) Uani 0.447(13) 1 d PU A 2
O1 O 0.659(2) 0.4366(12) 0.9666(8) 0.093(8) Uani 0.50 1 d P B 3
C01 C 0.7858(13) 0.4698(7) 0.9425(6) 0.117(4) Uani 0.50 1 d PU B 3
H01A H 0.8249 0.4456 0.8989 0.141 Uiso 0.50 1 calc PR B 3
H01B H 0.8738 0.4680 0.9810 0.141 Uiso 0.50 1 calc PR B 3
C03 C 0.6994(10) 0.3571(5) 0.9653(5) 0.082(3) Uani 0.50 1 d P B 3
H03A H 0.6992 0.3387 0.9148 0.098 Uiso 0.50 1 calc PR B 3
H03B H 0.8041 0.3465 0.9913 0.098 Uiso 0.50 1 calc PR B 3
O1' O 0.682(2) 0.4238(8) 0.9278(10) 0.094(6) Uani 0.50 1 d P B 4
C01' C 0.7858(13) 0.4698(7) 0.9425(6) 0.117(4) Uani 0.50 1 d PU B 4
H01C H 0.8875 0.4559 0.9195 0.141 Uiso 0.50 1 calc PR B 4
H01D H 0.8078 0.4686 0.9963 0.141 Uiso 0.50 1 calc PR B 4
C03' C 0.6994(10) 0.3571(5) 0.9653(5) 0.082(3) Uani 0.50 1 d P B 4
H03C H 0.7945 0.3596 1.0001 0.098 Uiso 0.50 1 calc PR B 4
H03D H 0.7239 0.3224 0.9280 0.098 Uiso 0.50 1 calc PR B 4
C02 C 0.7578(10) 0.5411(4) 0.9226(4) 0.094(3) Uani 1 1 d . . .
H02A H 0.8613 0.5626 0.9115 0.141 Uiso 1 1 calc R B 3
H02B H 0.7094 0.5649 0.9636 0.141 Uiso 1 1 calc R B 3
H02C H 0.6839 0.5436 0.8792 0.141 Uiso 1 1 calc R B 3
C04 C 0.5541(10) 0.3324(5) 1.0075(4) 0.095(3) Uani 1 1 d . . .
H04A H 0.5611 0.2831 1.0141 0.142 Uiso 1 1 calc R B 3
H04B H 0.4535 0.3437 0.9798 0.142 Uiso 1 1 calc R B 3
H04C H 0.5544 0.3546 1.0557 0.142 Uiso 1 1 calc R B 3

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 0.0105(4) 0.0231(5) 0.0243(5) 0.0017(4) 0.0020(3) -0.0004(4)
P1 0.0195(8) 0.0224(11) 0.0260(10) 0.0041(7) 0.0030(6) 0.0006(7)
P2 0.0162(7) 0.0234(10) 0.0222(8) 0.0010(7) 0.0015(6) 0.0000(7)
P3 0.0179(8) 0.0233(11) 0.0241(9) -0.0001(7) 0.0000(6) -0.0007(7)
C1 0.013(3) 0.036(5) 0.047(4) -0.002(4) 0.001(3) -0.006(3)
C2 0.015(3) 0.041(5) 0.039(5) -0.001(3) -0.007(3) -0.007(3)
C3 0.010(3) 0.040(5) 0.050(5) 0.011(3) -0.007(3) 0.007(3)
C4 0.009(3) 0.040(5) 0.055(5) -0.002(4) 0.002(3) 0.008(3)
C5 0.009(3) 0.049(5) 0.043(4) 0.008(4) 0.008(3) -0.001(3)
C6 0.015(3) 0.021(4) 0.041(4) 0.006(3) 0.005(3) -0.003(2)
C7 0.020(3) 0.015(4) 0.054(4) -0.006(3) 0.001(3) -0.004(2)
C8 0.023(3) 0.030(4) 0.025(4) -0.009(3) 0.000(2) 0.004(3)
C9 0.025(3) 0.020(4) 0.029(4) -0.001(3) -0.002(2) 0.005(3)
C10 0.020(3) 0.029(4) 0.034(4) 0.001(3) -0.002(3) 0.006(3)
C11 0.021(3) 0.011(4) 0.040(4) -0.006(3) 0.003(3) 0.004(2)
C12 0.032(4) 0.036(5) 0.027(4) 0.002(3) 0.000(3) 0.003(3)
C13 0.043(4) 0.045(5) 0.018(3) 0.002(3) 0.007(3) -0.005(3)
C14 0.042(4) 0.031(5) 0.031(4) 0.008(3) 0.010(3) 0.002(3)
C15 0.025(3) 0.021(4) 0.036(4) 0.003(3) 0.000(3) 0.004(3)
C16 0.047(4) 0.027(5) 0.049(5) 0.009(3) 0.005(3) 0.003(3)
