Electronic Supplementary Material for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_publ_section_title
;Tuning the Electronic Structure of Diboradiferrocenes
;
_publ_contact_author_address
;Rutgers University, Chemistry Department
73 Warren Street, Newark, NJ 07102, USA
;
_publ_contact_author_email fjaekle@rutgers.edu
_publ_contact_author_fax '(973) 353 1264'
_publ_contact_author_phone '(973) 353 5064 '
_publ_contact_author_name 'Prof. Frieder Jaekle'
loop_
_publ_author_name
F.Jaekle
R.A.Lalancette
T.Pakkirisamy
K.Venkatasubbaiah
# Attachment 'cif_all.cif'
data_2
_database_code_depnum_ccdc_archive 'CCDC 669587'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C20 H16 B2 Cl2 Fe2'
_chemical_formula_sum 'C20 H16 B2 Cl2 Fe2'
_chemical_formula_weight 460.55
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.1595(2)
_cell_length_b 12.9933(4)
_cell_length_c 14.0037(4)
_cell_angle_alpha 112.665(2)
_cell_angle_beta 97.722(2)
_cell_angle_gamma 95.855(2)
_cell_volume 1338.24(7)
_cell_formula_units_Z 3
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 8355
_cell_measurement_theta_min 3.74
_cell_measurement_theta_max 68.39
_exptl_crystal_description block
_exptl_crystal_colour red-brown
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.29
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.714
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 696
_exptl_absorpt_coefficient_mu 15.776
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.0480
_exptl_absorpt_correction_T_max 0.0917
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)'
_exptl_special_details
;
'crystal mounted on cryoloop using Paratone-N'
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART CCD area-detector'
_diffrn_measurement_method '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 0
_diffrn_reflns_number 8355
_diffrn_reflns_av_R_equivalents 0.0358
_diffrn_reflns_av_sigmaI/netI 0.0539
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 3.74
_diffrn_reflns_theta_max 68.39
_reflns_number_total 4409
_reflns_number_gt 4239
_reflns_threshold_expression I>2\s(I)
_publ_section_references
;
Bruker (2005). SAINT Version 7.23a. Bruker AXS Inc.,
Madison, Wisconsin, USA.
Bruker (2006). APEX 2 Version 2.0-2. Bruker AXS
Inc., Madison, Wisconsin, USA.
Sheldrick, G.M. (2001). SADABS. Version 2. University of
G\"ottingen, Germany.
Sheldrick, G. M. (2004). SHELXTL Version 6.14. Bruker AXS
Inc., Madison, Wisconsin, USA.
;
#====================================================================
_computing_data_collection 'APEX 2 (Bruker, 2006)'
_computing_cell_refinement 'APEX 2'
_computing_data_reduction 'SAINT (Bruker, 2005)'
_computing_structure_solution 'SHELXTL (Sheldrick, 2004)'
_computing_structure_refinement SHELXTL
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+1.2439P] 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 4409
_refine_ls_number_parameters 352
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0474
_refine_ls_R_factor_gt 0.0462
_refine_ls_wR_factor_ref 0.1211
_refine_ls_wR_factor_gt 0.1198
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_restrained_S_all 1.051
_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 0.86124(6) 0.74740(4) 0.02784(4) 0.01547(16) Uani 1 1 d . . .
Fe2 Fe 0.55496(6) 1.00720(4) 0.30645(4) 0.01530(16) Uani 1 1 d . . .
Fe3 Fe 0.80757(6) 0.57082(4) 0.37509(4) 0.01560(16) Uani 1 1 d . . .
Cl1 Cl 0.36063(10) 0.79009(7) -0.01096(6) 0.0251(2) Uani 1 1 d . . .
Cl2 Cl 1.05577(9) 0.97073(6) 0.34616(6) 0.02108(19) Uani 1 1 d . . .
Cl3 Cl 0.84840(11) 0.65721(7) 0.70355(6) 0.0269(2) Uani 1 1 d . . .
C1 C 0.7161(4) 0.8696(3) 0.0570(2) 0.0174(6) Uani 1 1 d . . .
C2 C 0.8714(4) 0.9082(2) 0.1358(2) 0.0173(6) Uani 1 1 d . . .
C3 C 1.0076(4) 0.9045(3) 0.0805(3) 0.0192(6) Uani 1 1 d . . .
H3 H 1.1295 0.9240 0.1131 0.023 Uiso 1 1 calc R . .
C4 C 0.9404(4) 0.8657(3) -0.0289(3) 0.0210(7) Uani 1 1 d . . .
H4 H 1.0072 0.8528 -0.0861 0.025 Uiso 1 1 calc R . .
C5 C 0.7627(4) 0.8444(3) -0.0435(3) 0.0206(7) Uani 1 1 d . . .
H5 H 0.6834 0.8151 -0.1127 0.025 Uiso 1 1 calc R . .
C6 C 0.7740(4) 0.5836(3) -0.0763(3) 0.0230(7) Uani 1 1 d . . .
H6 H 0.6968 0.5586 -0.1458 0.028 Uiso 1 1 calc R . .
C7 C 0.9512(4) 0.6058(3) -0.0586(3) 0.0214(7) Uani 1 1 d . . .
H7 H 1.0213 0.5993 -0.1133 0.026 Uiso 1 1 calc R . .
C8 C 1.0124(4) 0.6392(3) 0.0511(3) 0.0229(7) Uani 1 1 d . . .
H8 H 1.1330 0.6606 0.0866 0.027 Uiso 1 1 calc R . .
C9 C 0.8726(5) 0.6373(3) 0.1012(3) 0.0237(7) Uani 1 1 d . . .
H9 H 0.8773 0.6572 0.1781 0.028 Uiso 1 1 calc R . .
C10 C 0.7244(5) 0.6028(3) 0.0223(3) 0.0247(7) Uani 1 1 d . . .
H10 H 0.6065 0.5940 0.0340 0.030 Uiso 1 1 calc R . .
C11 C 0.5474(4) 0.8469(3) 0.1982(3) 0.0180(6) Uani 1 1 d . . .
C12 C 0.7027(4) 0.8854(2) 0.2769(2) 0.0174(6) Uani 1 1 d . . .
C13 C 0.6548(4) 0.9090(3) 0.3771(3) 0.0200(7) Uani 1 1 d . . .
H13 H 0.7339 0.9384 0.4464 0.024 Uiso 1 1 calc R . .
C14 C 0.4779(4) 0.8878(3) 0.3628(3) 0.0205(7) Uani 1 1 d . . .
H14 H 0.4113 0.8998 0.4200 0.025 Uiso 1 1 calc R . .
C15 C 0.4106(4) 0.8494(3) 0.2534(3) 0.0187(6) Uani 1 1 d . . .
H15 H 0.2886 0.8291 0.2207 0.022 Uiso 1 1 calc R . .
C16 C 0.6935(4) 1.1488(3) 0.3065(3) 0.0218(7) Uani 1 1 d . . .
H16 H 0.8118 1.1562 0.2951 0.026 Uiso 1 1 calc R . .
C17 C 0.6424(4) 1.1739(3) 0.4055(3) 0.0219(7) Uani 1 1 d . . .
H17 H 0.7186 1.2020 0.4757 0.026 Uiso 1 1 calc R . .
C18 C 0.4654(4) 1.1520(3) 0.3867(3) 0.0210(7) Uani 1 1 d . . .
H18 H 0.3944 1.1619 0.4416 0.025 Uiso 1 1 calc R . .
C19 C 0.4054(4) 1.1127(3) 0.2769(3) 0.0217(7) Uani 1 1 d . . .
H19 H 0.2849 1.0906 0.2410 0.026 Uiso 1 1 calc R . .
C20 C 0.5457(4) 1.1107(3) 0.2265(3) 0.0216(7) Uani 1 1 d . . .
H20 H 0.5417 1.0870 0.1492 0.026 Uiso 1 1 calc R . .
C21 C 0.9737(4) 0.6168(3) 0.5128(2) 0.0170(6) Uani 1 1 d . . .
C22 C 1.0447(4) 0.5493(3) 0.4229(2) 0.0185(6) Uani 1 1 d . . .
C23 C 1.0474(4) 0.6083(3) 0.3558(2) 0.0194(6) Uani 1 1 d . . .
H23 H 1.0872 0.5820 0.2871 0.023 Uiso 1 1 calc R . .
C24 C 0.9826(4) 0.7104(3) 0.4018(3) 0.0213(7) Uani 1 1 d . . .
H24 H 0.9684 0.7674 0.3709 0.026 Uiso 1 1 calc R . .
C25 C 0.9367(4) 0.7154(3) 0.4975(3) 0.0202(7) Uani 1 1 d . . .
H25 H 0.8851 0.7769 0.5456 0.024 Uiso 1 1 calc R . .
C26 C 0.5967(4) 0.4695(3) 0.3767(3) 0.0253(7) Uani 1 1 d . . .
H26 H 0.5819 0.4398 0.4317 0.030 Uiso 1 1 calc R . .
C27 C 0.6612(4) 0.4149(3) 0.2833(3) 0.0221(7) Uani 1 1 d . . .
H27 H 0.7005 0.3402 0.2615 0.027 Uiso 1 1 calc R . .
C28 C 0.6614(4) 0.4854(3) 0.2272(3) 0.0210(7) Uani 1 1 d . . .
H28 H 0.7002 0.4688 0.1588 0.025 Uiso 1 1 calc R . .
C29 C 0.5975(4) 0.5840(3) 0.2853(3) 0.0231(7) Uani 1 1 d . . .
H29 H 0.5824 0.6485 0.2646 0.028 Uiso 1 1 calc R . .
C30 C 0.5579(4) 0.5744(3) 0.3776(3) 0.0271(8) Uani 1 1 d . . .
H30 H 0.5102 0.6311 0.4333 0.033 Uiso 1 1 calc R . .
B2 B 0.8684(4) 0.9187(3) 0.2484(3) 0.0176(7) Uani 1 1 d . . .
B3 B 0.9296(4) 0.5711(3) 0.5932(3) 0.0178(7) Uani 1 1 d . . .
B1 B 0.5497(5) 0.8375(3) 0.0851(3) 0.0184(7) Uani 1 1 d . . .
