Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2002

data_global

_audit_creation_date 7-02-01  
_audit_creation_method from_SDP_and_SHELX97  
_audit_update_record	? 

_journal_coden_Cambridge      186

loop_
_publ_author_name
'Braunschweig, Holger'
'Colling, M.'
'Englert, Ulli'
'Kollann, C.'

_publ_contact_author_name     	'Dr Holger Braunschweig'  
_publ_contact_author_address 
;
Chemistry
Imperial College
South Kensington
Exhibition Road
London
SW7 2AY
UNITED KINGDOM
;


_publ_contact_author_email 'H.BRAUNSCHWEIG@IC.AC.UK'  
_publ_contact_author_fax '(0241) 8888288'  
_publ_contact_author_phone '(0241) 804666'  
_publ_requested_journal 'J. Chem. Soc. Dalton Trans.'  
_publ_requested_coeditor_name ?  
_publ_contact_letter  
;  
?  
;  

# 3. TITLE AND AUTHOR LIST  
_publ_section_title  
; 
The first silyl and germyl boryl complexes: synthesis from novel  
dichlorosilyl- and dichlorogermylboranes, structural features  
and reactivity  
;  

_publ_section_experimental  
;  

Backgrounds were obtained from analysis of the scan profile 
(Blessing, Coppens  & Becker, 1974)  
;  
_publ_section_references  
;  
Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492.  
Enraf-Nonius, CAD4 Operations Manual, Delft, 1977.  
Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal  
Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands.  
International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D.  
Reidel Publ. Comp., Dordrecht, (1983)  
Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory,  
Tennessee, USA.  
;  

data_MC1_270101

_database_code_CSD		178620   

# 5. CRYSTAL DATA  
_chemical_compound_source 'see paper'  
_exptl_crystal_description 'platelet'  
_exptl_crystal_colour 'orange'  
_exptl_crystal_size_max 0.70  
_exptl_crystal_size_mid 0.62  
_exptl_crystal_size_min 0.10  
_chemical_name_systematic  
; ?  
;  
_chemical_name_common  
; ?  
;  
_chemical_formula_sum 'C16 H32 B1 Cl1 Fe1 O2 Si4'  
loop_  
_atom_type_symbol  
_atom_type_description  
_atom_type_scat_dispersion_real  
_atom_type_scat_dispersion_imag  
_atom_type_scat_source  
'Fe' 'Fe' .3463 .8444  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'Cl' 'Cl' .1484 .1585  

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'Si' 'Si' .0817 .0704  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'O' 'O' .0106 .0060  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'C' 'C' .0033 .0016  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'B' 'B' .0013 .0007  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'H' 'H' .0000 .0000  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
_chemical_formula_weight 470.89  
_symmetry_cell_setting monoclinic  
_symmetry_space_group_name_h-m 'P21/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 17.262(5)  
_cell_length_b 9.403(2)  
_cell_length_c 16.525(5)  
_cell_angle_alpha 90.00  
_cell_angle_beta 106.72(2)  
_cell_angle_gamma 90.00  
_cell_volume 2569(1)  
_cell_measurement_reflns_used 25  
_cell_measurement_theta_min 7  
_cell_measurement_theta_max 14  
_cell_formula_units_z 4.00  
_exptl_crystal_density_diffrn 1.22  
_exptl_crystal_density_meas none  
_diffrn_radiation_type Mo-K\a  
_diffrn_radiation_wavelength 0.71073  
_exptl_absorpt_coefficient_mu 0.882  
_cell_measurement_temperature 213  
_exptl_crystal_F_000 992  
# 6. DATA COLLECTION  
_diffrn_ambient_temperature 213  
_diffrn_measurement_device Enraf_Nonius_CAD4  
_diffrn_measurement_method \q/2\q  
_exptl_absorpt_correction_type numerical  
_exptl_absorpt_correction_T_min 0.594  
_exptl_absorpt_correction_T_max 0.902  
_diffrn_reflns_number 14960  
_reflns_number_total 5031  
_diffrn_reflns_av_R_equivalents 0.154  
_diffrn_reflns_theta_min 3.0  
_diffrn_reflns_theta_max 26.0  
_diffrn_reflns_limit_h_min -21  
_diffrn_reflns_limit_k_min -11  
_diffrn_reflns_limit_l_min -20  
_diffrn_reflns_limit_h_max 21  
_diffrn_reflns_limit_k_max 6  
_diffrn_reflns_limit_l_max 20  
_diffrn_standards_number 3  
_diffrn_standards_interval_time 120  
_diffrn_standards_decay_% -21.98  
# 8. COMPUTING DATA  