C17 0.027(3) 0.048(5) 0.027(4) -0.001(3) 0.003(3) -0.002(3)
C18 0.049(4) 0.042(5) 0.035(4) 0.009(3) 0.002(3) -0.009(3)
C19 0.031(3) 0.021(4) 0.041(4) -0.004(3) -0.001(3) -0.006(3)
C20 0.053(5) 0.040(6) 0.083(6) -0.018(4) 0.016(4) -0.010(4)
B1 0.041(5) 0.070(9) 0.046(6) -0.033(5) 0.015(4) -0.017(5)
F1A 0.140(9) 0.091(8) 0.040(6) 0.013(5) -0.049(5) -0.023(6)
F2A 0.099(6) 0.131(6) 0.130(6) -0.009(4) 0.018(4) -0.013(4)
F3A 0.144(6) 0.154(7) 0.120(6) -0.031(4) 0.042(5) 0.008(5)
F1B 0.125(7) 0.122(7) 0.111(7) -0.012(5) -0.021(5) -0.023(5)
F2B 0.089(6) 0.102(7) 0.117(7) 0.018(5) -0.004(5) 0.031(5)
F3B 0.107(8) 0.113(8) 0.120(8) -0.014(5) 0.024(5) 0.013(5)
F4A 0.108(7) 0.134(7) 0.136(7) 0.012(4) 0.013(4) -0.030(4)
F4B 0.094(7) 0.072(7) 0.083(6) -0.038(4) -0.018(4) 0.002(5)
O1 0.060(8) 0.18(2) 0.043(9) 0.022(10) 0.018(7) 0.038(10)
C01 0.116(5) 0.116(5) 0.119(5) 0.007(4) 0.000(4) -0.004(4)
C03 0.078(6) 0.058(7) 0.109(8) 0.019(6) -0.002(5) 0.003(6)
O1' 0.115(14) 0.022(9) 0.142(18) 0.014(10) -0.046(11) -0.033(8)
C01' 0.116(5) 0.116(5) 0.119(5) 0.007(4) 0.000(4) -0.004(4)
C03' 0.078(6) 0.058(7) 0.109(8) 0.019(6) -0.002(5) 0.003(6)
C02 0.153(9) 0.045(7) 0.084(7) 0.012(5) 0.012(6) 0.007(6)
C04 0.114(7) 0.106(9) 0.064(7) 0.011(5) -0.008(5) 0.001(6)

_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 C3 2.088(5) . ?
Fe1 C2 2.098(5) . ?
Fe1 C1 2.102(5) . ?
Fe1 C4 2.103(5) . ?
Fe1 C5 2.109(5) . ?
Fe1 P3 2.1828(16) . ?
Fe1 P1 2.1875(16) . ?
Fe1 P2 2.2113(16) . ?
P1 C14 1.823(5) . ?
P1 C15 1.826(5) . ?
P1 C6 1.842(5) . ?
P2 C8 1.834(6) . ?
P2 C17 1.841(5) . ?
P2 C9 1.846(5) . ?
P3 C19 1.824(5) . ?
P3 C11 1.831(5) . ?
P3 C12 1.838(5) . ?
C1 C5 1.408(8) . ?
C1 C2 1.426(8) . ?
C2 C3 1.368(8) . ?
C3 C4 1.424(8) . ?
C4 C5 1.401(8) . ?
C6 C7 1.514(7) . ?
C7 C8 1.540(7) . ?
C9 C10 1.502(7) . ?
C10 C11 1.517(7) . ?
C12 C13 1.514(8) . ?
C13 C14 1.530(7) . ?
C15 C16 1.530(7) . ?
C17 C18 1.508(7) . ?
C19 C20 1.535(8) . ?
B1 F2B 1.234(15) . ?
B1 F1B 1.272(16) . ?
B1 F4B 1.306(15) . ?
B1 F1A 1.326(12) . ?
B1 F4A 1.356(12) . ?
B1 F3A 1.401(14) . ?
B1 F2A 1.418(13) . ?
B1 F3B 1.437(18) . ?
O1 C01 1.30(2) . ?
O1 C03 1.57(2) . ?
C01 C02 1.436(13) . ?
C03 C04 1.496(10) . ?

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
C3 Fe1 C2 38.1(2) . . ?
C3 Fe1 C1 65.5(2) . . ?
C2 Fe1 C1 39.7(2) . . ?
C3 Fe1 C4 39.7(2) . . ?
C2 Fe1 C4 65.5(2) . . ?
C1 Fe1 C4 65.8(2) . . ?
C3 Fe1 C5 65.4(2) . . ?
C2 Fe1 C5 65.5(2) . . ?
C1 Fe1 C5 39.1(2) . . ?
C4 Fe1 C5 38.9(2) . . ?
C3 Fe1 P3 117.14(19) . . ?
C2 Fe1 P3 88.88(18) . . ?
C1 Fe1 P3 96.38(17) . . ?