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 0.0198(3) 0.0132(2) 0.0134(3) 0.0056(2) 0.00267(18) 0.00299(19)
Fe2 0.0199(3) 0.0128(2) 0.0125(2) 0.0047(2) 0.00231(18) 0.00232(19)
Fe3 0.0193(3) 0.0128(2) 0.0137(3) 0.0052(2) 0.00093(18) 0.00164(19)
Cl1 0.0226(4) 0.0321(4) 0.0160(4) 0.0063(3) -0.0001(3) 0.0033(3)
Cl2 0.0213(4) 0.0206(3) 0.0177(4) 0.0062(3) -0.0016(3) 0.0010(3)
Cl3 0.0369(4) 0.0268(4) 0.0176(4) 0.0061(3) 0.0104(3) 0.0132(3)
C1 0.0211(15) 0.0158(13) 0.0158(14) 0.0070(12) 0.0011(12) 0.0060(12)
C2 0.0182(14) 0.0125(13) 0.0187(15) 0.0033(12) 0.0037(12) 0.0039(11)
C3 0.0223(15) 0.0152(14) 0.0208(16) 0.0070(13) 0.0081(12) 0.0026(12)
C4 0.0285(17) 0.0171(14) 0.0217(16) 0.0108(13) 0.0083(13) 0.0052(13)
C5 0.0248(16) 0.0196(15) 0.0190(15) 0.0084(13) 0.0045(13) 0.0082(13)
C6 0.0299(17) 0.0156(14) 0.0196(16) 0.0049(13) -0.0012(13) 0.0030(13)
C7 0.0278(16) 0.0122(13) 0.0226(16) 0.0041(13) 0.0064(13) 0.0065(12)
C8 0.0263(16) 0.0145(14) 0.0266(17) 0.0094(14) -0.0020(13) 0.0033(12)
C9 0.0384(19) 0.0151(14) 0.0220(16) 0.0114(13) 0.0069(14) 0.0058(13)
C10 0.0286(17) 0.0179(15) 0.0302(18) 0.0126(15) 0.0069(14) 0.0015(13)
C11 0.0183(14) 0.0137(13) 0.0193(15) 0.0035(12) 0.0045(12) 0.0029(11)
C12 0.0222(15) 0.0130(13) 0.0168(14) 0.0057(12) 0.0025(12) 0.0052(12)
C13 0.0243(16) 0.0171(14) 0.0181(15) 0.0054(13) 0.0038(12) 0.0081(12)
C14 0.0267(17) 0.0171(14) 0.0197(16) 0.0090(13) 0.0069(13) 0.0035(13)
C15 0.0217(15) 0.0141(13) 0.0193(15) 0.0048(12) 0.0070(12) 0.0015(12)
C16 0.0206(15) 0.0157(14) 0.0305(17) 0.0111(14) 0.0048(13) 0.0023(12)
C17 0.0260(16) 0.0149(14) 0.0194(15) 0.0033(13) -0.0010(13) 0.0025(12)
C18 0.0258(16) 0.0152(14) 0.0226(16) 0.0066(13) 0.0077(13) 0.0062(12)
C19 0.0233(16) 0.0171(14) 0.0255(16) 0.0096(13) 0.0019(13) 0.0061(12)
C20 0.0279(16) 0.0174(14) 0.0234(16) 0.0121(13) 0.0052(13) 0.0046(13)
C21 0.0225(15) 0.0143(13) 0.0114(13) 0.0039(12) -0.0009(11) 0.0013(12)
C22 0.0177(14) 0.0196(15) 0.0152(14) 0.0052(12) -0.0008(11) 0.0028(12)
C23 0.0200(14) 0.0219(15) 0.0176(15) 0.0108(13) 0.0018(12) 0.0002(12)
C24 0.0233(15) 0.0163(14) 0.0220(16) 0.0091(13) -0.0022(13) -0.0040(12)
C25 0.0214(15) 0.0141(14) 0.0211(16) 0.0054(13) -0.0019(12) -0.0001(12)
C26 0.0246(16) 0.0279(17) 0.0233(17) 0.0116(15) 0.0053(13) -0.0019(14)
C27 0.0243(16) 0.0158(14) 0.0221(16) 0.0060(13) 0.0000(13) -0.0019(12)
C28 0.0209(15) 0.0212(15) 0.0152(14) 0.0050(13) -0.0027(12) -0.0033(12)
C29 0.0203(15) 0.0192(15) 0.0246(16) 0.0078(14) -0.0076(13) 0.0000(12)
C30 0.0223(16) 0.0236(16) 0.0292(18) 0.0044(15) 0.0051(14) 0.0014(13)
B2 0.0191(16) 0.0132(15) 0.0196(17) 0.0054(14) 0.0027(13) 0.0051(13)
B3 0.0189(16) 0.0211(17) 0.0118(15) 0.0053(13) 0.0014(12) 0.0042(13)
B1 0.0206(17) 0.0147(15) 0.0163(16) 0.0031(13) -0.0003(13) 0.0057(13)
_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 C1 2.026(3) . ?
Fe1 C2 2.038(3) . ?
Fe1 C6 2.045(3) . ?
Fe1 C7 2.046(3) . ?
Fe1 C5 2.047(3) . ?
Fe1 C8 2.049(3) . ?
Fe1 C10 2.054(4) . ?
Fe1 C3 2.059(3) . ?
Fe1 C9 2.060(3) . ?
Fe1 C4 2.070(3) . ?
Fe2 C12 2.037(3) . ?
Fe2 C11 2.039(3) . ?
Fe2 C19 2.046(3) . ?
Fe2 C18 2.051(3) . ?
Fe2 C20 2.056(3) . ?
Fe2 C17 2.056(3) . ?
Fe2 C16 2.058(3) . ?
Fe2 C13 2.059(3) . ?
Fe2 C15 2.060(3) . ?
Fe2 C14 2.075(3) . ?
Fe3 C21 2.039(3) . ?
Fe3 C22 2.043(3) . ?
Fe3 C23 2.047(3) . ?
Fe3 C30 2.047(4) . ?
Fe3 C29 2.048(3) . ?
Fe3 C25 2.050(3) . ?
Fe3 C28 2.059(3) . ?
Fe3 C26 2.065(4) . ?
Fe3 C27 2.067(3) . ?
Fe3 C24 2.067(3) . ?
Cl1 B1 1.783(3) . ?
Cl2 B2 1.784(3) . ?
Cl3 B3 1.781(4) . ?
C1 C5 1.430(5) . ?
C1 C2 1.463(4) . ?
C1 B1 1.526(5) . ?
C2 C3 1.431(5) . ?
C2 B2 1.533(5) . ?
C3 C4 1.423(5) . ?
C3 H3 1.0000 . ?
C4 C5 1.420(5) . ?
C4 H4 1.0000 . ?
C5 H5 1.0000 . ?
C6 C7 1.414(5) . ?
C6 C10 1.427(5) . ?
C6 H6 1.0000 . ?
C7 C8 1.425(5) . ?
C7 H7 1.0000 . ?
C8 C9 1.420(5) . ?
C8 H8 1.0000 . ?
C9 C10 1.426(5) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C11 C15 1.437(5) . ?
C11 C12 1.463(4) . ?
C11 B1 1.543(5) . ?
C12 C13 1.434(5) . ?
C12 B2 1.528(5) . ?
C13 C14 1.414(5) . ?
C13 H13 1.0000 . ?
C14 C15 1.424(5) . ?
C14 H14 1.0000 . ?
C15 H15 1.0000 . ?
C16 C17 1.426(5) . ?
C16 C20 1.430(5) . ?
C16 H16 1.0000 . ?
C17 C18 1.412(5) . ?
C17 H17 1.0000 . ?
C18 C19 1.417(5) . ?
C18 H18 1.0000 . ?
C19 C20 1.420(5) . ?
C19 H19 1.0000 . ?
C20 H20 1.0000 . ?
C21 C25 1.432(4) . ?
C21 C22 1.462(4) . ?
C21 B3 1.526(5) . ?
C22 C23 1.424(5) . ?
C22 B3 1.534(4) 2_766 ?
C23 C24 1.425(5) . ?
C23 H23 1.0000 . ?
C24 C25 1.418(5) . ?
C24 H24 1.0000 . ?
C25 H25 1.0000 . ?
C26 C30 1.426(5) . ?
C26 C27 1.428(5) . ?
C26 H26 1.0000 . ?
C27 C28 1.418(5) . ?
C27 H27 1.0000 . ?
C28 C29 1.422(5) . ?
C28 H28 1.0000 . ?
C29 C30 1.421(5) . ?
C29 H29 1.0000 . ?
C30 H30 1.0000 . ?
B3 C22 1.534(5) 2_766 ?
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 Fe1 C2 42.21(12) . . ?
C1 Fe1 C6 122.73(13) . . ?
C2 Fe1 C6 162.06(14) . . ?
C1 Fe1 C7 157.47(13) . . ?
C2 Fe1 C7 157.15(13) . . ?
C6 Fe1 C7 40.43(14) . . ?
C1 Fe1 C5 41.10(13) . . ?
C2 Fe1 C5 69.47(13) . . ?
C6 Fe1 C5 105.24(13) . . ?
C7 Fe1 C5 120.06(14) . . ?
C1 Fe1 C8 160.87(14) . . ?
C2 Fe1 C8 123.28(13) . . ?
C6 Fe1 C8 68.22(13) . . ?
C7 Fe1 C8 40.72(14) . . ?
C5 Fe1 C8 156.89(15) . . ?
C1 Fe1 C10 108.90(14) . . ?
C2 Fe1 C10 126.64(14) . . ?
C6 Fe1 C10 40.75(15) . . ?
C7 Fe1 C10 68.25(14) . . ?
C5 Fe1 C10 122.29(14) . . ?
C8 Fe1 C10 68.09(14) . . ?
C1 Fe1 C3 69.50(13) . . ?
C2 Fe1 C3 40.88(13) . . ?
C6 Fe1 C3 154.62(15) . . ?
C7 Fe1 C3 119.95(14) . . ?
C5 Fe1 C3 68.34(13) . . ?
C8 Fe1 C3 107.55(13) . . ?
C10 Fe1 C3 163.02(14) . . ?
C1 Fe1 C9 125.01(14) . . ?
C2 Fe1 C9 110.36(13) . . ?
C6 Fe1 C9 68.40(14) . . ?
C7 Fe1 C9 68.34(14) . . ?
C5 Fe1 C9 159.78(15) . . ?
C8 Fe1 C9 40.43(15) . . ?
C10 Fe1 C9 40.56(14) . . ?
C3 Fe1 C9 125.62(14) . . ?
C1 Fe1 C4 68.83(13) . . ?
C2 Fe1 C4 68.65(13) . . ?
C6 Fe1 C4 119.08(14) . . ?
C7 Fe1 C4 104.34(14) . . ?
C5 Fe1 C4 40.33(13) . . ?
C8 Fe1 C4 121.90(14) . . ?
C10 Fe1 C4 156.16(14) . . ?