_computing_data_collection CAD4_(Enraf-Nonius,_1977)  
_computing_cell_refinement CAD4_(Enraf-Nonius,_1977)  
_computing_data_reduction PROCESS_MolEN_(Fair,_1990)  
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'  
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'  
_computing_molecular_graphics ?  
_computing_publication_material ?  
_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 w=1/[\s^2^(Fo^2^)+(0.0650P)^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 5031  
_refine_ls_number_parameters 235  
_refine_ls_number_restraints 0  
_refine_ls_R_factor_all 0.1941  
_refine_ls_R_factor_gt 0.0793  
_refine_ls_wR_factor_ref 0.1649  
_refine_ls_wR_factor_gt 0.1482  
_refine_ls_goodness_of_fit_ref 0.905  
_refine_ls_restrained_S_all 0.905  
_refine_ls_shift/su_max 0.010  
_refine_ls_shift/su_mean 0.001  
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_calc_flag  
_atom_site_refinement_flags  
_atom_site_disorder_assembly  
_atom_site_disorder_group  
Fe Fe 0.41300(6) 0.79967(10) 0.34050(6) 0.0435(3) Uani 1 d . . .  
C1 C 0.4244(4) 0.8098(8) 0.2386(5) 0.0502(18) Uani 1 d . . .  
O1 O 0.4341(3) 0.8203(6) 0.1737(3) 0.0743(17) Uani 1 d . . .  
C2 C 0.4860(5) 0.9254(9) 0.3749(4) 0.061(2) Uani 1 d . . .  
O2 O 0.5360(4) 1.0103(7) 0.3973(4) 0.098(2) Uani 1 d . . .  
C10 C 0.3278(4) 0.7085(8) 0.3925(4) 0.0547(19) Uani 1 d . . .  
H10 H 0.2748 0.7490 0.3896 0.071 Uiso 1 calc R . .  
C11 C 0.3450(5) 0.6168(8) 0.3351(5) 0.062(2) Uani 1 d . . .  
H11 H 0.3062 0.5840 0.2826 0.080 Uiso 1 calc R . .  
C12 C 0.4263(6) 0.5780(9) 0.3636(6) 0.082(3) Uani 1 d . . .  
H12 H 0.4536 0.5096 0.3363 0.106 Uiso 1 calc R . .  
C13 C 0.4615(5) 0.6528(10) 0.4370(6) 0.078(3) Uani 1 d . . .  
H13 H 0.5187 0.6501 0.4699 0.101 Uiso 1 calc R . .  
C14 C 0.4008(5) 0.7332(8) 0.4559(4) 0.062(2) Uani 1 d . . .  
H14 H 0.4079 0.7959 0.5049 0.081 Uiso 1 calc R . .  
B B 0.3306(5) 0.9503(9) 0.3125(4) 0.044(2) Uani 1 d . . .  
Cl Cl 0.33878(15) 1.0915(3) 0.38963(13) 0.1058(10) Uani 1 d . . .  
Si1 Si 0.23063(11) 0.97745(19) 0.21245(10) 0.0373(5) Uani 1 d . . .  
Si2 Si 0.17737(11) 0.7796(2) 0.12839(11) 0.0434(5) Uani 1 d . . .  
C20 C 0.2531(4) 0.6735(7) 0.0941(4) 0.0543(19) Uani 1 d . . .  
H20A H 0.2933 0.6348 0.1438 0.071 Uiso 1 calc R . .  
H20B H 0.2800 0.7347 0.0625 0.071 Uiso 1 calc R . .  
H20C H 0.2257 0.5951 0.0578 0.071 Uiso 1 calc R . .  
C21 C 0.1009(5) 0.8399(9) 0.0291(4) 0.078(3) Uani 1 d . . .  
H21A H 0.0602 0.8996 0.0434 0.102 Uiso 1 calc R . .  
H21B H 0.0745 0.7566 -0.0030 0.102 Uiso 1 calc R . .  
H21C H 0.1280 0.8951 -0.0052 0.102 Uiso 1 calc R . .  
C22 C 0.1223(5) 0.6566(8) 0.1825(5) 0.078(3) Uani 1 d . . .  
H22A H 0.1599 0.6214 0.2351 0.102 Uiso 1 calc R . .  
H22B H 0.1003 0.5759 0.1452 0.102 Uiso 1 calc R . .  
H22C H 0.0779 0.7082 0.1953 0.102 Uiso 1 calc R . .  
Si3 Si 0.12802(13) 1.0689(2) 0.26546(12) 0.0577(6) Uani 1 d . . .  
C23 C 0.1213(5) 0.9623(9) 0.3582(4) 0.084(3) Uani 1 d . . .  
H23A H 0.0793 1.0026 0.3806 0.109 Uiso 1 calc R . .  
H23B H 0.1735 0.9647 0.4021 0.109 Uiso 1 calc R . .  
H23C H 0.1074 0.8635 0.3407 0.109 Uiso 1 calc R . .  
C24 C 0.0284(4) 1.0607(10) 0.1836(5) 0.086(3) Uani 1 d . . .  
H24A H 0.0140 0.9610 0.1691 0.112 Uiso 1 calc R . .  
H24B H 0.0315 1.1120 0.1331 0.112 Uiso 1 calc R . .  
H24C H -0.0129 1.1047 0.2055 0.112 Uiso 1 calc R . .  
C25 C 0.1451(5) 1.2580(8) 0.2990(5) 0.083(3) Uani 1 d . . .  
H25A H 0.1994 1.2685 0.3384 0.108 Uiso 1 calc R . .  
H25B H 0.1046 1.2870 0.3269 0.108 Uiso 1 calc R . .  
H25C H 0.1401 1.3182 0.2493 0.108 Uiso 1 calc R . .  
Si4 Si 0.26071(13) 1.1534(2) 0.12454(13) 0.0528(6) Uani 1 d . . .  
C26 C 0.3058(5) 1.0761(8) 0.0448(5) 0.082(3) Uani 1 d . . .  
H26A H 0.3524 1.0169 0.0733 0.106 Uiso 1 calc R . .  
H26B H 0.3234 1.1532 0.0142 0.106 Uiso 1 calc R . .  
H26C H 0.2653 1.0176 0.0048 0.106 Uiso 1 calc R . .  
C27 C 0.1669(5) 1.2486(8) 0.0652(5) 0.077(3) Uani 1 d . . .  
H27A H 0.1271 1.1795 0.0333 0.101 Uiso 1 calc R . .  
H27B H 0.1797 1.3168 0.0261 0.101 Uiso 1 calc R . .  
H27C H 0.1444 1.2995 0.1051 0.101 Uiso 1 calc R . .  
C28 C 0.3324(5) 1.2830(9) 0.1879(6) 0.098(3) Uani 1 d . . .  
H28A H 0.3822 1.2339 0.2193 0.127 Uiso 1 calc R . .  
H28B H 0.3083 1.3299 0.2277 0.127 Uiso 1 calc R . .  
H28C H 0.3453 1.3546 0.1506 0.127 Uiso 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  
Fe 0.0480(6) 0.0403(6) 0.0406(5) 0.0028(5) 0.0101(4) 0.0065(6)  
C1 0.043(4) 0.043(5) 0.062(5) -0.005(4) 0.012(4) -0.001(4)  
O1 0.083(4) 0.101(5) 0.047(3) 0.002(3) 0.032(3) -0.015(3)  
C2 0.057(5) 0.065(6) 0.053(5) -0.003(4) 0.003(4) 0.002(5)  
O2 0.090(5) 0.097(5) 0.095(4) -0.020(4) 0.008(4) -0.038(4)  
C10 0.063(5) 0.056(5) 0.050(4) 0.002(4) 0.024(4) 0.000(4)  
C11 0.095(7) 0.044(5) 0.051(5) 0.007(4) 0.030(5) -0.007(5)  
C12 0.104(8) 0.055(6) 0.091(7) 0.003(5) 0.036(6) 0.029(6)  
C13 0.057(6) 0.078(7) 0.089(7) 0.043(6) 0.007(5) 0.016(5)  
C14 0.102(7) 0.046(5) 0.036(4) 0.009(4) 0.015(5) -0.003(5)  
B 0.058(5) 0.039(5) 0.034(4) 0.002(4) 0.012(4) 0.004(4)  
Cl 0.118(2) 0.0862(18) 0.0785(15) -0.0482(13) -0.0268(14) 0.0472(16)  
Si1 0.0433(11) 0.0330(11) 0.0345(10) 0.0017(9) 0.0097(8) 0.0073(9)  
Si2 0.0448(11) 0.0397(12) 0.0432(11) -0.0044(9) 0.0090(9) -0.0049(10)  
C20 0.077(5) 0.042(5) 0.045(4) -0.011(3) 0.018(4) -0.005(4)  
C21 0.078(6) 0.079(6) 0.059(5) -0.013(5) -0.009(4) 0.007(5)  
C22 0.074(6) 0.060(6) 0.113(7) -0.004(5) 0.047(5) -0.016(5)  
Si3 0.0676(15) 0.0662(16) 0.0455(12) 0.0091(11) 0.0262(10) 0.0307(13)  
C23 0.111(7) 0.092(7) 0.067(5) 0.013(5) 0.054(5) 0.027(6)  
C24 0.069(6) 0.115(8) 0.083(6) 0.010(6) 0.037(5) 0.036(6)  
C25 0.108(7) 0.071(6) 0.076(6) -0.005(5) 0.034(5) 0.039(5)  
Si4 0.0661(14) 0.0331(12) 0.0636(13) 0.0089(10) 0.0257(11) 0.0032(11)  
C26 0.104(7) 0.063(6) 0.100(6) 0.031(5) 0.064(6) 0.010(5)  
C27 0.094(6) 0.068(6) 0.073(5) 0.019(4) 0.027(5) 0.010(5)  
C28 0.091(7) 0.064(6) 0.135(8) 0.012(6) 0.027(6) -0.021(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  
Fe C2 1.699(9) . ?  
Fe C1 1.755(8) . ?  
Fe B 1.964(8) . ?  
Fe C11 2.067(7) . ?  
Fe C14 2.075(7) . ?  
Fe C10 2.089(7) . ?  
Fe C13 2.091(7) . ?  
Fe C12 2.116(9) . ?  
C1 O1 1.136(7) . ?  
C2 O2 1.154(8) . ?  
C10 C11 1.375(9) . ?  
C10 C14 1.404(9) . ?  
C11 C12 1.393(10) . ?  
C12 C13 1.382(11) . ?  
C13 C14 1.398(10) . ?  
B Cl 1.817(8) . ?  
B Si1 2.030(8) . ?  
Si1 Si2 2.342(3) . ?  
Si1 Si3 2.355(3) . ?  
Si1 Si4 2.356(3) . ?  
Si2 C20 1.857(7) . ?  
Si2 C21 1.872(7) . ?  
Si2 C22 1.879(7) . ?  
Si3 C24 1.856(8) . ?  
Si3 C25 1.857(8) . ?  
Si3 C23 1.863(7) . ?  
Si4 C28 1.833(8) . ?  
Si4 C27 1.860(8) . ?  
Si4 C26 1.862(7) . ?  
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  
C2 Fe C1 90.3(3) . . ?  
C2 Fe B 89.7(3) . . ?  
C1 Fe B 90.5(3) . . ?  
C2 Fe C11 161.4(3) . . ?  
C1 Fe C11 102.9(3) . . ?  
B Fe C11 102.9(3) . . ?  
C2 Fe C14 99.4(3) . . ?  
C1 Fe C14 165.6(3) . . ?  
B Fe C14 100.0(3) . . ?  
C11 Fe C14 65.3(3) . . ?  
C2 Fe C10 133.5(3) . . ?  
C1 Fe C10 134.8(3) . . ?  
B Fe C10 81.0(3) . . ?  
C11 Fe C10 38.6(3) . . ?  
C14 Fe C10 39.4(3) . . ?  
C2 Fe C13 96.2(4) . . ?  
C1 Fe C13 129.6(4) . . ?  
B Fe C13 139.2(3) . . ?  
C11 Fe C13 65.3(3) . . ?  
C14 Fe C13 39.2(3) . . ?  
C10 Fe C13 65.8(3) . . ?  
C2 Fe C12 126.3(4) . . ?  
C1 Fe C12 101.0(3) . . ?  
B Fe C12 141.6(4) . . ?  
C11 Fe C12 38.9(3) . . ?  
C14 Fe C12 64.7(3) . . ?  
C10 Fe C12 64.9(3) . . ?  
C13 Fe C12 38.3(3) . . ?  
O1 C1 Fe 177.3(6) . . ?  
O2 C2 Fe 179.0(7) . . ?  
C11 C10 C14 107.0(7) . . ?  
C11 C10 Fe 69.8(4) . . ?  
C14 C10 Fe 69.8(4) . . ?  
C10 C11 C12 109.2(7) . . ?  
C10 C11 Fe 71.5(4) . . ?  
C12 C11 Fe 72.5(5) . . ?  
C13 C12 C11 107.9(8) . . ?  
C13 C12 Fe 69.8(5) . . ?  
C11 C12 Fe 68.6(5) . . ?  
C12 C13 C14 107.6(7) . . ?  
C12 C13 Fe 71.8(5) . . ?  
C14 C13 Fe 69.8(4) . . ?  
C13 C14 C10 108.2(7) . . ?  
C13 C14 Fe 71.0(4) . . ?  
C10 C14 Fe 70.8(4) . . ?  
Cl B Fe 117.1(4) . . ?  
Cl B Si1 110.8(4) . . ?  
Fe B Si1 132.0(4) . . ?  
B Si1 Si2 118.6(2) . . ?  
B Si1 Si3 107.2(2) . . ?  
Si2 Si1 Si3 107.57(10) . . ?  
B Si1 Si4 107.7(2) . . ?  
Si2 Si1 Si4 107.98(9) . . ?  
Si3 Si1 Si4 107.34(10) . . ?  
C20 Si2 C21 105.9(3) . . ?  
C20 Si2 C22 108.3(3) . . ?  
C21 Si2 C22 106.1(4) . . ?  
C20 Si2 Si1 114.6(2) . . ?  
C21 Si2 Si1 109.7(3) . . ?  
C22 Si2 Si1 111.8(3) . . ?  
C24 Si3 C25 106.9(4) . . ?  
C24 Si3 C23 108.2(4) . . ?  
C25 Si3 C23 108.1(4) . . ?  
C24 Si3 Si1 110.6(2) . . ?  
C25 Si3 Si1 112.9(3) . . ?  
C23 Si3 Si1 110.1(3) . . ?  
C28 Si4 C27 108.9(4) . . ?  
C28 Si4 C26 108.2(4) . . ?  
C27 Si4 C26 107.0(4) . . ?  
C28 Si4 Si1 110.2(3) . . ?  
C27 Si4 Si1 110.4(3) . . ?  
C26 Si4 Si1 112.1(2) . . ?  
_diffrn_measured_fraction_theta_max .933  
_diffrn_reflns_theta_full 25.00  
_diffrn_measured_fraction_theta_full .935  
_refine_diff_density_max .842  
_refine_diff_density_min -.387  
_refine_diff_density_rms .132  
#===END  
data_MC8170801 