C4 Fe1 P3 154.32(19) . . ?
C5 Fe1 P3 133.1(2) . . ?
C3 Fe1 P1 89.72(18) . . ?
C2 Fe1 P1 117.40(18) . . ?
C1 Fe1 P1 154.99(18) . . ?
C4 Fe1 P1 97.67(18) . . ?
C5 Fe1 P1 134.2(2) . . ?
P3 Fe1 P1 92.06(6) . . ?
C3 Fe1 P2 147.42(19) . . ?
C2 Fe1 P2 151.81(18) . . ?
C1 Fe1 P2 112.14(18) . . ?
C4 Fe1 P2 108.17(19) . . ?
C5 Fe1 P2 92.05(17) . . ?
P3 Fe1 P2 95.43(6) . . ?
P1 Fe1 P2 90.34(6) . . ?
C14 P1 C15 102.8(3) . . ?
C14 P1 C6 102.9(2) . . ?
C15 P1 C6 101.8(3) . . ?
C14 P1 Fe1 114.6(2) . . ?
C15 P1 Fe1 116.09(17) . . ?
C6 P1 Fe1 116.55(19) . . ?
C8 P2 C17 98.8(2) . . ?
C8 P2 C9 102.2(2) . . ?
C17 P2 C9 100.3(3) . . ?
C8 P2 Fe1 112.45(19) . . ?
C17 P2 Fe1 119.17(19) . . ?
C9 P2 Fe1 120.58(18) . . ?
C19 P3 C11 101.6(3) . . ?
C19 P3 C12 102.5(3) . . ?
C11 P3 C12 102.1(2) . . ?
C19 P3 Fe1 115.13(17) . . ?
C11 P3 Fe1 119.21(18) . . ?
C12 P3 Fe1 114.02(19) . . ?
C5 C1 C2 106.9(6) . . ?
C5 C1 Fe1 70.7(3) . . ?
C2 C1 Fe1 70.0(3) . . ?
C3 C2 C1 108.4(6) . . ?
C3 C2 Fe1 70.5(3) . . ?
C1 C2 Fe1 70.3(3) . . ?
C2 C3 C4 109.1(6) . . ?
C2 C3 Fe1 71.3(3) . . ?
C4 C3 Fe1 70.7(3) . . ?
C5 C4 C3 106.8(6) . . ?
C5 C4 Fe1 70.8(3) . . ?
C3 C4 Fe1 69.6(3) . . ?
C4 C5 C1 108.8(6) . . ?
C4 C5 Fe1 70.4(3) . . ?
C1 C5 Fe1 70.2(3) . . ?
C7 C6 P1 114.6(3) . . ?
C6 C7 C8 118.1(4) . . ?
C7 C8 P2 115.5(4) . . ?
C10 C9 P2 116.3(4) . . ?
C9 C10 C11 112.4(5) . . ?
C10 C11 P3 113.5(3) . . ?
C13 C12 P3 115.3(4) . . ?
C12 C13 C14 115.3(4) . . ?
C13 C14 P1 114.9(4) . . ?
C16 C15 P1 117.2(4) . . ?
C18 C17 P2 114.2(4) . . ?
C20 C19 P3 118.6(4) . . ?
F2B B1 F1B 105.6(13) . . ?
F2B B1 F4B 133.5(13) . . ?
F1B B1 F4B 120.7(13) . . ?
F2B B1 F1A 57.2(9) . . ?
F1B B1 F1A 122.6(13) . . ?
F4B B1 F1A 97.7(9) . . ?
F2B B1 F4A 78.7(9) . . ?
F1B B1 F4A 117.3(12) . . ?
F4B B1 F4A 76.3(9) . . ?
F1A B1 F4A 111.9(10) . . ?
F2B B1 F3A 91.4(10) . . ?
F1B B1 F3A 49.3(9) . . ?
F4B B1 F3A 114.2(11) . . ?
F1A B1 F3A 146.3(11) . . ?
F4A B1 F3A 68.3(8) . . ?
F2B B1 F2A 111.2(12) . . ?
F1B B1 F2A 43.6(9) . . ?
F4B B1 F2A 105.7(10) . . ?
F1A B1 F2A 88.4(9) . . ?
F4A B1 F2A 159.4(11) . . ?
F3A B1 F2A 92.8(9) . . ?
F2B B1 F3B 163.2(14) . . ?
F1B B1 F3B 90.0(12) . . ?
F4B B1 F3B 32.6(8) . . ?
F1A B1 F3B 109.1(10) . . ?
F4A B1 F3B 100.0(11) . . ?
F3A B1 F3B 103.8(10) . . ?
F2A B1 F3B 75.6(9) . . ?
C01 O1 C03 107.9(12) . . ?
O1 C01 C02 115.8(14) . . ?
C04 C03 O1 97.7(9) . . ?

_diffrn_measured_fraction_theta_max 0.770
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.770
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.089