C3 Fe1 C4 40.30(13) . . ?
C9 Fe1 C4 159.70(15) . . ?
C12 Fe2 C11 42.08(12) . . ?
C12 Fe2 C19 158.27(14) . . ?
C11 Fe2 C19 121.63(13) . . ?
C12 Fe2 C18 159.38(13) . . ?
C11 Fe2 C18 157.34(13) . . ?
C19 Fe2 C18 40.48(14) . . ?
C12 Fe2 C20 122.10(14) . . ?
C11 Fe2 C20 107.28(14) . . ?
C19 Fe2 C20 40.51(14) . . ?
C18 Fe2 C20 68.13(14) . . ?
C12 Fe2 C17 123.09(13) . . ?
C11 Fe2 C17 160.77(14) . . ?
C19 Fe2 C17 68.02(13) . . ?
C18 Fe2 C17 40.22(13) . . ?
C20 Fe2 C17 68.32(14) . . ?
C12 Fe2 C16 107.15(13) . . ?
C11 Fe2 C16 124.00(14) . . ?
C19 Fe2 C16 68.10(13) . . ?
C18 Fe2 C16 67.92(14) . . ?
C20 Fe2 C16 40.67(13) . . ?
C17 Fe2 C16 40.57(14) . . ?
C12 Fe2 C13 41.00(13) . . ?
C11 Fe2 C13 69.14(13) . . ?
C19 Fe2 C13 159.51(15) . . ?
C18 Fe2 C13 123.39(13) . . ?
C20 Fe2 C13 158.48(14) . . ?
C17 Fe2 C13 107.69(13) . . ?
C16 Fe2 C13 122.58(14) . . ?
C12 Fe2 C15 69.50(13) . . ?
C11 Fe2 C15 41.04(13) . . ?
C19 Fe2 C15 107.67(13) . . ?
C18 Fe2 C15 121.79(13) . . ?
C20 Fe2 C15 124.11(14) . . ?
C17 Fe2 C15 156.93(15) . . ?
C16 Fe2 C15 160.93(14) . . ?
C13 Fe2 C15 67.95(13) . . ?
C12 Fe2 C14 68.75(13) . . ?
C11 Fe2 C14 68.69(13) . . ?
C19 Fe2 C14 123.84(14) . . ?
C18 Fe2 C14 107.70(14) . . ?
C20 Fe2 C14 160.23(14) . . ?
C17 Fe2 C14 121.85(14) . . ?
C16 Fe2 C14 157.54(14) . . ?
C13 Fe2 C14 40.00(13) . . ?
C15 Fe2 C14 40.29(13) . . ?
C21 Fe3 C22 41.98(12) . . ?
C21 Fe3 C23 69.25(13) . . ?
C22 Fe3 C23 40.75(13) . . ?
C21 Fe3 C30 119.71(14) . . ?
C22 Fe3 C30 156.35(16) . . ?
C23 Fe3 C30 161.22(15) . . ?
C21 Fe3 C29 153.27(13) . . ?
C22 Fe3 C29 162.29(15) . . ?
C23 Fe3 C29 124.24(14) . . ?
C30 Fe3 C29 40.61(16) . . ?
C21 Fe3 C25 41.00(12) . . ?
C22 Fe3 C25 69.32(12) . . ?
C23 Fe3 C25 68.35(13) . . ?
C30 Fe3 C25 106.69(14) . . ?
C29 Fe3 C25 117.82(13) . . ?
C21 Fe3 C28 165.27(13) . . ?
C22 Fe3 C28 126.28(13) . . ?
C23 Fe3 C28 107.39(13) . . ?
C30 Fe3 C28 68.13(14) . . ?
C29 Fe3 C28 40.51(13) . . ?
C25 Fe3 C28 152.44(14) . . ?
C21 Fe3 C26 109.03(14) . . ?
C22 Fe3 C26 122.13(14) . . ?
C23 Fe3 C26 156.50(14) . . ?
C30 Fe3 C26 40.56(15) . . ?
C29 Fe3 C26 68.20(15) . . ?
C25 Fe3 C26 126.66(14) . . ?
C28 Fe3 C26 67.99(14) . . ?
C21 Fe3 C27 128.30(13) . . ?
C22 Fe3 C27 109.57(13) . . ?
C23 Fe3 C27 121.16(14) . . ?
C30 Fe3 C27 68.03(14) . . ?
C29 Fe3 C27 67.93(13) . . ?
C25 Fe3 C27 165.11(15) . . ?
C28 Fe3 C27 40.21(13) . . ?
C26 Fe3 C27 40.44(14) . . ?
C21 Fe3 C24 68.69(13) . . ?
C22 Fe3 C24 68.68(13) . . ?
C23 Fe3 C24 40.53(13) . . ?
C30 Fe3 C24 124.17(14) . . ?
C29 Fe3 C24 105.55(14) . . ?
C25 Fe3 C24 40.28(14) . . ?
C28 Fe3 C24 118.70(14) . . ?
C26 Fe3 C24 162.39(14) . . ?
C27 Fe3 C24 154.25(15) . . ?
C5 C1 C2 107.1(3) . . ?
C5 C1 B1 130.5(3) . . ?
C2 C1 B1 120.6(3) . . ?
C5 C1 Fe1 70.24(17) . . ?
C2 C1 Fe1 69.33(16) . . ?
B1 C1 Fe1 113.6(2) . . ?
C3 C2 C1 107.1(3) . . ?
C3 C2 B2 130.9(3) . . ?
C1 C2 B2 120.3(3) . . ?
C3 C2 Fe1 70.35(17) . . ?
C1 C2 Fe1 68.46(16) . . ?
B2 C2 Fe1 114.7(2) . . ?
C4 C3 C2 108.5(3) . . ?
C4 C3 Fe1 70.26(19) . . ?
C2 C3 Fe1 68.77(17) . . ?
C4 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
Fe1 C3 H3 125.7 . . ?
C5 C4 C3 108.5(3) . . ?
C5 C4 Fe1 68.96(19) . . ?
C3 C4 Fe1 69.43(19) . . ?
C5 C4 H4 125.7 . . ?
C3 C4 H4 125.7 . . ?
Fe1 C4 H4 125.7 . . ?
C4 C5 C1 108.7(3) . . ?
C4 C5 Fe1 70.71(18) . . ?
C1 C5 Fe1 68.66(18) . . ?
C4 C5 H5 125.6 . . ?
C1 C5 H5 125.6 . . ?
Fe1 C5 H5 125.6 . . ?
C7 C6 C10 108.1(3) . . ?
C7 C6 Fe1 69.82(18) . . ?
C10 C6 Fe1 69.95(19) . . ?
C7 C6 H6 125.9 . . ?
C10 C6 H6 125.9 . . ?
Fe1 C6 H6 125.9 . . ?
C6 C7 C8 108.0(3) . . ?
C6 C7 Fe1 69.75(18) . . ?
C8 C7 Fe1 69.76(17) . . ?
C6 C7 H7 126.0 . . ?
C8 C7 H7 126.0 . . ?
Fe1 C7 H7 126.0 . . ?
C9 C8 C7 108.3(3) . . ?
C9 C8 Fe1 70.20(18) . . ?
C7 C8 Fe1 69.52(18) . . ?
C9 C8 H8 125.8 . . ?
C7 C8 H8 125.8 . . ?
Fe1 C8 H8 125.8 . . ?
C8 C9 C10 107.6(3) . . ?
C8 C9 Fe1 69.37(18) . . ?
C10 C9 Fe1 69.48(19) . . ?
C8 C9 H9 126.2 . . ?
C10 C9 H9 126.2 . . ?
Fe1 C9 H9 126.2 . . ?
C9 C10 C6 108.0(3) . . ?
C9 C10 Fe1 70.0(2) . . ?
C6 C10 Fe1 69.3(2) . . ?
C9 C10 H10 126.0 . . ?
C6 C10 H10 126.0 . . ?
Fe1 C10 H10 126.0 . . ?
C15 C11 C12 107.2(3) . . ?
C15 C11 B1 130.7(3) . . ?
C12 C11 B1 120.4(3) . . ?
C15 C11 Fe2 70.27(17) . . ?
C12 C11 Fe2 68.89(16) . . ?
B1 C11 Fe2 114.5(2) . . ?
C13 C12 C11 106.7(3) . . ?
C13 C12 B2 131.2(3) . . ?
C11 C12 B2 120.3(3) . . ?
C13 C12 Fe2 70.32(17) . . ?
C11 C12 Fe2 69.03(16) . . ?
B2 C12 Fe2 113.5(2) . . ?
C14 C13 C12 109.2(3) . . ?
C14 C13 Fe2 70.62(19) . . ?
C12 C13 Fe2 68.68(18) . . ?
C14 C13 H13 125.4 . . ?
C12 C13 H13 125.4 . . ?
Fe2 C13 H13 125.4 . . ?
C13 C14 C15 108.4(3) . . ?
C13 C14 Fe2 69.39(19) . . ?
C15 C14 Fe2 69.3(2) . . ?
C13 C14 H14 125.8 . . ?
C15 C14 H14 125.8 . . ?
Fe2 C14 H14 125.8 . . ?
C14 C15 C11 108.4(3) . . ?
C14 C15 Fe2 70.42(18) . . ?
C11 C15 Fe2 68.69(17) . . ?
C14 C15 H15 125.8 . . ?
C11 C15 H15 125.8 . . ?
Fe2 C15 H15 125.8 . . ?
C17 C16 C20 107.9(3) . . ?
C17 C16 Fe2 69.6(2) . . ?
C20 C16 Fe2 69.57(19) . . ?
C17 C16 H16 126.1 . . ?
C20 C16 H16 126.1 . . ?
Fe2 C16 H16 126.1 . . ?
C18 C17 C16 108.0(3) . . ?
C18 C17 Fe2 69.72(18) . . ?
C16 C17 Fe2 69.81(18) . . ?
C18 C17 H17 126.0 . . ?
C16 C17 H17 126.0 . . ?
Fe2 C17 H17 126.0 . . ?
C17 C18 C19 108.3(3) . . ?
C17 C18 Fe2 70.06(18) . . ?
C19 C18 Fe2 69.54(17) . . ?
C17 C18 H18 125.8 . . ?
C19 C18 H18 125.8 . . ?
Fe2 C18 H18 125.8 . . ?
C18 C19 C20 108.3(3) . . ?
C18 C19 Fe2 69.98(18) . . ?
C20 C19 Fe2 70.13(18) . . ?
C18 C19 H19 125.8 . . ?
C20 C19 H19 125.8 . . ?
Fe2 C19 H19 125.8 . . ?