_database_code_CSD	178621 
# 5. CRYSTAL DATA

_chemical_compound_source          'see paper'
_exptl_crystal_description         'plate '
_exptl_crystal_colour              'brown '
_exptl_crystal_size_max            0.8
_exptl_crystal_size_mid            0.7
_exptl_crystal_size_min            0.5
_chemical_name_systematic
; ?
;
_chemical_name_common
; ?
;
_chemical_formula_sum              'C16 H32 B1 Cl1 Fe1 Ge1 O2 Si3'
_chemical_formula_weight              515.39
_symmetry_cell_setting             monoclinic
_symmetry_space_group_name_h-m     'P21/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'
_atom_type_scat_source
'C'  'C'    .0033    .0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H'  'H'    .0000    .0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B'  'B'    .0013    .0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'    .1484    .1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Fe'  'Fe'    .3463    .8444
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ge'  'Ge'    .1547   1.8001
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'    .0106    .0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si'  'Si'    .0817    .0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_cell_length_a                    17.320(3)
_cell_length_b                    9.425(2)
_cell_length_c                    16.572(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  106.532(16)
_cell_angle_gamma                 90.00
_cell_volume                      2593.5(9)
_cell_measurement_reflns_used       23
_cell_measurement_theta_min         12
_cell_measurement_theta_max         16
_cell_formula_units_z                4.00
_exptl_crystal_density_diffrn      1.32
_exptl_crystal_density_meas   none
_diffrn_radiation_type             Mo-K\a
_diffrn_radiation_wavelength         0.71073
_exptl_absorpt_coefficient_mu          1.950
_cell_measurement_temperature        228
_exptl_crystal_F_000               1064

# 6. DATA COLLECTION

_diffrn_ambient_temperature         228
_diffrn_measurement_device         Enraf_Nonius_CAD4
_diffrn_measurement_method         \q/2\q
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_correction_T_min     0.604
_exptl_absorpt_correction_T_max     0.999
_diffrn_reflns_number               12034
_reflns_number_total              5105
_reflns_number_gt                 2317
_reflns_threshold_expression      >2sigma(I)
_diffrn_reflns_av_R_equivalents   0.1856
_diffrn_reflns_av_sigmaI/netI     0.2279
_diffrn_reflns_theta_min             2.2
_diffrn_reflns_theta_max            26.0
_diffrn_reflns_limit_h_min           -16
_diffrn_reflns_limit_k_min           -11
_diffrn_reflns_limit_l_min           -21
_diffrn_reflns_limit_h_max            20
_diffrn_reflns_limit_k_max            11
_diffrn_reflns_limit_l_max            20
_diffrn_standards_number              3
_diffrn_standards_interval_time      120
_diffrn_standards_decay_%            0.00

# 8. COMPUTING DATA


_computing_data_collection         CAD4_(Enraf-Nonius,_1977)
_computing_cell_refinement         CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction          PROCESS_MolEN_(Fair,_1990)
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_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 w=1/[\s^2^(Fo^2^)+(0.0750P)^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          5105
_refine_ls_number_parameters      235
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1961
_refine_ls_R_factor_gt            0.0851
_refine_ls_wR_factor_ref          0.1925
_refine_ls_wR_factor_gt           0.1673
_refine_ls_goodness_of_fit_ref    0.969
_refine_ls_restrained_S_all       0.969
_refine_ls_shift/su_max           0.004
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.41409(9) 0.79992(13) 0.34125(9) 0.0474(4) Uani 1 d . . .
C1 C 0.4244(7) 0.8092(10) 0.2388(8) 0.061(3) Uani 1 d . . .
O1 O 0.4347(5) 0.8220(9) 0.1759(5) 0.080(3) Uani 1 d . . .
C2 C 0.4874(7) 0.9273(14) 0.3765(8) 0.073(3) Uani 1 d . . .
O2 O 0.5367(6) 1.0115(10) 0.3981(6) 0.104(3) Uani 1 d . . .
C10 C 0.3305(8) 0.7083(11) 0.3931(7) 0.061(3) Uani 1 d . . .
H10 H 0.2785 0.7514 0.3911 0.080 Uiso 1 calc R . .
C11 C 0.3442(8) 0.6182(11) 0.3345(7) 0.066(3) Uani 1 d . . .
H11 H 0.3045 0.5843 0.2834 0.085 Uiso 1 calc R . .
C12 C 0.4294(11) 0.5821(12) 0.3623(10) 0.092(5) Uani 1 d . . .
H12 H 0.4577 0.5195 0.3330 0.120 Uiso 1 calc R . .
C13 C 0.4633(7) 0.6517(14) 0.4373(10) 0.088(5) Uani 1 d . . .
H13 H 0.5199 0.6472 0.4707 0.115 Uiso 1 calc R . .
C14 C 0.4030(10) 0.7295(13) 0.4572(7) 0.081(4) Uani 1 d . . .
H14 H 0.4097 0.7889 0.5072 0.106 Uiso 1 calc R . .
B B 0.3309(7) 0.9509(10) 0.3128(7) 0.049(3) Uani 1 d . . .
Cl Cl 0.3387(2) 1.0905(4) 0.3907(2) 0.1184(16) Uani 1 d . . .
Ge1 Ge 0.23018(6) 0.97721(9) 0.21150(6) 0.0382(3) Uani 1 d . . .
Si2 Si 0.17719(17) 0.7761(3) 0.12732(18) 0.0476(7) Uani 1 d . . .
C20 C 0.2549(7) 0.6741(9) 0.0939(7) 0.060(3) Uani 1 d . . .
H20A H 0.2906 0.6258 0.1427 0.079 Uiso 1 calc R . .
H20B H 0.2865 0.7392 0.0697 0.079 Uiso 1 calc R . .
H20C H 0.2285 0.6036 0.0515 0.079 Uiso 1 calc R . .
C21 C 0.0992(7) 0.8406(13) 0.0293(7) 0.083(4) Uani 1 d . . .
H21A H 0.0542 0.8840 0.0451 0.108 Uiso 1 calc R . .
H21B H 0.0795 0.7603 -0.0084 0.108 Uiso 1 calc R . .
H21C H 0.1236 0.9111 0.0006 0.108 Uiso 1 calc R . .
C22 C 0.1216(8) 0.6588(11) 0.1815(10) 0.099(5) Uani 1 d . . .
H22A H 0.1601 0.6094 0.2280 0.129 Uiso 1 calc R . .
H22B H 0.0905 0.5890 0.1415 0.129 Uiso 1 calc R . .
H22C H 0.0851 0.7160 0.2038 0.129 Uiso 1 calc R . .
Si3 Si 0.1263(2) 1.0692(3) 0.2655(2) 0.0623(9) Uani 1 d . . .
C23 C 0.1188(8) 0.9648(15) 0.3570(7) 0.090(4) Uani 1 d . . .
H23A H 0.0743 1.0011 0.3766 0.118 Uiso 1 calc R . .
H23B H 0.1693 0.9729 0.4023 0.118 Uiso 1 calc R . .
H23C H 0.1089 0.8651 0.3407 0.118 Uiso 1 calc R . .
C24 C 0.0295(7) 1.0596(14) 0.1859(8) 0.087(4) Uani 1 d . . .
H24A H 0.0191 0.9615 0.1662 0.113 Uiso 1 calc R . .
H24B H 0.0302 1.1211 0.1385 0.113 Uiso 1 calc R . .
H24C H -0.0131 1.0909 0.2102 0.113 Uiso 1 calc R . .
C25 C 0.1419(9) 1.2571(13) 0.2980(9) 0.100(5) Uani 1 d . . .
H25A H 0.1983 1.2716 0.3304 0.130 Uiso 1 calc R . .
H25B H 0.1067 1.2816 0.3329 0.130 Uiso 1 calc R . .
H25C H 0.1291 1.3178 0.2479 0.130 Uiso 1 calc R . .
Si4 Si 0.26000(19) 1.1549(3) 0.1224(2) 0.0561(8) Uani 1 d . . .
C26 C 0.3047(8) 1.0826(13) 0.0425(8) 0.087(4) Uani 1 d . . .
H26A H 0.3523 1.0260 0.0702 0.113 Uiso 1 calc R . .
H26B H 0.3204 1.1609 0.0116 0.113 Uiso 1 calc R . .
H26C H 0.2651 1.0225 0.0032 0.113 Uiso 1 calc R . .
C27 C 0.1651(8) 1.2483(12) 0.0621(8) 0.086(4) Uani 1 d . . .
H27A H 0.1218 1.1787 0.0425 0.112 Uiso 1 calc R . .
H27B H 0.1744 1.2974 0.0136 0.112 Uiso 1 calc R . .
H27C H 0.1496 1.3176 0.0989 0.112 Uiso 1 calc R . .
C28 C 0.3329(8) 1.2863(11) 0.1879(9) 0.095(4) Uani 1 d . . .
H28A H 0.3853 1.2405 0.2115 0.124 Uiso 1 calc R . .
H28B H 0.3124 1.3204 0.2338 0.124 Uiso 1 calc R . .
H28C H 0.3389 1.3666 0.1526 0.124 Uiso 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
Fe 0.0576(10) 0.0356(7) 0.0477(9) 0.0039(6) 0.0128(7) 0.0093(6)
C1 0.076(8) 0.038(5) 0.078(9) 0.001(6) 0.036(7) 0.008(5)
O1 0.115(7) 0.085(5) 0.055(5) 0.002(4) 0.045(5) -0.006(5)
C2 0.051(8) 0.095(9) 0.072(8) 0.000(7) 0.014(7) -0.005(7)
O2 0.095(7) 0.097(7) 0.104(7) -0.018(6) 0.002(6) -0.035(6)
C10 0.083(9) 0.054(6) 0.054(7) 0.020(6) 0.030(7) 0.012(6)
C11 0.098(10) 0.046(6) 0.053(7) -0.003(5) 0.022(7) -0.006(6)
C12 0.168(16) 0.043(6) 0.087(11) 0.018(7) 0.070(11) 0.035(8)
C13 0.053(8) 0.088(9) 0.121(13) 0.067(9) 0.019(8) 0.036(7)
C14 0.139(13) 0.066(7) 0.039(7) 0.018(6) 0.026(8) 0.009(8)
B 0.061(8) 0.035(6) 0.048(7) -0.004(5) 0.013(6) 0.010(5)
Cl 0.138(3) 0.087(2) 0.093(3) -0.054(2) -0.028(2) 0.061(2)
Ge1 0.0497(6) 0.0242(4) 0.0407(6) 0.0010(4) 0.0128(5) 0.0059(5)
Si2 0.0529(18) 0.0351(13) 0.0531(18) -0.0071(12) 0.0122(15) -0.0051(12)
C20 0.096(9) 0.034(5) 0.055(7) -0.011(5) 0.026(6) 0.002(5)
C21 0.091(10) 0.075(8) 0.066(8) -0.010(7) -0.006(7) 0.014(7)
C22 0.106(11) 0.045(6) 0.179(15) -0.001(8) 0.092(11) -0.032(7)
Si3 0.074(2) 0.0622(18) 0.0595(19) 0.0079(15) 0.0327(18) 0.0280(16)
C23 0.121(11) 0.111(10) 0.058(7) 0.016(8) 0.054(8) 0.038(9)
C24 0.060(8) 0.103(10) 0.102(10) -0.002(8) 0.030(8) 0.024(7)
C25 0.120(12) 0.067(7) 0.112(12) -0.020(8) 0.031(10) 0.047(8)
Si4 0.077(2) 0.0276(12) 0.070(2) 0.0100(13) 0.0306(18) 0.0035(13)
C26 0.102(10) 0.077(8) 0.103(10) 0.038(8) 0.064(9) 0.019(7)
C27 0.133(12) 0.049(6) 0.084(9) 0.039(6) 0.041(9) 0.019(7)
C28 0.102(11) 0.043(6) 0.133(13) -0.003(7) 0.022(9) -0.027(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
Fe C2 1.724(13) . ?
Fe C1 1.760(12) . ?
Fe B 1.985(11) . ?
Fe C10 2.072(10) . ?
Fe C11 2.082(11) . ?
Fe C12 2.086(11) . ?
Fe C14 2.093(11) . ?
Fe C13 2.107(11) . ?
C1 O1 1.112(12) . ?
C2 O2 1.146(13) . ?
C10 C11 1.362(14) . ?
C10 C14 1.409(16) . ?
C10 H10 0.9800 . ?
C11 C12 1.456(19) . ?
C11 H11 0.9800 . ?
C12 C13 1.380(18) . ?
C12 H12 0.9800 . ?
C13 C14 1.390(17) . ?
C13 H13 0.9800 . ?
C14 H14 0.9800 . ?
B Cl 1.821(11) . ?
B Ge1 2.063(12) . ?
Ge1 Si2 2.378(3) . ?
Ge1 Si4 2.384(3) . ?
Ge1 Si3 2.389(3) . ?
Si2 C22 1.857(10) . ?
Si2 C20 1.862(10) . ?
Si2 C21 1.893(11) . ?
C20 H20A 0.9801 . ?
C20 H20B 0.9801 . ?
C20 H20C 0.9801 . ?
C21 H21A 0.9801 . ?
C21 H21B 0.9801 . ?
C21 H21C 0.9801 . ?
C22 H22A 0.9801 . ?
C22 H22B 0.9801 . ?
C22 H22C 0.9801 . ?
Si3 C24 1.817(12) . ?
Si3 C23 1.842(11) . ?
Si3 C25 1.849(12) . ?
C23 H23A 0.9801 . ?
C23 H23B 0.9801 . ?
C23 H23C 0.9801 . ?
C24 H24A 0.9801 . ?
C24 H24B 0.9801 . ?
C24 H24C 0.9801 . ?
C25 H25A 0.9801 . ?
C25 H25B 0.9801 . ?
C25 H25C 0.9801 . ?
Si4 C26 1.845(11) . ?
Si4 C28 1.878(12) . ?
Si4 C27 1.882(12) . ?
C26 H26A 0.9801 . ?
C26 H26B 0.9801 . ?
C26 H26C 0.9801 . ?
C27 H27A 0.9801 . ?
C27 H27B 0.9801 . ?
C27 H27C 0.9801 . ?
C28 H28A 0.9801 . ?
C28 H28B 0.9801 . ?
C28 H28C 0.9801 . ?

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
C2 Fe C1 91.4(5) . . ?
C2 Fe B 89.8(5) . . ?
C1 Fe B 90.1(5) . . ?
C2 Fe C10 133.2(5) . . ?
C1 Fe C10 134.1(5) . . ?
B Fe C10 81.5(5) . . ?
C2 Fe C11 162.2(5) . . ?
C1 Fe C11 101.9(5) . . ?
B Fe C11 101.9(5) . . ?
C10 Fe C11 38.3(4) . . ?
C2 Fe C12 125.6(7) . . ?
C1 Fe C12 99.6(5) . . ?
B Fe C12 142.6(6) . . ?
C10 Fe C12 65.9(5) . . ?
C11 Fe C12 40.9(5) . . ?
C2 Fe C14 99.3(6) . . ?
C1 Fe C14 164.4(5) . . ?
B Fe C14 101.3(5) . . ?
C10 Fe C14 39.5(5) . . ?
C11 Fe C14 65.5(5) . . ?
C12 Fe C14 64.8(5) . . ?
C2 Fe C13 96.0(6) . . ?
C1 Fe C13 129.2(5) . . ?
B Fe C13 139.9(5) . . ?
C10 Fe C13 65.8(4) . . ?
C11 Fe C13 66.4(5) . . ?
C12 Fe C13 38.4(5) . . ?
C14 Fe C13 38.7(5) . . ?
O1 C1 Fe 175.3(10) . . ?
O2 C2 Fe 178.3(12) . . ?
C11 C10 C14 109.1(11) . . ?
C11 C10 Fe 71.3(6) . . ?
C14 C10 Fe 71.0(7) . . ?
C11 C10 H10 125.5 . . ?
C14 C10 H10 125.5 . . ?
Fe C10 H10 123.9 . . ?
C10 C11 C12 106.7(11) . . ?
C10 C11 Fe 70.5(6) . . ?
C12 C11 Fe 69.7(7) . . ?
C10 C11 H11 126.7 . . ?
C12 C11 H11 126.7 . . ?
Fe C11 H11 124.7 . . ?
C13 C12 C11 107.9(11) . . ?
C13 C12 Fe 71.6(7) . . ?
C11 C12 Fe 69.4(6) . . ?
C13 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
Fe C12 H12 124.6 . . ?
C12 C13 C14 107.9(12) . . ?
C12 C13 Fe 70.0(7) . . ?
C14 C13 Fe 70.1(6) . . ?
C12 C13 H13 126.0 . . ?
C14 C13 H13 126.0 . . ?
Fe C13 H13 125.5 . . ?
C13 C14 C10 108.4(12) . . ?
C13 C14 Fe 71.2(7) . . ?
C10 C14 Fe 69.4(6) . . ?
C13 C14 H14 125.8 . . ?
C10 C14 H14 125.8 . . ?
Fe C14 H14 125.1 . . ?
Cl B Fe 116.5(6) . . ?
Cl B Ge1 111.5(5) . . ?
Fe B Ge1 131.9(5) . . ?
B Ge1 Si2 118.5(3) . . ?
B Ge1 Si4 107.8(3) . . ?
Si2 Ge1 Si4 108.19(11) . . ?
B Ge1 Si3 106.9(3) . . ?
Si2 Ge1 Si3 107.64(12) . . ?
Si4 Ge1 Si3 107.22(11) . . ?
C22 Si2 C20 110.8(5) . . ?
C22 Si2 C21 105.4(7) . . ?
C20 Si2 C21 108.1(5) . . ?
C22 Si2 Ge1 110.9(4) . . ?
C20 Si2 Ge1 113.3(3) . . ?
C21 Si2 Ge1 108.0(4) . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 Si3 C23 107.7(6) . . ?
C24 Si3 C25 106.7(6) . . ?
C23 Si3 C25 108.1(7) . . ?
C24 Si3 Ge1 110.4(4) . . ?
C23 Si3 Ge1 110.6(4) . . ?
C25 Si3 Ge1 113.2(5) . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si3 C24 H24A 109.5 . . ?
Si3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si3 C25 H25A 109.5 . . ?
Si3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 Si4 C28 108.0(6) . . ?
C26 Si4 C27 105.8(6) . . ?
C28 Si4 C27 109.9(6) . . ?
C26 Si4 Ge1 113.2(4) . . ?
C28 Si4 Ge1 109.5(4) . . ?
C27 Si4 Ge1 110.3(4) . . ?
Si4 C26 H26A 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si4 C27 H27A 109.5 . . ?
Si4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si4 C28 H28A 109.5 . . ?
Si4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_diffrn_measured_fraction_theta_max     .933
_diffrn_reflns_theta_full              26.04
_diffrn_measured_fraction_theta_full    .933
_refine_diff_density_max    1.145
_refine_diff_density_min    -.785
_refine_diff_density_rms     .135