C19 C20 C16 107.5(3) . . ?
C19 C20 Fe2 69.36(19) . . ?
C16 C20 Fe2 69.76(19) . . ?
C19 C20 H20 126.3 . . ?
C16 C20 H20 126.3 . . ?
Fe2 C20 H20 126.3 . . ?
C25 C21 C22 107.1(3) . . ?
C25 C21 B3 131.0(3) . . ?
C22 C21 B3 121.3(3) . . ?
C25 C21 Fe3 69.93(17) . . ?
C22 C21 Fe3 69.16(16) . . ?
B3 C21 Fe3 118.9(2) . . ?
C23 C22 C21 107.1(3) . . ?
C23 C22 B3 132.3(3) . 2_766 ?
C21 C22 B3 119.6(3) . 2_766 ?
C23 C22 Fe3 69.75(17) . . ?
C21 C22 Fe3 68.86(16) . . ?
B3 C22 Fe3 117.1(2) 2_766 . ?
C22 C23 C24 109.0(3) . . ?
C22 C23 Fe3 69.50(18) . . ?
C24 C23 Fe3 70.51(19) . . ?
C22 C23 H23 125.5 . . ?
C24 C23 H23 125.5 . . ?
Fe3 C23 H23 125.5 . . ?
C25 C24 C23 108.1(3) . . ?
C25 C24 Fe3 69.23(18) . . ?
C23 C24 Fe3 68.96(19) . . ?
C25 C24 H24 125.9 . . ?
C23 C24 H24 125.9 . . ?
Fe3 C24 H24 125.9 . . ?
C24 C25 C21 108.8(3) . . ?
C24 C25 Fe3 70.50(18) . . ?
C21 C25 Fe3 69.08(17) . . ?
C24 C25 H25 125.6 . . ?
C21 C25 H25 125.6 . . ?
Fe3 C25 H25 125.6 . . ?
C30 C26 C27 107.5(3) . . ?
C30 C26 Fe3 69.0(2) . . ?
C27 C26 Fe3 69.8(2) . . ?
C30 C26 H26 126.3 . . ?
C27 C26 H26 126.3 . . ?
Fe3 C26 H26 126.3 . . ?
C28 C27 C26 108.2(3) . . ?
C28 C27 Fe3 69.59(18) . . ?
C26 C27 Fe3 69.73(19) . . ?
C28 C27 H27 125.9 . . ?
C26 C27 H27 125.9 . . ?
Fe3 C27 H27 125.9 . . ?
C27 C28 C29 108.1(3) . . ?
C27 C28 Fe3 70.20(18) . . ?
C29 C28 Fe3 69.35(17) . . ?
C27 C28 H28 125.9 . . ?
C29 C28 H28 125.9 . . ?
Fe3 C28 H28 125.9 . . ?
C30 C29 C28 108.0(3) . . ?
C30 C29 Fe3 69.67(19) . . ?
C28 C29 Fe3 70.14(18) . . ?
C30 C29 H29 126.0 . . ?
C28 C29 H29 126.0 . . ?
Fe3 C29 H29 126.0 . . ?
C29 C30 C26 108.2(3) . . ?
C29 C30 Fe3 69.72(19) . . ?
C26 C30 Fe3 70.4(2) . . ?
C29 C30 H30 125.9 . . ?
C26 C30 H30 125.9 . . ?
Fe3 C30 H30 125.9 . . ?
C12 B2 C2 119.4(3) . . ?
C12 B2 Cl2 120.0(3) . . ?
C2 B2 Cl2 120.6(3) . . ?
C21 B3 C22 119.2(3) . 2_766 ?
C21 B3 Cl3 120.0(2) . . ?
C22 B3 Cl3 120.9(3) 2_766 . ?
C1 B1 C11 119.0(3) . . ?
C1 B1 Cl1 120.6(3) . . ?
C11 B1 Cl1 120.4(3) . . ?
_diffrn_measured_fraction_theta_max 0.895
_diffrn_reflns_theta_full 68.39
_diffrn_measured_fraction_theta_full 0.895
_refine_diff_density_max 1.465
_refine_diff_density_min -0.607
_refine_diff_density_rms 0.124
#===END
data_3Mes
_database_code_depnum_ccdc_archive 'CCDC 669588'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C38 H38 B2 Fe2, C H Cl3'
_chemical_formula_sum 'C39 H39 B2 Cl3 Fe2'
_chemical_formula_weight 747.37
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.2730(2)
_cell_length_b 11.9306(2)
_cell_length_c 14.7300(2)
_cell_angle_alpha 90.4950(10)
_cell_angle_beta 103.3200(10)
_cell_angle_gamma 114.8210(10)
_cell_volume 1737.22(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 5483
_cell_measurement_theta_min 4.11
_cell_measurement_theta_max 64.31
_exptl_crystal_description BLADE
_exptl_crystal_colour RED
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.429
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 772
_exptl_absorpt_coefficient_mu 9.018
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.188
_exptl_absorpt_correction_T_max 0.582
_exptl_absorpt_process_details '(SADABS; Blessing, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART CCD area-detector'
_diffrn_measurement_method '\f and \w'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 10934
_diffrn_reflns_av_R_equivalents 0.0399
_diffrn_reflns_av_sigmaI/netI 0.0425
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 3.11
_diffrn_reflns_theta_max 59.99
_reflns_number_total 4720
_reflns_number_gt 3856
_reflns_threshold_expression >2sigma(I)
_publ_section_references
;
Bruker (2005). SAINT Version 7.23a. Bruker AXS Inc.,
Madison, Wisconsin, USA.
Bruker (2006). APEX 2 Version 2.0-2. Bruker AXS
Inc., Madison, Wisconsin, USA.
Sheldrick, G.M. (2001). SADABS. Version 2. University of
G\"ottingen, Germany.
Sheldrick, G. M. (2004). SHELXTL Version 6.14. Bruker AXS
Inc., Madison, Wisconsin, USA.
;
#====================================================================
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement SMART
_computing_data_reduction 'SAINT-Plus (Bruker, 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SHELXTL (Bruker, 2000)'
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
one solvent chloroform (CDCl3) molecule is present in the asymmetric unit,
in which two chlorine and one carbon atom are disordered over two positions.
The disordered atoms are well behaved and thus are refined anisotropically.
The occupancy factors for the major domain of the CHCl3 site refined to 0.643.
;
_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^)+(0.0999P)^2^+1.3226P] 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 4720
_refine_ls_number_parameters 449
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0660
_refine_ls_R_factor_gt 0.0528
_refine_ls_wR_factor_ref 0.1595
_refine_ls_wR_factor_gt 0.1468
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_restrained_S_all 1.062
_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
B1 B 0.9322(5) 0.9258(5) 0.3996(4) 0.0317(12) Uani 1 1 d . . .
B2 B 0.0998(5) 0.6170(4) -0.0340(3) 0.0261(11) Uani 1 1 d . . .
C1 C 0.9650(6) 0.6681(5) 0.5252(4) 0.0462(13) Uani 1 1 d . . .
H1 H 0.8897 0.6299 0.4669 0.055 Uiso 1 1 calc R . .
C2 C 1.0915(5) 0.6630(5) 0.5449(4) 0.0427(13) Uani 1 1 d . . .
H2 H 1.1223 0.6221 0.5017 0.051 Uiso 1 1 calc R . .
C3 C 1.1672(5) 0.7267(5) 0.6341(4) 0.0406(12) Uani 1 1 d . . .
H3 H 1.2609 0.7386 0.6658 0.049 Uiso 1 1 calc R . .
C4 C 1.0884(5) 0.7705(5) 0.6717(4) 0.0435(13) Uani 1 1 d . . .
H4 H 1.1163 0.8184 0.7350 0.052 Uiso 1 1 calc R . .
C5 C 0.9637(5) 0.7342(5) 0.6058(4) 0.0464(13) Uani 1 1 d . . .
H5 H 0.8870 0.7515 0.6139 0.056 Uiso 1 1 calc R . .
C6 C 1.0790(5) 0.9561(4) 0.4522(3) 0.0326(10) Uani 1 1 d . . .
C7 C 1.1713(5) 0.9123(5) 0.4300(3) 0.0383(12) Uani 1 1 d . . .
H7 H 1.1555 0.8608 0.3707 0.046 Uiso 1 1 calc R . .
C8 C 1.2888(5) 0.9536(5) 0.5077(4) 0.0379(11) Uani 1 1 d . . .
H8 H 1.3686 0.9354 0.5120 0.046 Uiso 1 1 calc R . .
C9 C 1.2712(5) 1.0213(4) 0.5780(3) 0.0336(11) Uani 1 1 d . . .
H9 H 1.3370 1.0593 0.6405 0.040 Uiso 1 1 calc R . .
C10 C 1.1429(4) 1.0264(4) 0.5461(3) 0.0302(10) Uani 1 1 d . . .
C11 C 0.8641(4) 0.8548(4) 0.2975(3) 0.0311(10) Uani 1 1 d . . .
C12 C 0.9211(5) 0.9030(4) 0.2217(3) 0.0323(11) Uani 1 1 d . . .
C13 C 0.8575(5) 0.8429(4) 0.1307(3) 0.0324(10) Uani 1 1 d . . .
H13 H 0.8979 0.8767 0.0813 0.039 Uiso 1 1 calc R . .
C14 C 0.7360(5) 0.7343(5) 0.1095(4) 0.0383(12) Uani 1 1 d . . .
C15 C 0.6820(5) 0.6868(5) 0.1831(4) 0.0394(12) Uani 1 1 d . . .
H15 H 0.6005 0.6123 0.1705 0.047 Uiso 1 1 calc R . .
C16 C 0.7424(5) 0.7442(4) 0.2757(3) 0.0344(11) Uani 1 1 d . . .
C17 C 1.0483(5) 1.0218(5) 0.2351(4) 0.0416(12) Uani 1 1 d . . .
H17A H 1.1241 1.0023 0.2337 0.062 Uiso 1 1 calc R . .
H17B H 1.0670 1.0686 0.2958 0.062 Uiso 1 1 calc R . .
H17C H 1.0366 1.0720 0.1845 0.062 Uiso 1 1 calc R . .
C18 C 0.6680(6) 0.6769(6) 0.0097(4) 0.0560(16) Uani 1 1 d . . .
H18A H 0.5940 0.5949 0.0081 0.084 Uiso 1 1 calc R . .
H18B H 0.7338 0.6679 -0.0196 0.084 Uiso 1 1 calc R . .
H18C H 0.6319 0.7304 -0.0249 0.084 Uiso 1 1 calc R . .