data_MC2_301100 

_database_code_CSD	178622  
# 5. CRYSTAL DATA  
_chemical_compound_source 'see paper'  
_exptl_crystal_description 'platelet'  
_exptl_crystal_colour 'red'  
_exptl_crystal_size_max 0.55  
_exptl_crystal_size_mid 0.35  
_exptl_crystal_size_min 0.08  
_chemical_name_systematic  
; ?  
;  
_chemical_name_common  
; ?  
;  
_chemical_formula_sum 'C17 H35 B1 Cl1 Mn1 O2 Si4'  
_chemical_formula_weight 485.01  
loop_  
_atom_type_symbol  
_atom_type_description  
_atom_type_scat_dispersion_real  
_atom_type_scat_dispersion_imag  
_atom_type_scat_source  
'Mn' 'Mn' .3368 .7283  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'Cl' 'Cl' .1484 .1585  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'Si' 'Si' .0817 .0704  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'O' 'O' .0106 .0060  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'C' 'C' .0033 .0016  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'B' 'B' .0013 .0007  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'H' 'H' .0000 .0000  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
loop_  
_symmetry_equiv_pos_as_xyz  
'x, y, z'  
'-x, y, -z+1/2'  
'x+1/2, y+1/2, z'  
'-x+1/2, y+1/2, -z+1/2'  
'-x, -y, -z'  
'x, -y, z-1/2'  
'-x+1/2, -y+1/2, -z'  
'x+1/2, -y+1/2, z-1/2'  
_symmetry_cell_setting monoclinic  
_symmetry_space_group_name_h-m 'C2/c'  
_cell_length_a 34.35(2)  
_cell_length_b 9.268(9)  
_cell_length_c 17.00(2)  
_cell_angle_alpha 90.00  
_cell_angle_beta 100.94(5)  
_cell_angle_gamma 90.00  
_cell_volume 5312(9)  

_cell_measurement_reflns_used 12  
_cell_measurement_theta_min 3  
_cell_measurement_theta_max 8  
_cell_formula_units_z 8.00  
_exptl_crystal_density_diffrn 1.21  
_exptl_crystal_density_meas none  
_diffrn_radiation_type Mo-K\a  
_diffrn_radiation_wavelength 0.71073  
_exptl_absorpt_coefficient_mu 0.765  
_cell_measurement_temperature 233  
_exptl_crystal_F_000 2048  
# 6. DATA COLLECTION  
_diffrn_ambient_temperature 233  
_diffrn_measurement_device Enraf_Nonius_CAD4  
_diffrn_measurement_method \w  
_exptl_absorpt_correction_type numerical  
_exptl_absorpt_correction_T_min 0.746  
_exptl_absorpt_correction_T_max 0.943  
_diffrn_reflns_number 11192  
_reflns_number_total 4687  
_diffrn_reflns_av_R_equivalents 0.246  
_diffrn_reflns_theta_min 2.3  
_diffrn_reflns_theta_max 25.0  
_diffrn_reflns_limit_h_min -11  
_diffrn_reflns_limit_k_min -20  
_diffrn_reflns_limit_l_min -21  
_diffrn_reflns_limit_h_max 11  
_diffrn_reflns_limit_k_max 2  
_diffrn_reflns_limit_l_max 20  
_diffrn_standards_number 3  
_diffrn_standards_interval_time 120  
_diffrn_standards_decay_% 0.00  
_reflns_number_gt 925  
_reflns_threshold_expression >2sigma(I)  
_computing_data_collection CAD4_(Enraf-Nonius,_1977)  
_computing_cell_refinement CAD4_(Enraf-Nonius,_1977)  
_computing_data_reduction PROCESS_MolEN_(Fair,_1990)  
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'  
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'  
_computing_molecular_graphics ?  
_computing_publication_material ?  
_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 w=1/[\s^2^(Fo^2^)+(0.0300P)^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 4687  
_refine_ls_number_parameters 145  
_refine_ls_number_restraints 0  
_refine_ls_R_factor_all 0.3943  
_refine_ls_R_factor_gt 0.1145  
_refine_ls_wR_factor_ref 0.2245  
_refine_ls_wR_factor_gt 0.1814  
_refine_ls_goodness_of_fit_ref 0.894  
_refine_ls_restrained_S_all 0.894  
_refine_ls_shift/su_max 0.024  
_refine_ls_shift/su_mean 0.001  
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_calc_flag  
_atom_site_refinement_flags  
_atom_site_disorder_assembly  
_atom_site_disorder_group  
Mn Mn 0.29604(7) 0.0774(3) 0.91630(16) 0.0455(8) Uani 1 d . . .  
H1 H 0.3305 -0.0025 0.9148 0.059 Uiso 1 d R . .  
C1 C 0.2942(5) 0.2352(19) 0.8686(10) 0.059(6) Uiso 1 d . . .  
O1 O 0.2918(3) 0.3556(11) 0.8378(6) 0.059(4) Uiso 1 d . . .  
C2 C 0.3244(4) 0.1542(16) 1.0044(9) 0.038(4) Uiso 1 d . . .  
O2 O 0.3403(3) 0.1888(12) 1.0682(7) 0.072(4) Uiso 1 d . . .  
C10 C 0.2462(4) -0.0327(15) 0.8480(9) 0.043(5) Uiso 1 d . . .  
H10 H 0.2399 -0.0351 0.7893 0.056 Uiso 1 calc R . .  
C11 C 0.2345(5) 0.079(2) 0.9015(10) 0.079(6) Uiso 1 d . . .  
H11 H 0.2197 0.1678 0.8859 0.102 Uiso 1 calc R . .  
C12 C 0.2485(5) 0.0313(18) 0.9755(10) 0.064(6) Uiso 1 d . . .  
H12 H 0.2434 0.0777 1.0244 0.084 Uiso 1 calc R . .  
C13 C 0.2700(4) -0.0857(18) 0.9744(10) 0.056(5) Uiso 1 d . . .  
H13 H 0.2854 -0.1319 1.0222 0.073 Uiso 1 calc R . .  
C14 C 0.2682(5) -0.1337(19) 0.8994(11) 0.064(6) Uiso 1 d . . .  
C15 C 0.2848(5) -0.2673(16) 0.8661(9) 0.073(6) Uiso 1 d . . .  
H15A H 0.3063 -0.3074 0.9065 0.095 Uiso 1 calc R . .  
H15B H 0.2952 -0.2416 0.8180 0.095 Uiso 1 calc R . .  
H15C H 0.2637 -0.3394 0.8521 0.095 Uiso 1 calc R . .  
B B 0.3343(4) 0.0880(19) 0.8308(10) 0.031(5) Uiso 1 d . . .  
Cl Cl 0.31800(12) -0.0064(5) 0.7418(3) 0.0779(17) Uani 1 d . . .  
Si1 Si 0.38733(13) 0.1912(5) 0.8331(3) 0.0413(14) Uani 1 d . . .  
Si2 Si 0.41449(14) 0.3420(5) 0.9406(3) 0.0522(16) Uani 1 d . . .  
C20 C 0.3776(4) 0.4798(16) 0.9622(8) 0.065(6) Uiso 1 d . . .  
H20A H 0.3567 0.4314 0.9843 0.085 Uiso 1 calc R . .  
H20B H 0.3658 0.5295 0.9125 0.085 Uiso 1 calc R . .  
H20C H 0.3911 0.5502 1.0011 0.085 Uiso 1 calc R . .  
C21 C 0.4560(4) 0.4488(16) 0.9109(8) 0.066(6) Uiso 1 d . . .  
H21A H 0.4710 0.4982 0.9580 0.086 Uiso 1 calc R . .  
H21B H 0.4449 0.5202 0.8702 0.086 Uiso 1 calc R . .  
H21C H 0.4737 0.3835 0.8889 0.086 Uiso 1 calc R . .  
C22 C 0.4352(5) 0.2439(16) 1.0345(8) 0.068(6) Uiso 1 d . . .  
H22A H 0.4594 0.1928 1.0279 0.088 Uiso 1 calc R . .  
H22B H 0.4157 0.1742 1.0464 0.088 Uiso 1 calc R . .  
H22C H 0.4416 0.3129 1.0788 0.088 Uiso 1 calc R . .  
Si3 Si 0.38540(14) 0.3264(6) 0.7154(3) 0.0634(17) Uani 1 d . . .  
C30 C 0.3678(5) 0.5172(17) 0.7301(9) 0.079(6) Uiso 1 d . . .  
H30A H 0.3895 0.5724 0.7624 0.103 Uiso 1 calc R . .  
H30B H 0.3453 0.5138 0.7577 0.103 Uiso 1 calc R . .  
H30C H 0.3597 0.5637 0.6778 0.103 Uiso 1 calc R . .  
C31 C 0.3513(4) 0.2437(17) 0.6250(8) 0.069(6) Uiso 1 d . . .  
H31A H 0.3469 0.3134 0.5809 0.090 Uiso 1 calc R . .  
H31B H 0.3259 0.2188 0.6395 0.090 Uiso 1 calc R . .  
H31C H 0.3636 0.1564 0.6082 0.090 Uiso 1 calc R . .  
C32 C 0.4376(4) 0.3428(17) 0.6910(9) 0.088(7) Uiso 1 d . . .  
H32A H 0.4482 0.2463 0.6846 0.114 Uiso 1 calc R . .  
H32B H 0.4549 0.3931 0.7349 0.114 Uiso 1 calc R . .  
H32C H 0.4362 0.3975 0.6412 0.114 Uiso 1 calc R . .  
Si4 Si 0.43089(14) -0.0073(6) 0.8373(3) 0.0562(16) Uani 1 d . . .  
C40 C 0.4840(4) 0.0633(17) 0.8620(8) 0.069(6) Uiso 1 d . . .  
H40A H 0.5025 -0.0182 0.8682 0.090 Uiso 1 calc R . .  
H40B H 0.4877 0.1186 0.9120 0.090 Uiso 1 calc R . .  
H40C H 0.4890 0.1257 0.8184 0.090 Uiso 1 calc R . .  
C41 C 0.4219(4) -0.1316(17) 0.9163(9) 0.083(7) Uiso 1 d . . .  
H41A H 0.4007 -0.1993 0.8939 0.108 Uiso 1 calc R . .  
H41B H 0.4139 -0.0764 0.9598 0.108 Uiso 1 calc R . .  
H41C H 0.4462 -0.1855 0.9371 0.108 Uiso 1 calc R . .  
C42 C 0.4239(5) -0.0984(19) 0.7409(9) 0.100(7) Uiso 1 d . . .  
H42A H 0.4427 -0.1787 0.7438 0.131 Uiso 1 calc R . .  
H42B H 0.4285 -0.0300 0.6996 0.131 Uiso 1 calc R . .  
H42C H 0.3967 -0.1355 0.7272 0.131 Uiso 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  
Mn 0.0379(16) 0.0394(18) 0.060(2) 0.0052(17) 0.0112(14) 0.0023(15)  
Cl 0.058(3) 0.088(4) 0.092(4) -0.034(3) 0.023(3) -0.030(3)  
Si1 0.043(3) 0.026(3) 0.054(4) 0.000(3) 0.007(3) -0.004(3)  
Si2 0.045(3) 0.040(4) 0.068(4) -0.013(3) -0.001(3) 0.005(3)  
Si3 0.053(4) 0.067(4) 0.067(4) 0.019(4) 0.004(3) -0.012(3)  
Si4 0.056(3) 0.050(4) 0.065(4) -0.003(3) 0.016(3) 0.004(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  
Mn C1 1.667(18) . ?  
Mn C2 1.773(15) . ?  
Mn C11 2.081(16) . ?  
Mn C13 2.096(16) . ?  
Mn C12 2.117(16) . ?  

Mn C10 2.136(14) . ?  
Mn B 2.138(16) . ?  
Mn C14 2.172(17) . ?  
C1 O1 1.229(17) . ?  
C2 O2 1.163(15) . ?  
C10 C14 1.400(18) . ?  
C10 C11 1.481(19) . ?  
C11 C12 1.332(19) . ?  
C12 C13 1.314(19) . ?  
C13 C14 1.340(19) . ?  
C14 C15 1.518(19) . ?  
B Cl 1.745(16) . ?  
B Si1 2.052(16) . ?  
Si1 Si2 2.348(7) . ?  
Si1 Si3 2.351(7) . ?  
Si1 Si4 2.364(7) . ?  
Si2 C22 1.857(14) . ?  
Si2 C21 1.882(14) . ?  
Si2 C20 1.884(14) . ?  
Si3 C30 1.900(15) . ?  
Si3 C31 1.906(14) . ?  
Si3 C32 1.920(15) . ?  
Si4 C42 1.818(15) . ?  
Si4 C41 1.839(15) . ?  
Si4 C40 1.908(13) . ?  
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  
C1 Mn C2 91.3(7) . . ?  
C1 Mn C11 89.5(8) . . ?  
C2 Mn C11 118.9(7) . . ?  
C1 Mn C13 151.8(7) . . ?  
C2 Mn C13 96.2(6) . . ?  
C11 Mn C13 63.1(6) . . ?  
C1 Mn C12 116.5(8) . . ?  
C2 Mn C12 91.7(6) . . ?  
C11 Mn C12 37.0(5) . . ?  
C13 Mn C12 36.4(5) . . ?  
C1 Mn C10 101.6(7) . . ?  
C2 Mn C10 155.0(6) . . ?  
C11 Mn C10 41.1(5) . . ?  
C13 Mn C10 62.7(6) . . ?  
C12 Mn C10 63.3(6) . . ?  
C1 Mn B 66.5(7) . . ?  
C2 Mn B 104.2(6) . . ?  
C11 Mn B 131.2(7) . . ?  
C13 Mn B 136.5(7) . . ?  
C12 Mn B 163.9(7) . . ?  
C10 Mn B 100.7(6) . . ?  
C1 Mn C14 138.6(7) . . ?  
C2 Mn C14 129.1(7) . . ?  
C11 Mn C14 65.0(7) . . ?  
C13 Mn C14 36.5(5) . . ?  
C12 Mn C14 61.4(6) . . ?  
C10 Mn C14 37.9(5) . . ?  
B Mn C14 105.2(7) . . ?  
O1 C1 Mn 175.6(16) . . ?  
O2 C2 Mn 169.6(14) . . ?  
C14 C10 C11 105.1(14) . . ?  
C14 C10 Mn 72.5(9) . . ?  
C11 C10 Mn 67.4(8) . . ?  
C12 C11 C10 104.9(17) . . ?  
C12 C11 Mn 73.0(11) . . ?  
C10 C11 Mn 71.5(9) . . ?  
C13 C12 C11 111.2(18) . . ?  
C13 C12 Mn 70.9(10) . . ?  
C11 C12 Mn 70.0(11) . . ?  
C12 C13 C14 111.3(17) . . ?  
C12 C13 Mn 72.7(11) . . ?  
C14 C13 Mn 74.9(10) . . ?  
C13 C14 C10 107.1(16) . . ?  
C13 C14 C15 132.3(18) . . ?  
C10 C14 C15 120.7(16) . . ?  
C13 C14 Mn 68.6(10) . . ?  
C10 C14 Mn 69.6(9) . . ?  
C15 C14 Mn 126.7(11) . . ?  
Cl B Si1 112.8(8) . . ?  
Cl B Mn 115.4(8) . . ?  
Si1 B Mn 131.8(8) . . ?  
B Si1 Si2 120.8(5) . . ?  
B Si1 Si3 110.5(5) . . ?  
Si2 Si1 Si3 106.7(3) . . ?  
B Si1 Si4 101.1(5) . . ?  
Si2 Si1 Si4 106.5(2) . . ?  
Si3 Si1 Si4 110.9(3) . . ?  
C22 Si2 C21 107.6(7) . . ?  
C22 Si2 C20 109.1(7) . . ?  
C21 Si2 C20 105.5(7) . . ?  
C22 Si2 Si1 114.1(5) . . ?  
C21 Si2 Si1 108.3(5) . . ?  
C20 Si2 Si1 111.9(5) . . ?  
C30 Si3 C31 108.6(7) . . ?  
C30 Si3 C32 106.7(7) . . ?  
C31 Si3 C32 108.3(7) . . ?  
C30 Si3 Si1 110.0(5) . . ?  
C31 Si3 Si1 112.6(5) . . ?  
C32 Si3 Si1 110.4(5) . . ?  
C42 Si4 C41 110.8(8) . . ?  
C42 Si4 C40 108.3(7) . . ?  
C41 Si4 C40 109.9(7) . . ?  
C42 Si4 Si1 111.1(6) . . ?  
C41 Si4 Si1 108.5(5) . . ?  
C40 Si4 Si1 108.2(5) . . ?  
_diffrn_measured_fraction_theta_max .930  
_diffrn_reflns_theta_full 25.10  
_diffrn_measured_fraction_theta_full .930  
_refine_diff_density_max .720  
_refine_diff_density_min -.809  
_refine_diff_density_rms .143  
#===END  
data_MC3_170401  
# 5. CRYSTAL DATA  
_database_code_CSD 	178623