C19 C 0.6732(5) 0.6820(5) 0.3507(4) 0.0447(13) Uani 1 1 d . . .
H19A H 0.7324 0.7226 0.4129 0.067 Uiso 1 1 calc R . .
H19B H 0.6546 0.5939 0.3453 0.067 Uiso 1 1 calc R . .
H19C H 0.5880 0.6892 0.3422 0.067 Uiso 1 1 calc R . .
C20 C 0.0474(5) 0.6595(4) 0.2137(3) 0.0341(11) Uani 1 1 d . . .
H20 H -0.0363 0.6595 0.1720 0.041 Uiso 1 1 calc R . .
C21 C 0.1817(5) 0.7477(4) 0.2206(3) 0.0348(11) Uani 1 1 d . . .
H21 H 0.2095 0.8208 0.1844 0.042 Uiso 1 1 calc R . .
C22 C 0.2698(5) 0.7148(4) 0.2873(3) 0.0376(11) Uani 1 1 d . . .
H22 H 0.3707 0.7607 0.3068 0.045 Uiso 1 1 calc R . .
C23 C 0.1898(5) 0.6051(5) 0.3223(3) 0.0385(12) Uani 1 1 d . . .
H23 H 0.2243 0.5603 0.3708 0.046 Uiso 1 1 calc R . .
C24 C 0.0524(5) 0.5718(5) 0.2768(3) 0.0373(12) Uani 1 1 d . . .
H24 H -0.0274 0.4985 0.2871 0.045 Uiso 1 1 calc R . .
C25 C 0.1489(4) 0.5427(4) 0.0394(3) 0.0269(10) Uani 1 1 d . . .
C26 C 0.2811(4) 0.5715(4) 0.0975(3) 0.0279(10) Uani 1 1 d . . .
H26 H 0.3667 0.6436 0.0939 0.033 Uiso 1 1 calc R . .
C27 C 0.2709(5) 0.4817(4) 0.1619(3) 0.0316(10) Uani 1 1 d . . .
H27 H 0.3477 0.4796 0.2108 0.038 Uiso 1 1 calc R . .
C28 C 0.1322(5) 0.3964(4) 0.1455(3) 0.0317(10) Uani 1 1 d . . .
H28 H 0.0952 0.3242 0.1813 0.038 Uiso 1 1 calc R . .
C29 C 0.0539(4) 0.4320(4) 0.0700(3) 0.0277(10) Uani 1 1 d . . .
C30 C 0.2037(4) 0.7368(4) -0.0658(3) 0.0288(10) Uani 1 1 d . . .
C31 C 0.3002(4) 0.7318(4) -0.1108(3) 0.0289(10) Uani 1 1 d . . .
C32 C 0.3924(4) 0.8402(4) -0.1350(3) 0.0325(11) Uani 1 1 d . . .
H32 H 0.4579 0.8354 -0.1635 0.039 Uiso 1 1 calc R . .
C33 C 0.3931(4) 0.9561(4) -0.1191(3) 0.0341(11) Uani 1 1 d . . .
C34 C 0.2968(4) 0.9591(4) -0.0752(3) 0.0322(10) Uani 1 1 d . . .
H34 H 0.2953 1.0366 -0.0626 0.039 Uiso 1 1 calc R . .
C35 C 0.2031(4) 0.8531(4) -0.0493(3) 0.0304(10) Uani 1 1 d . . .
C36 C 0.3042(5) 0.6105(4) -0.1356(4) 0.0359(11) Uani 1 1 d . . .
H36A H 0.2432 0.5723 -0.1978 0.054 Uiso 1 1 calc R . .
H36B H 0.2754 0.5542 -0.0888 0.054 Uiso 1 1 calc R . .
H36C H 0.3967 0.6264 -0.1362 0.054 Uiso 1 1 calc R . .
C37 C 0.4913(5) 1.0719(5) -0.1463(4) 0.0444(13) Uani 1 1 d . . .
H37A H 0.4447 1.1220 -0.1730 0.067 Uiso 1 1 calc R . .
H37B H 0.5297 1.0500 -0.1931 0.067 Uiso 1 1 calc R . .
H37C H 0.5641 1.1199 -0.0906 0.067 Uiso 1 1 calc R . .
C38 C 0.1066(5) 0.8694(4) -0.0011(3) 0.0360(11) Uani 1 1 d . . .
H38A H 0.1552 0.9445 0.0444 0.054 Uiso 1 1 calc R . .
H38B H 0.0676 0.7969 0.0317 0.054 Uiso 1 1 calc R . .
H38C H 0.0341 0.8775 -0.0479 0.054 Uiso 1 1 calc R . .
C39 C 0.5963(10) 0.8008(10) 0.6071(8) 0.054(3) Uani 0.643(4) 1 d P . .
H39 H 0.6736 0.8486 0.5795 0.064 Uiso 0.643(4) 1 calc PR . .
C39A C 0.588(2) 0.726(2) 0.5928(15) 0.063(5) Uani 0.357(4) 1 d P . .
H39A H 0.6702 0.7925 0.5791 0.076 Uiso 0.357(4) 1 calc PR . .
Cl1 Cl 0.45176(16) 0.72526(16) 0.51632(13) 0.0715(5) Uani 1 1 d . . .
Cl2 Cl 0.6346(3) 0.6942(3) 0.6746(3) 0.1025(18) Uani 0.643(4) 1 d P . .
Cl3 Cl 0.5747(2) 0.9052(3) 0.67749(16) 0.0656(9) Uani 0.643(4) 1 d P . .
Cl2A Cl 0.6015(8) 0.7510(9) 0.7121(5) 0.123(3) Uani 0.357(4) 1 d P . .
Cl3A Cl 0.5899(5) 0.5828(5) 0.5667(4) 0.0785(19) Uani 0.357(4) 1 d P . .
Fe1 Fe 1.11761(7) 0.84536(7) 0.54945(5) 0.0317(2) Uani 1 1 d . . .
Fe2 Fe 0.15776(6) 0.57296(6) 0.17948(5) 0.0262(2) Uani 1 1 d . . .
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
B1 0.037(3) 0.024(3) 0.030(3) 0.007(2) 0.011(2) 0.008(2)
B2 0.034(3) 0.019(2) 0.024(3) -0.002(2) 0.010(2) 0.010(2)
C1 0.052(3) 0.028(3) 0.044(3) 0.002(2) 0.003(3) 0.009(2)
C2 0.056(3) 0.032(3) 0.045(3) 0.007(2) 0.018(3) 0.021(3)
C3 0.045(3) 0.043(3) 0.034(3) 0.014(2) 0.009(2) 0.019(2)
C4 0.056(3) 0.039(3) 0.029(3) 0.009(2) 0.015(2) 0.013(3)
C5 0.047(3) 0.034(3) 0.063(4) 0.016(3) 0.030(3) 0.014(2)
C6 0.038(3) 0.034(3) 0.028(3) 0.005(2) 0.011(2) 0.016(2)
C7 0.045(3) 0.041(3) 0.032(3) 0.005(2) 0.014(2) 0.020(2)
C8 0.033(2) 0.045(3) 0.039(3) 0.009(2) 0.012(2) 0.019(2)
C9 0.032(2) 0.033(3) 0.030(3) 0.002(2) 0.006(2) 0.009(2)
C10 0.031(2) 0.025(2) 0.028(3) 0.0028(19) 0.0065(19) 0.006(2)
C11 0.032(2) 0.033(2) 0.029(3) 0.001(2) 0.006(2) 0.016(2)
C12 0.032(2) 0.033(3) 0.035(3) 0.004(2) 0.008(2) 0.018(2)
C13 0.040(3) 0.039(3) 0.026(3) 0.005(2) 0.008(2) 0.024(2)
C14 0.043(3) 0.041(3) 0.036(3) -0.003(2) 0.002(2) 0.028(3)
C15 0.032(2) 0.035(3) 0.048(3) -0.009(2) 0.001(2) 0.016(2)
C16 0.031(2) 0.035(3) 0.037(3) 0.002(2) 0.007(2) 0.015(2)
C17 0.048(3) 0.045(3) 0.031(3) 0.007(2) 0.014(2) 0.016(3)
C18 0.056(3) 0.055(4) 0.045(3) -0.018(3) -0.013(3) 0.027(3)
C19 0.042(3) 0.035(3) 0.050(3) 0.000(2) 0.016(2) 0.008(2)
C20 0.035(3) 0.037(3) 0.031(3) -0.003(2) 0.008(2) 0.017(2)
C21 0.043(3) 0.026(2) 0.032(3) 0.001(2) 0.011(2) 0.012(2)
C22 0.034(3) 0.038(3) 0.032(3) -0.004(2) 0.006(2) 0.009(2)
C23 0.049(3) 0.044(3) 0.021(3) 0.005(2) 0.009(2) 0.020(3)
C24 0.038(3) 0.036(3) 0.033(3) 0.000(2) 0.018(2) 0.007(2)
C25 0.030(2) 0.026(2) 0.025(2) 0.0028(19) 0.0109(19) 0.009(2)
C26 0.028(2) 0.026(2) 0.030(3) 0.007(2) 0.0108(19) 0.0097(19)
C27 0.030(2) 0.032(2) 0.036(3) 0.005(2) 0.006(2) 0.017(2)
C28 0.037(2) 0.027(2) 0.034(3) 0.009(2) 0.011(2) 0.014(2)
C29 0.034(2) 0.026(2) 0.026(3) 0.0049(19) 0.0087(19) 0.015(2)
C30 0.030(2) 0.028(2) 0.025(2) 0.0052(19) 0.0066(19) 0.010(2)
C31 0.027(2) 0.029(2) 0.026(3) 0.007(2) 0.0046(19) 0.010(2)
C32 0.026(2) 0.032(3) 0.033(3) 0.005(2) 0.008(2) 0.007(2)
C33 0.025(2) 0.036(3) 0.028(3) 0.005(2) -0.0006(19) 0.005(2)
C34 0.034(2) 0.026(2) 0.031(3) 0.006(2) 0.003(2) 0.011(2)
C35 0.032(2) 0.029(2) 0.026(3) 0.006(2) 0.0043(19) 0.011(2)
C36 0.032(2) 0.037(3) 0.038(3) 0.007(2) 0.013(2) 0.013(2)
C37 0.041(3) 0.037(3) 0.044(3) 0.013(2) 0.005(2) 0.009(2)
C38 0.040(3) 0.029(2) 0.039(3) 0.007(2) 0.010(2) 0.014(2)
C39 0.034(5) 0.053(6) 0.073(8) 0.028(6) 0.014(4) 0.017(5)
C39A 0.073(13) 0.074(15) 0.057(13) 0.029(12) 0.027(10) 0.040(13)
Cl1 0.0560(9) 0.0709(10) 0.0779(12) 0.0054(9) 0.0012(8) 0.0266(8)
Cl2 0.0446(14) 0.094(2) 0.142(4) 0.087(3) 0.0076(18) 0.0129(15)
Cl3 0.0485(13) 0.0847(18) 0.0469(14) -0.0024(12) 0.0191(10) 0.0100(12)
Cl2A 0.087(4) 0.176(8) 0.076(4) -0.027(5) 0.027(3) 0.025(5)
Cl3A 0.083(3) 0.070(3) 0.111(5) 0.040(3) 0.060(3) 0.041(3)
Fe1 0.0359(4) 0.0322(4) 0.0263(4) 0.0016(3) 0.0074(3) 0.0146(3)
Fe2 0.0259(4) 0.0265(4) 0.0235(4) 0.0050(3) 0.0064(3) 0.0087(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
B1 C6 1.541(7) . ?