_chemical_compound_source 'see paper'  
_exptl_crystal_description 'platelet'  
_exptl_crystal_colour 'orange'  
_exptl_crystal_size_max 0.65  
_exptl_crystal_size_mid 0.50  
_exptl_crystal_size_min 0.17  
_chemical_name_systematic  
; ?  
;  
_chemical_name_common  
; ?  
;  
_chemical_formula_sum 'C16 H32 B1 F1 Fe1 O2 Si4'  
loop_  
_atom_type_symbol  
_atom_type_description  
_atom_type_scat_dispersion_real  
_atom_type_scat_dispersion_imag  
_atom_type_scat_source  
'Fe' 'Fe' .3463 .8444  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'Si' 'Si' .0817 .0704  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'F' 'F' .0171 .0103  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'O' 'O' .0106 .0060  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'C' 'C' .0033 .0016  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'B' 'B' .0013 .0007  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
'H' 'H' .0000 .0000  
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'  
_chemical_formula_weight 454.43  
_symmetry_cell_setting monoclinic  
_symmetry_space_group_name_h-m 'C2/c '  
loop_  
_symmetry_equiv_pos_as_xyz  
'x, y, z'  
'-x, y, -z+1/2'  
'x+1/2, y+1/2, z'  
'-x+1/2, y+1/2, -z+1/2'  
'-x, -y, -z'  
'x, -y, z-1/2'  
'-x+1/2, -y+1/2, -z'  
'x+1/2, -y+1/2, z-1/2'  
_cell_length_a 16.782(5)  
_cell_length_b 9.611(3)  
_cell_length_c 31.15(1)  
_cell_angle_alpha 90.00  
_cell_angle_beta 94.84(3)  
_cell_angle_gamma 90.00  
_cell_volume 5006(3)  
_cell_measurement_reflns_used 25  
_cell_measurement_theta_min 10  
_cell_measurement_theta_max 12  
_cell_formula_units_z 8.00  
_exptl_crystal_density_diffrn 1.21  
_exptl_crystal_density_meas none  
_diffrn_radiation_type Mo-K\a  
_diffrn_radiation_wavelength 0.71073  
_exptl_absorpt_coefficient_mu 0.803  
_cell_measurement_temperature 213  

_exptl_crystal_F_000 1920  
# 6. DATA COLLECTION  
_diffrn_ambient_temperature 213  
_diffrn_measurement_device Enraf_Nonius_CAD4  
_diffrn_measurement_method \q/2\q  
_exptl_absorpt_correction_type numerical  
_exptl_absorpt_correction_T_min 0.684  
_exptl_absorpt_correction_T_max 0.912  
_diffrn_reflns_number 10134  
_reflns_number_total 4894  
_reflns_number_gt 3012  
_reflns_threshold_expression >2sigma(I)  
_diffrn_reflns_av_R_equivalents 0.116  
_diffrn_reflns_theta_min 2.4  
_diffrn_reflns_theta_max 26.0  
_diffrn_reflns_limit_h_min 0  
_diffrn_reflns_limit_k_min -11  
_diffrn_reflns_limit_l_min -38  
_diffrn_reflns_limit_h_max 20  
_diffrn_reflns_limit_k_max 11  
_diffrn_reflns_limit_l_max 38  
_diffrn_standards_number 3  
_diffrn_standards_interval_time 120  
_diffrn_standards_decay_% 0.00  
# 8. COMPUTING DATA  
_computing_data_collection CAD4_(Enraf-Nonius,_1977)  
_computing_cell_refinement CAD4_(Enraf-Nonius,_1977)  
_computing_data_reduction PROCESS_MolEN_(Fair,_1990)  
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'  
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'  
_computing_molecular_graphics ?  
_computing_publication_material ?  
_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 w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+40.0000P] 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 4894  
_refine_ls_number_parameters 235  
_refine_ls_number_restraints 0  
_refine_ls_R_factor_all 0.1522  