B1 C10 1.546(7) 2_776 ?
B1 C11 1.571(7) . ?
B2 C29 1.531(7) 2_565 ?
B2 C25 1.554(7) . ?
B2 C30 1.579(7) . ?
C1 C2 1.415(8) . ?
C1 C5 1.426(8) . ?
C1 Fe1 2.052(5) . ?
C1 H1 1.0000 . ?
C2 C3 1.398(7) . ?
C2 Fe1 2.068(5) . ?
C2 H2 1.0000 . ?
C3 C4 1.408(7) . ?
C3 Fe1 2.060(5) . ?
C3 H3 1.0000 . ?
C4 C5 1.400(8) . ?
C4 Fe1 2.050(5) . ?
C4 H4 1.0000 . ?
C5 Fe1 2.052(5) . ?
C5 H5 1.0000 . ?
C6 C7 1.439(7) . ?
C6 C10 1.467(6) . ?
C6 Fe1 2.053(5) . ?
C7 C8 1.432(7) . ?
C7 Fe1 2.052(5) . ?
C7 H7 1.0000 . ?
C8 C9 1.406(7) . ?
C8 Fe1 2.058(5) . ?
C8 H8 1.0000 . ?
C9 C10 1.442(7) . ?
C9 Fe1 2.044(5) . ?
C9 H9 1.0000 . ?
C10 B1 1.546(7) 2_776 ?
C10 Fe1 2.059(4) . ?
C11 C16 1.413(6) . ?
C11 C12 1.421(7) . ?
C12 C13 1.391(7) . ?
C12 C17 1.505(7) . ?
C13 C14 1.399(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(7) . ?
C14 C18 1.497(7) . ?
C15 C16 1.399(7) . ?
C15 H15 0.9500 . ?
C16 C19 1.518(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.414(7) . ?
C20 C24 1.415(7) . ?
C20 Fe2 2.056(4) . ?
C20 H20 1.0000 . ?
C21 C22 1.410(7) . ?
C21 Fe2 2.053(5) . ?
C21 H21 1.0000 . ?
C22 C23 1.424(7) . ?
C22 Fe2 2.054(5) . ?
C22 H22 1.0000 . ?
C23 C24 1.417(7) . ?
C23 Fe2 2.055(5) . ?
C23 H23 1.0000 . ?
C24 Fe2 2.058(4) . ?
C24 H24 1.0000 . ?
C25 C26 1.432(6) . ?
C25 C29 1.463(6) . ?
C25 Fe2 2.065(4) . ?
C26 C27 1.423(6) . ?
C26 Fe2 2.046(4) . ?
C26 H26 1.0000 . ?
C27 C28 1.422(6) . ?
C27 Fe2 2.047(4) . ?
C27 H27 1.0000 . ?
C28 C29 1.438(6) . ?
C28 Fe2 2.044(4) . ?
C28 H28 1.0000 . ?
C29 B2 1.531(7) 2_565 ?
C29 Fe2 2.057(4) . ?
C30 C35 1.411(6) . ?
C30 C31 1.418(6) . ?
C31 C32 1.389(6) . ?
C31 C36 1.511(6) . ?
C32 C33 1.396(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.397(7) . ?
C33 C37 1.492(7) . ?
C34 C35 1.391(6) . ?
C34 H34 0.9500 . ?
C35 C38 1.501(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 Cl1 1.731(11) . ?
C39 Cl3 1.742(12) . ?
C39 Cl2 1.754(10) . ?
C39 H39 1.0000 . ?
C39A Cl1 1.68(2) . ?
C39A Cl2A 1.74(2) . ?
C39A Cl3A 1.75(2) . ?
C39A H39A 1.0000 . ?
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
C6 B1 C10 114.9(4) . 2_776 ?
C6 B1 C11 122.9(4) . . ?
C10 B1 C11 122.1(4) 2_776 . ?
C29 B2 C25 115.4(4) 2_565 . ?
C29 B2 C30 123.4(4) 2_565 . ?
C25 B2 C30 121.1(4) . . ?
C2 C1 C5 107.0(5) . . ?
C2 C1 Fe1 70.5(3) . . ?
C5 C1 Fe1 69.7(3) . . ?
C2 C1 H1 126.5 . . ?
C5 C1 H1 126.5 . . ?
Fe1 C1 H1 126.5 . . ?
C3 C2 C1 108.5(4) . . ?
C3 C2 Fe1 69.9(3) . . ?
C1 C2 Fe1 69.3(3) . . ?
C3 C2 H2 125.7 . . ?
C1 C2 H2 125.7 . . ?
Fe1 C2 H2 125.7 . . ?
C2 C3 C4 108.2(5) . . ?
C2 C3 Fe1 70.5(3) . . ?
C4 C3 Fe1 69.6(3) . . ?
C2 C3 H3 125.9 . . ?
C4 C3 H3 125.9 . . ?
Fe1 C3 H3 125.9 . . ?
C5 C4 C3 108.3(5) . . ?
C5 C4 Fe1 70.1(3) . . ?
C3 C4 Fe1 70.4(3) . . ?
C5 C4 H4 125.8 . . ?
C3 C4 H4 125.8 . . ?
Fe1 C4 H4 125.8 . . ?
C4 C5 C1 108.0(5) . . ?
C4 C5 Fe1 70.0(3) . . ?
C1 C5 Fe1 69.6(3) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 126.0 . . ?
C7 C6 C10 107.1(4) . . ?
C7 C6 B1 130.1(4) . . ?
C10 C6 B1 122.3(4) . . ?
C7 C6 Fe1 69.5(3) . . ?
C10 C6 Fe1 69.3(3) . . ?
B1 C6 Fe1 120.1(3) . . ?
C8 C7 C6 108.5(4) . . ?
C8 C7 Fe1 69.8(3) . . ?
C6 C7 Fe1 69.5(3) . . ?
C8 C7 H7 125.8 . . ?
C6 C7 H7 125.8 . . ?
Fe1 C7 H7 125.8 . . ?
C9 C8 C7 108.5(4) . . ?
C9 C8 Fe1 69.4(3) . . ?
C7 C8 Fe1 69.4(3) . . ?
C9 C8 H8 125.8 . . ?
C7 C8 H8 125.8 . . ?
Fe1 C8 H8 125.8 . . ?
C8 C9 C10 109.3(4) . . ?
C8 C9 Fe1 70.5(3) . . ?
C10 C9 Fe1 70.0(3) . . ?
C8 C9 H9 125.3 . . ?
C10 C9 H9 125.3 . . ?
Fe1 C9 H9 125.3 . . ?
C9 C10 C6 106.7(4) . . ?
C9 C10 B1 129.8(4) . 2_776 ?
C6 C10 B1 122.8(4) . 2_776 ?
C9 C10 Fe1 68.9(3) . . ?
C6 C10 Fe1 68.9(3) . . ?
B1 C10 Fe1 119.6(3) 2_776 . ?
C16 C11 C12 117.0(4) . . ?
C16 C11 B1 122.4(4) . . ?
C12 C11 B1 120.6(4) . . ?
C13 C12 C11 120.5(4) . . ?
C13 C12 C17 117.2(4) . . ?
C11 C12 C17 122.2(4) . . ?
C12 C13 C14 122.2(4) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C15 C14 C13 117.2(4) . . ?
C15 C14 C18 122.7(5) . . ?
C13 C14 C18 120.1(5) . . ?
C14 C15 C16 122.5(5) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C11 120.6(4) . . ?
C15 C16 C19 117.4(4) . . ?
C11 C16 C19 122.0(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C24 107.9(4) . . ?
C21 C20 Fe2 69.8(3) . . ?
C24 C20 Fe2 70.0(3) . . ?
C21 C20 H20 126.1 . . ?
C24 C20 H20 126.1 . . ?
Fe2 C20 H20 126.1 . . ?
C22 C21 C20 108.3(4) . . ?
C22 C21 Fe2 70.0(3) . . ?
C20 C21 Fe2 70.0(3) . . ?
C22 C21 H21 125.8 . . ?
C20 C21 H21 125.8 . . ?
Fe2 C21 H21 125.8 . . ?
C21 C22 C23 108.0(4) . . ?
C21 C22 Fe2 69.9(3) . . ?
C23 C22 Fe2 69.8(3) . . ?
C21 C22 H22 126.0 . . ?
C23 C22 H22 126.0 . . ?
Fe2 C22 H22 126.0 . . ?
C24 C23 C22 107.6(4) . . ?
C24 C23 Fe2 70.0(3) . . ?
C22 C23 Fe2 69.7(3) . . ?
C24 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
Fe2 C23 H23 126.2 . . ?
C20 C24 C23 108.2(4) . . ?
C20 C24 Fe2 69.8(2) . . ?
C23 C24 Fe2 69.7(3) . . ?
C20 C24 H24 125.9 . . ?
C23 C24 H24 125.9 . . ?
Fe2 C24 H24 125.9 . . ?
C26 C25 C29 107.2(4) . . ?
C26 C25 B2 130.5(4) . . ?
C29 C25 B2 121.8(4) . . ?
C26 C25 Fe2 68.9(2) . . ?
C29 C25 Fe2 68.9(2) . . ?
B2 C25 Fe2 120.8(3) . . ?
C27 C26 C25 108.9(4) . . ?
C27 C26 Fe2 69.7(2) . . ?
C25 C26 Fe2 70.3(2) . . ?
C27 C26 H26 125.5 . . ?
C25 C26 H26 125.5 . . ?
Fe2 C26 H26 125.5 . . ?
C28 C27 C26 108.1(4) . . ?
C28 C27 Fe2 69.5(2) . . ?