_refine_ls_R_factor_gt 0.0940  
_refine_ls_wR_factor_ref 0.1981  
_refine_ls_wR_factor_gt 0.1859  
_refine_ls_goodness_of_fit_ref 1.134  
_refine_ls_restrained_S_all 1.134  
_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_calc_flag  
_atom_site_refinement_flags  
_atom_site_disorder_assembly  
_atom_site_disorder_group  
Fe1 Fe 0.41150(6) 0.67140(11) 0.45992(3) 0.0342(3) Uani 1 d . . .  
C1 C 0.3704(5) 0.5839(9) 0.5017(3) 0.0431(19) Uani 1 d . . .  
O1 O 0.3414(4) 0.5240(8) 0.5274(2) 0.0704(19) Uani 1 d . . .  
C2 C 0.4456(4) 0.5185(10) 0.4379(2) 0.042(2) Uani 1 d . . .  
O2 O 0.4687(4) 0.4169(7) 0.4232(2) 0.068(2) Uani 1 d . . .  
C10 C 0.3964(5) 0.8752(10) 0.4808(3) 0.053(2) Uani 1 d . . .  
H10 H 0.3522 0.9044 0.4974 0.069 Uiso 1 calc R . .  
C11 C 0.3976(6) 0.8728(9) 0.4361(3) 0.061(3) Uani 1 d . . .  
H11 H 0.3540 0.9052 0.4157 0.080 Uiso 1 calc R . .  
C12 C 0.4691(6) 0.8181(10) 0.4247(3) 0.063(3) Uani 1 d . . .  
H12 H 0.4838 0.8006 0.3954 0.082 Uiso 1 calc R . .  
C13 C 0.5179(6) 0.7916(11) 0.4643(4) 0.067(3) Uani 1 d . . .  
H13 H 0.5727 0.7556 0.4669 0.088 Uiso 1 calc R . .  
C14 C 0.4736(6) 0.8261(10) 0.4974(3) 0.062(3) Uani 1 d . . .  
H14 H 0.4918 0.8185 0.5280 0.080 Uiso 1 calc R . .  
B1 B 0.3065(5) 0.6454(9) 0.4267(3) 0.040(2) Uani 1 d . . .  
F1 F 0.2421(3) 0.6787(7) 0.44742(15) 0.0712(18) Uani 1 d . . .  
Si1 Si 0.27608(11) 0.5791(2) 0.36508(6) 0.0283(4) Uani 1 d . . .  
Si2 Si 0.15374(12) 0.6936(2) 0.34703(7) 0.0371(5) Uani 1 d . . .  
C21 C 0.1132(6) 0.6702(13) 0.2886(3) 0.080(3) Uani 1 d . . .  
H21A H 0.0645 0.7259 0.2829 0.104 Uiso 1 calc R . .  
H21B H 0.1008 0.5719 0.2831 0.104 Uiso 1 calc R . .  
H21C H 0.1535 0.7009 0.2696 0.104 Uiso 1 calc R . .  
C22 C 0.1695(5) 0.8827(8) 0.3566(3) 0.052(2) Uani 1 d . . .  
H22A H 0.2071 0.9185 0.3368 0.067 Uiso 1 calc R . .  
H22B H 0.1914 0.8978 0.3864 0.067 Uiso 1 calc R . .  
H22C H 0.1184 0.9317 0.3516 0.067 Uiso 1 calc R . .  
C23 C 0.0766(5) 0.6343(10) 0.3835(3) 0.066(3) Uani 1 d . . .  
H23A H 0.1032 0.5876 0.4087 0.086 Uiso 1 calc R . .  
H23B H 0.0395 0.5695 0.3679 0.086 Uiso 1 calc R . .  
H23C H 0.0469 0.7151 0.3928 0.086 Uiso 1 calc R . .  
Si3 Si 0.25168(13) 0.3389(2) 0.37125(8) 0.0458(6) Uani 1 d . . .  
C31 C 0.3316(5) 0.2243(10) 0.3522(3) 0.064(3) Uani 1 d . . .  
H31A H 0.3158 0.1267 0.3546 0.083 Uiso 1 calc R . .  
H31B H 0.3818 0.2405 0.3700 0.083 Uiso 1 calc R . .  
H31C H 0.3391 0.2458 0.3221 0.083 Uiso 1 calc R . .  
C32 C 0.2413(8) 0.2971(11) 0.4301(4) 0.100(4) Uani 1 d . . .  
H32A H 0.2274 0.1987 0.4329 0.130 Uiso 1 calc R . .  
H32B H 0.1990 0.3549 0.4407 0.130 Uiso 1 calc R . .  
H32C H 0.2920 0.3162 0.4470 0.130 Uiso 1 calc R . .  
C33 C 0.1563(6) 0.2925(10) 0.3387(4) 0.079(4) Uani 1 d . . .  
H33A H 0.1635 0.3029 0.3080 0.103 Uiso 1 calc R . .  
H33B H 0.1134 0.3545 0.3465 0.103 Uiso 1 calc R . .  
H33C H 0.1421 0.1959 0.3446 0.103 Uiso 1 calc R . .  
Si4 Si 0.36266(12) 0.6238(2) 0.31146(7) 0.0373(5) Uani 1 d . . .  
C41 C 0.4648(5) 0.5490(11) 0.3225(3) 0.062(3) Uani 1 d . . .  
H41A H 0.4606 0.4490 0.3281 0.080 Uiso 1 calc R . .  
H41B H 0.4920 0.5948 0.3478 0.080 Uiso 1 calc R . .  
H41C H 0.4954 0.5638 0.2975 0.080 Uiso 1 calc R . .  
C42 C 0.3170(6) 0.5412(12) 0.2606(3) 0.067(3) Uani 1 d . . .  
H42A H 0.3518 0.5567 0.2374 0.087 Uiso 1 calc R . .  
H42B H 0.2644 0.5827 0.2528 0.087 Uiso 1 calc R . .  
H42C H 0.3109 0.4410 0.2652 0.087 Uiso 1 calc R . .  
C43 C 0.3744(6) 0.8152(10) 0.3019(3) 0.064(3) Uani 1 d . . .  
H43A H 0.3991 0.8297 0.2749 0.083 Uiso 1 calc R . .  
H43B H 0.4085 0.8558 0.3258 0.083 Uiso 1 calc R . .  
H43C H 0.3218 0.8600 0.3002 0.083 Uiso 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 0.0340(5) 0.0340(5) 0.0340(6) 0.0023(5) 0.0000(4) -0.0043(5)  
C1 0.051(5) 0.043(5) 0.035(4) 0.005(4) 0.002(4) -0.003(4)  
O1 0.090(5) 0.072(5) 0.051(4) 0.015(4) 0.012(4) -0.015(4)  
C2 0.029(4) 0.068(6) 0.028(4) 0.013(4) -0.009(3) 0.001(4)  
O2 0.076(4) 0.065(4) 0.062(4) -0.023(4) -0.009(3) 0.039(4)  
C10 0.059(5) 0.048(5) 0.054(5) -0.004(4) 0.012(4) -0.006(5)  
C11 0.075(6) 0.036(5) 0.070(7) 0.016(5) -0.014(5) -0.004(5)  
C12 0.084(7) 0.055(6) 0.053(6) 0.004(5) 0.025(5) -0.023(6)  
C13 0.051(5) 0.061(6) 0.089(8) 0.001(6) -0.002(5) -0.024(5)  
C14 0.073(6) 0.051(5) 0.059(5) -0.003(5) -0.006(5) -0.026(5)  
B1 0.040(5) 0.029(4) 0.051(5) 0.002(4) 0.010(4) 0.003(4)  
F1 0.041(2) 0.128(5) 0.044(3) -0.024(3) 0.004(2) 0.022(3)  
Si1 0.0245(9) 0.0260(9) 0.0338(10) -0.0002(8) 0.0001(7) -0.0004(8)  
Si2 0.0299(10) 0.0332(11) 0.0469(12) 0.0008(10) -0.0043(9) 0.0056(9)  
C21 0.060(6) 0.086(8) 0.087(7) -0.022(7) -0.033(5) 0.025(6)  
C22 0.054(5) 0.036(4) 0.065(6) 0.004(4) 0.002(4) 0.020(4)  
C23 0.045(5) 0.052(5) 0.104(8) 0.015(6) 0.028(5) 0.005(5)  
Si3 0.0401(12) 0.0281(11) 0.0695(16) 0.0000(11) 0.0062(11) -0.0051(10)  
C31 0.054(5) 0.042(5) 0.094(8) -0.006(5) -0.006(5) 0.008(5)  
C32 0.140(11) 0.052(7) 0.114(10) 0.029(7) 0.038(9) -0.022(8)  
C33 0.059(6) 0.044(5) 0.133(10) -0.026(6) -0.003(6) -0.016(5)  
Si4 0.0367(11) 0.0439(12) 0.0318(11) 0.0006(10) 0.0059(8) -0.0005(10)  
C41 0.038(4) 0.077(7) 0.072(6) 0.001(6) 0.015(4) 0.009(5)  
C42 0.083(7) 0.089(8) 0.029(4) -0.004(5) 0.004(4) -0.002(7)  
C43 0.084(7) 0.054(6) 0.054(5) 0.014(5) 0.011(5) -0.021(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 C2 1.739(10) . ?  
Fe1 C1 1.741(8) . ?  
Fe1 B1 1.983(9) . ?  
Fe1 C12 2.074(9) . ?  
Fe1 C11 2.079(9) . ?  
Fe1 C10 2.086(9) . ?  
Fe1 C14 2.110(9) . ?  
Fe1 C13 2.122(9) . ?  
C1 O1 1.129(9) . ?  
C2 O2 1.159(10) . ?  
C10 C11 1.393(12) . ?  
C10 C14 1.434(13) . ?  
C11 C12 1.384(13) . ?  
C12 C13 1.445(14) . ?  
C13 C14 1.361(13) . ?  
B1 F1 1.342(9) . ?  
B1 Si1 2.046(10) . ?  
Si1 Si4 2.344(3) . ?  
Si1 Si2 2.355(3) . ?  
Si1 Si3 2.356(3) . ?  
Si2 C22 1.858(9) . ?  
Si2 C23 1.881(8) . ?  
Si2 C21 1.902(10) . ?  
Si3 C31 1.871(9) . ?  
Si3 C33 1.875(10) . ?  
Si3 C32 1.898(12) . ?  
Si4 C41 1.864(8) . ?  
Si4 C43 1.876(9) . ?  
Si4 C42 1.876(9) . ?  
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  
C2 Fe1 C1 92.9(4) . . ?  
C2 Fe1 B1 89.8(3) . . ?  
C1 Fe1 B1 86.4(4) . . ?  
C2 Fe1 C12 100.5(4) . . ?  
C1 Fe1 C12 162.9(4) . . ?  
B1 Fe1 C12 104.1(4) . . ?  
C2 Fe1 C11 132.6(4) . . ?  
C1 Fe1 C11 132.6(4) . . ?  
B1 Fe1 C11 82.2(4) . . ?  
C12 Fe1 C11 38.9(4) . . ?  
C2 Fe1 C10 165.7(3) . . ?  
C1 Fe1 C10 98.9(4) . . ?  
B1 Fe1 C10 98.9(4) . . ?  
C12 Fe1 C10 66.5(4) . . ?  
C11 Fe1 C10 39.1(3) . . ?  
C2 Fe1 C14 130.5(4) . . ?  
C1 Fe1 C14 97.8(4) . . ?  
B1 Fe1 C14 138.9(4) . . ?  
C12 Fe1 C14 65.3(4) . . ?  
C11 Fe1 C14 64.9(4) . . ?  
C10 Fe1 C14 39.9(4) . . ?  
C2 Fe1 C13 100.5(4) . . ?  
C1 Fe1 C13 126.8(4) . . ?  
B1 Fe1 C13 144.0(4) . . ?  
C12 Fe1 C13 40.3(4) . . ?  
C11 Fe1 C13 65.4(4) . . ?  
C10 Fe1 C13 65.9(4) . . ?  
C14 Fe1 C13 37.5(4) . . ?  
O1 C1 Fe1 176.8(8) . . ?  
O2 C2 Fe1 179.7(7) . . ?  
C11 C10 C14 105.4(8) . . ?  
C11 C10 Fe1 70.2(5) . . ?  
C14 C10 Fe1 70.9(5) . . ?  
C12 C11 C10 110.4(9) . . ?  
C12 C11 Fe1 70.4(5) . . ?  
C10 C11 Fe1 70.8(6) . . ?  
C11 C12 C13 106.8(8) . . ?  
C11 C12 Fe1 70.7(5) . . ?  
C13 C12 Fe1 71.6(5) . . ?  
C14 C13 C12 107.3(9) . . ?  
C14 C13 Fe1 70.8(5) . . ?  
C12 C13 Fe1 68.1(5) . . ?  
C13 C14 C10 110.0(9) . . ?  
C13 C14 Fe1 71.7(6) . . ?  
C10 C14 Fe1 69.1(5) . . ?  
F1 B1 Fe1 115.8(6) . . ?  
F1 B1 Si1 112.2(6) . . ?  
Fe1 B1 Si1 132.0(4) . . ?  
B1 Si1 Si4 119.4(3) . . ?  
B1 Si1 Si2 102.8(3) . . ?  
Si4 Si1 Si2 108.94(11) . . ?  
B1 Si1 Si3 105.1(3) . . ?  
Si4 Si1 Si3 111.12(11) . . ?  
Si2 Si1 Si3 108.86(11) . . ?  
C22 Si2 C23 107.2(4) . . ?  
C22 Si2 C21 107.7(5) . . ?  
C23 Si2 C21 109.5(5) . . ?  
C22 Si2 Si1 108.0(3) . . ?  
C23 Si2 Si1 110.2(3) . . ?  
C21 Si2 Si1 114.0(3) . . ?  
C31 Si3 C33 106.9(4) . . ?  
C31 Si3 C32 108.0(5) . . ?  
C33 Si3 C32 109.1(6) . . ?  
C31 Si3 Si1 114.6(3) . . ?  
C33 Si3 Si1 109.6(4) . . ?  
C32 Si3 Si1 108.5(4) . . ?  
C41 Si4 C43 107.5(5) . . ?  
C41 Si4 C42 107.2(5) . . ?  
C43 Si4 C42 108.8(5) . . ?  
C41 Si4 Si1 114.4(3) . . ?  
C43 Si4 Si1 111.9(3) . . ?  
C42 Si4 Si1 106.8(3) . . ?  
_diffrn_measured_fraction_theta_max .936  
_diffrn_reflns_theta_full 25.98  
_diffrn_measured_fraction_theta_full .936  
_refine_diff_density_max .766  
_refine_diff_density_min -.604  
_refine_diff_density_rms .098