C26 C27 Fe2 69.6(2) . . ?
C28 C27 H27 125.9 . . ?
C26 C27 H27 125.9 . . ?
Fe2 C27 H27 125.9 . . ?
C27 C28 C29 108.8(4) . . ?
C27 C28 Fe2 69.8(2) . . ?
C29 C28 Fe2 69.9(2) . . ?
C27 C28 H28 125.6 . . ?
C29 C28 H28 125.6 . . ?
Fe2 C28 H28 125.6 . . ?
C28 C29 C25 106.9(4) . . ?
C28 C29 B2 129.7(4) . 2_565 ?
C25 C29 B2 122.7(4) . 2_565 ?
C28 C29 Fe2 69.0(3) . . ?
C25 C29 Fe2 69.5(2) . . ?
B2 C29 Fe2 119.6(3) 2_565 . ?
C35 C30 C31 118.0(4) . . ?
C35 C30 B2 120.1(4) . . ?
C31 C30 B2 121.9(4) . . ?
C32 C31 C30 119.8(4) . . ?
C32 C31 C36 118.4(4) . . ?
C30 C31 C36 121.8(4) . . ?
C31 C32 C33 122.9(4) . . ?
C31 C32 H32 118.6 . . ?
C33 C32 H32 118.6 . . ?
C32 C33 C34 116.5(4) . . ?
C32 C33 C37 122.6(4) . . ?
C34 C33 C37 120.9(5) . . ?
C35 C34 C33 122.7(4) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C34 C35 C30 120.1(4) . . ?
C34 C35 C38 117.4(4) . . ?
C30 C35 C38 122.5(4) . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C31 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Cl1 C39 Cl3 109.7(5) . . ?
Cl1 C39 Cl2 111.1(6) . . ?
Cl3 C39 Cl2 110.3(7) . . ?
Cl1 C39 H39 108.6 . . ?
Cl3 C39 H39 108.6 . . ?
Cl2 C39 H39 108.6 . . ?
Cl2A C39A H39A 107.5 . . ?
Cl3A C39A H39A 107.5 . . ?
C9 Fe1 C4 110.4(2) . . ?
C9 Fe1 C1 178.2(2) . . ?
C4 Fe1 C1 67.8(2) . . ?
C9 Fe1 C5 138.0(2) . . ?
C4 Fe1 C5 39.9(2) . . ?
C1 Fe1 C5 40.7(2) . . ?
C9 Fe1 C7 68.4(2) . . ?
C4 Fe1 C7 171.0(2) . . ?
C1 Fe1 C7 113.3(2) . . ?
C5 Fe1 C7 146.2(2) . . ?
C9 Fe1 C6 69.43(19) . . ?
C4 Fe1 C6 147.7(2) . . ?
C1 Fe1 C6 112.2(2) . . ?
C5 Fe1 C6 118.1(2) . . ?
C7 Fe1 C6 41.03(19) . . ?
C9 Fe1 C8 40.09(19) . . ?
C4 Fe1 C8 132.8(2) . . ?
C1 Fe1 C8 140.9(2) . . ?
C5 Fe1 C8 172.5(2) . . ?
C7 Fe1 C8 40.8(2) . . ?
C6 Fe1 C8 69.03(19) . . ?
C9 Fe1 C10 41.14(18) . . ?
C4 Fe1 C10 116.2(2) . . ?
C1 Fe1 C10 139.6(2) . . ?
C5 Fe1 C10 114.58(19) . . ?
C7 Fe1 C10 69.27(19) . . ?
C6 Fe1 C10 41.79(18) . . ?
C8 Fe1 C10 68.70(19) . . ?
C9 Fe1 C3 111.0(2) . . ?
C4 Fe1 C3 40.1(2) . . ?
C1 Fe1 C3 67.5(2) . . ?
C5 Fe1 C3 67.2(2) . . ?
C7 Fe1 C3 131.3(2) . . ?
C6 Fe1 C3 172.12(19) . . ?
C8 Fe1 C3 106.0(2) . . ?
C10 Fe1 C3 143.2(2) . . ?
C9 Fe1 C2 139.2(2) . . ?
C4 Fe1 C2 67.0(2) . . ?
C1 Fe1 C2 40.2(2) . . ?
C5 Fe1 C2 67.3(2) . . ?
C7 Fe1 C2 107.7(2) . . ?
C6 Fe1 C2 135.2(2) . . ?
C8 Fe1 C2 109.7(2) . . ?
C10 Fe1 C2 176.81(19) . . ?
C3 Fe1 C2 39.6(2) . . ?
C28 Fe2 C26 68.59(18) . . ?
C28 Fe2 C27 40.69(18) . . ?
C26 Fe2 C27 40.70(18) . . ?
C28 Fe2 C21 176.88(19) . . ?
C26 Fe2 C21 113.94(18) . . ?
C27 Fe2 C21 140.13(19) . . ?
C28 Fe2 C22 137.9(2) . . ?
C26 Fe2 C22 108.18(18) . . ?
C27 Fe2 C22 108.66(19) . . ?
C21 Fe2 C22 40.2(2) . . ?
C28 Fe2 C23 109.2(2) . . ?
C26 Fe2 C23 132.41(19) . . ?
C27 Fe2 C23 105.4(2) . . ?
C21 Fe2 C23 67.8(2) . . ?
C22 Fe2 C23 40.5(2) . . ?
C28 Fe2 C20 138.38(18) . . ?
C26 Fe2 C20 145.49(18) . . ?
C27 Fe2 C20 173.00(19) . . ?
C21 Fe2 C20 40.26(18) . . ?
C22 Fe2 C20 67.70(19) . . ?
C23 Fe2 C20 67.8(2) . . ?
C28 Fe2 C29 41.07(18) . . ?
C26 Fe2 C29 69.20(17) . . ?
C27 Fe2 C29 69.06(18) . . ?
C21 Fe2 C29 141.00(19) . . ?
C22 Fe2 C29 177.32(18) . . ?
C23 Fe2 C29 140.89(19) . . ?
C20 Fe2 C29 114.72(18) . . ?
C28 Fe2 C24 109.63(19) . . ?
C26 Fe2 C24 172.24(19) . . ?
C27 Fe2 C24 133.2(2) . . ?
C21 Fe2 C24 67.61(19) . . ?
C22 Fe2 C24 67.74(19) . . ?
C23 Fe2 C24 40.3(2) . . ?
C20 Fe2 C24 40.24(19) . . ?
C29 Fe2 C24 114.80(18) . . ?
C28 Fe2 C25 69.14(18) . . ?
C26 Fe2 C25 40.77(17) . . ?
C27 Fe2 C25 68.82(18) . . ?
C21 Fe2 C25 113.95(18) . . ?
C22 Fe2 C25 136.62(18) . . ?
C23 Fe2 C25 173.16(19) . . ?
C20 Fe2 C25 118.04(18) . . ?
C29 Fe2 C25 41.58(17) . . ?
C24 Fe2 C25 146.47(19) . . ?
_diffrn_measured_fraction_theta_max 0.915
_diffrn_reflns_theta_full 59.99
_diffrn_measured_fraction_theta_full 0.915
_refine_diff_density_max 0.682
_refine_diff_density_min -0.750
_refine_diff_density_rms 0.084
#===END
data_3Pf2
_database_code_depnum_ccdc_archive 'CCDC 669589'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C32 H16 B2 F10 Fe2'
_chemical_formula_sum 'C32 H16 B2 F10 Fe2'
_chemical_formula_weight 723.77
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting MONOCLINIC
_symmetry_space_group_name_H-M C2/c
_symmetry_space_group_name_Hall -C2yc
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 23.7946(2)
_cell_length_b 7.0879(1)
_cell_length_c 18.0370(2)
_cell_angle_alpha 90.00
_cell_angle_beta 119.329(2)
_cell_angle_gamma 90.00
_cell_volume 2652.09(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 7725
_cell_measurement_theta_min 4.26
_cell_measurement_theta_max 67.64
_exptl_crystal_description 'RECTANGULAR BLOCK'
_exptl_crystal_colour RED
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.813
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1440
_exptl_absorpt_coefficient_mu 9.645
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.1882
_exptl_absorpt_correction_T_max 0.4168
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)'
_exptl_special_details
;
'crystal mounted on cryoloop using Paratone-N'
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 13082
_diffrn_reflns_av_R_equivalents 0.0431
_diffrn_reflns_av_sigmaI/netI 0.0270
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 4.26
_diffrn_reflns_theta_max 67.89
_reflns_number_total 2400
_reflns_number_gt 2210
_reflns_threshold_expression >2sigma(I)
_publ_section_references
;
Bruker (2005). SAINT Version 7.23a. Bruker AXS Inc.,
Madison, Wisconsin, USA.
Bruker (2006). APEX 2 Version 2.0-2. Bruker AXS
Inc., Madison, Wisconsin, USA.
Sheldrick, G.M. (2001). SADABS. Version 2. University of
G\"ottingen, Germany.
Sheldrick, G. M. (2004). SHELXTL Version 6.14. Bruker AXS
Inc., Madison, Wisconsin, USA.
;
#====================================================================
_computing_data_collection 'APEX 2 (Bruker, 2006)'
_computing_cell_refinement 'APEX 2'
_computing_data_reduction 'SAINT (Bruker, 2005)'
_computing_structure_solution 'SHELXTL (Sheldrick, 2004)'
_computing_structure_refinement SHELXTL
_computing_molecular_graphics SHELXTL
_computing_publication_material SHELXTL
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.7194P] 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 2400
_refine_ls_number_parameters 208
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0337
_refine_ls_R_factor_gt 0.0301
_refine_ls_wR_factor_ref 0.0778
_refine_ls_wR_factor_gt 0.0756
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.042
_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 1.068761(13) 0.83843(4) 0.440030(19) 0.01311(12) Uani 1 1 d . . .
F1 F 0.83934(5) 0.73533(18) 0.33231(8) 0.0230(3) Uani 1 1 d . . .
F2 F 0.73687(6) 0.7572(2) 0.17659(8) 0.0283(3) Uani 1 1 d . . .
F3 F 0.72069(5) 1.0591(2) 0.07542(8) 0.0279(3) Uani 1 1 d . . .
F4 F 0.80895(7) 1.34455(18) 0.13348(9) 0.0306(3) Uani 1 1 d . . .
F5 F 0.91394(6) 1.31984(17) 0.28723(8) 0.0252(3) Uani 1 1 d . . .
B1 B 0.94200(10) 1.0134(3) 0.40985(14) 0.0138(4) Uani 1 1 d . . .
C1 C 0.98323(9) 0.8336(3) 0.44152(13) 0.0151(4) Uani 1 1 d . . .
C2 C 0.98715(9) 0.6744(3) 0.39512(13) 0.0173(4) Uani 1 1 d . . .
H2 H 0.9567 0.6465 0.3339 0.021 Uiso 1 1 calc R . .
C3 C 1.04208(10) 0.5660(3) 0.44936(14) 0.0182(4) Uani 1 1 d . . .
H3 H 1.0568 0.4490 0.4329 0.022 Uiso 1 1 calc R . .
C4 C 1.07330(10) 0.6532(3) 0.53060(14) 0.0173(4) Uani 1 1 d . . .
H4 H 1.1137 0.6076 0.5811 0.021 Uiso 1 1 calc R . .
C5 C 1.03801(9) 0.8197(3) 0.52771(13) 0.0154(4) Uani 1 1 d . . .
C6 C 1.13668(11) 0.8052(3) 0.40261(17) 0.0275(5) Uani 1 1 d . . .
H6 H 1.1547 0.6826 0.3962 0.033 Uiso 1 1 calc R . .
C7 C 1.16182(10) 0.9169(4) 0.47723(15) 0.0256(5) Uani 1 1 d . . .
H7 H 1.2005 0.8861 0.5330 0.031 Uiso 1 1 calc R . .
C8 C 1.12234(10) 1.0797(3) 0.45956(14) 0.0227(5) Uani 1 1 d . . .
H8 H 1.1284 1.1832 0.5005 0.027 Uiso 1 1 calc R . .
C9 C 1.07264(10) 1.0688(3) 0.37324(14) 0.0218(5) Uani 1 1 d . . .
H9 H 1.0375 1.1633 0.3428 0.026 Uiso 1 1 calc R . .
C10 C 1.08138(11) 0.8994(3) 0.33828(15) 0.0245(5) Uani 1 1 d . . .
H10 H 1.0536 0.8540 0.2787 0.029 Uiso 1 1 calc R . .
C11 C 0.88118(9) 1.0280(3) 0.31769(13) 0.0149(4) Uani 1 1 d . . .
C12 C 0.83420(9) 0.8880(3) 0.28470(13) 0.0168(4) Uani 1 1 d . . .
C13 C 0.78061(9) 0.8974(3) 0.20514(13) 0.0196(4) Uani 1 1 d . . .
C14 C 0.77193(9) 1.0507(3) 0.15356(13) 0.0196(4) Uani 1 1 d . . .
C15 C 0.81686(10) 1.1943(3) 0.18328(14) 0.0198(4) Uani 1 1 d . . .
C16 C 0.86992(10) 1.1802(3) 0.26324(14) 0.0177(4) Uani 1 1 d . . .
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 0.01234(17) 0.01479(18) 0.01453(18) -0.00085(12) 0.00838(13) -0.00112(11)
F1 0.0204(6) 0.0259(7) 0.0199(6) 0.0032(5) 0.0077(5) -0.0082(5)
F2 0.0182(6) 0.0404(8) 0.0216(7) -0.0045(6) 0.0060(5) -0.0133(6)
F3 0.0167(6) 0.0439(8) 0.0154(6) 0.0005(6) 0.0018(5) 0.0059(5)
F4 0.0375(7) 0.0258(7) 0.0219(7) 0.0096(5) 0.0094(6) 0.0073(6)
F5 0.0302(7) 0.0196(6) 0.0228(7) 0.0004(5) 0.0107(6) -0.0066(5)
B1 0.0123(9) 0.0183(11) 0.0147(11) 0.0007(9) 0.0096(9) -0.0023(8)
C1 0.0127(9) 0.0181(10) 0.0173(10) -0.0009(8) 0.0096(8) -0.0043(7)
C2 0.0170(9) 0.0190(10) 0.0173(10) -0.0027(8) 0.0095(8) -0.0053(8)
C3 0.0223(9) 0.0154(10) 0.0233(11) -0.0005(8) 0.0162(9) -0.0022(8)
C4 0.0172(9) 0.0185(10) 0.0188(10) 0.0020(8) 0.0108(8) -0.0010(8)
C5 0.0140(9) 0.0184(10) 0.0166(10) 0.0025(8) 0.0098(8) -0.0007(7)
C6 0.0278(11) 0.0293(12) 0.0411(14) 0.0030(10) 0.0291(11) 0.0002(9)
C7 0.0141(9) 0.0360(13) 0.0272(12) 0.0063(10) 0.0105(9) -0.0039(9)
C8 0.0223(10) 0.0229(11) 0.0255(12) -0.0017(9) 0.0137(9) -0.0107(9)
C9 0.0206(10) 0.0246(11) 0.0228(11) 0.0071(9) 0.0126(9) -0.0021(9)
C10 0.0271(11) 0.0324(12) 0.0216(11) -0.0007(10) 0.0177(9) -0.0077(10)
C11 0.0140(9) 0.0178(10) 0.0157(10) -0.0019(8) 0.0093(8) 0.0003(8)
C12 0.0152(9) 0.0214(10) 0.0176(10) 0.0004(8) 0.0109(8) 0.0001(8)
C13 0.0111(9) 0.0304(12) 0.0185(11) -0.0051(9) 0.0083(8) -0.0031(8)
C14 0.0126(8) 0.0308(12) 0.0142(10) -0.0006(9) 0.0056(8) 0.0063(8)
C15 0.0224(10) 0.0207(10) 0.0178(11) 0.0055(8) 0.0109(9) 0.0095(8)
C16 0.0175(10) 0.0175(10) 0.0193(11) -0.0025(8) 0.0099(8) -0.0012(8)
_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 C10 2.046(2) . ?
Fe1 C5 2.046(2) . ?
Fe1 C6 2.047(2) . ?
Fe1 C1 2.0489(19) . ?
Fe1 C7 2.051(2) . ?
Fe1 C4 2.057(2) . ?
Fe1 C8 2.058(2) . ?
Fe1 C9 2.058(2) . ?
Fe1 C2 2.059(2) . ?
Fe1 C3 2.065(2) . ?
F1 C12 1.349(2) . ?
F2 C13 1.346(3) . ?
F3 C14 1.339(2) . ?
F4 C15 1.346(2) . ?
F5 C16 1.349(2) . ?
B1 C1 1.537(3) . ?
B1 C5 1.540(3) 5_776 ?
B1 C11 1.585(3) . ?
C1 C2 1.435(3) . ?
C1 C5 1.463(3) . ?
C2 C3 1.415(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.419(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.434(3) . ?
C4 H4 1.0000 . ?
C5 B1 1.540(3) 5_776 ?
C6 C7 1.417(4) . ?
C6 C10 1.424(4) . ?
C6 H6 1.0000 . ?
C7 C8 1.422(3) . ?
C7 H7 1.0000 . ?
C8 C9 1.423(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.418(3) . ?
C9 H9 1.0000 . ?
C10 H10 1.0000 . ?
C11 C12 1.392(3) . ?
C11 C16 1.393(3) . ?
C12 C13 1.377(3) . ?
C13 C14 1.379(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.378(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
C10 Fe1 C5 166.46(9) . . ?
C10 Fe1 C6 40.72(10) . . ?
C5 Fe1 C6 152.38(10) . . ?
C10 Fe1 C1 126.77(9) . . ?
C5 Fe1 C1 41.86(8) . . ?
C6 Fe1 C1 162.18(10) . . ?
C10 Fe1 C7 68.09(9) . . ?
C5 Fe1 C7 120.14(9) . . ?
C6 Fe1 C7 40.45(10) . . ?
C1 Fe1 C7 156.98(9) . . ?
C10 Fe1 C4 150.88(9) . . ?
C5 Fe1 C4 40.91(8) . . ?
C6 Fe1 C4 116.45(9) . . ?
C1 Fe1 C4 69.20(8) . . ?
C7 Fe1 C4 106.56(9) . . ?
C10 Fe1 C8 68.11(9) . . ?
C5 Fe1 C8 110.35(9) . . ?
C6 Fe1 C8 68.23(9) . . ?
C1 Fe1 C8 123.22(8) . . ?
C7 Fe1 C8 40.49(9) . . ?
C4 Fe1 C8 127.40(9) . . ?
C10 Fe1 C9 40.44(10) . . ?
C5 Fe1 C9 129.76(9) . . ?
C6 Fe1 C9 68.25(9) . . ?
C1 Fe1 C9 110.53(8) . . ?
C7 Fe1 C9 68.01(9) . . ?
C4 Fe1 C9 166.26(9) . . ?
C8 Fe1 C9 40.45(9) . . ?
C10 Fe1 C2 106.92(9) . . ?
C5 Fe1 C2 69.02(8) . . ?
C6 Fe1 C2 123.37(9) . . ?
C1 Fe1 C2 40.89(8) . . ?
C7 Fe1 C2 160.22(9) . . ?
C4 Fe1 C2 67.94(8) . . ?
C8 Fe1 C2 157.32(9) . . ?
C9 Fe1 C2 121.46(8) . . ?
C10 Fe1 C3 117.17(9) . . ?
C5 Fe1 C3 68.63(8) . . ?
C6 Fe1 C3 104.07(9) . . ?
C1 Fe1 C3 68.67(8) . . ?
C7 Fe1 C3 123.55(9) . . ?
C4 Fe1 C3 40.28(8) . . ?
C8 Fe1 C3 162.29(9) . . ?
C9 Fe1 C3 153.30(9) . . ?
C2 Fe1 C3 40.14(8) . . ?
C1 B1 C5 116.94(18) . 5_776 ?
C1 B1 C11 122.19(18) . . ?
C5 B1 C11 120.86(18) 5_776 . ?
C2 C1 C5 106.74(17) . . ?
C2 C1 B1 130.32(19) . . ?
C5 C1 B1 121.66(18) . . ?
C2 C1 Fe1 69.92(11) . . ?
C5 C1 Fe1 68.98(11) . . ?
B1 C1 Fe1 116.00(13) . . ?
C3 C2 C1 109.01(18) . . ?
C3 C2 Fe1 70.18(11) . . ?
C1 C2 Fe1 69.19(11) . . ?
C3 C2 H2 125.5 . . ?
C1 C2 H2 125.5 . . ?
Fe1 C2 H2 125.5 . . ?
C2 C3 C4 108.43(18) . . ?
C2 C3 Fe1 69.68(12) . . ?
C4 C3 Fe1 69.54(12) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
Fe1 C3 H3 125.8 . . ?
C3 C4 C5 108.65(18) . . ?
C3 C4 Fe1 70.17(12) . . ?
C5 C4 Fe1 69.15(11) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Fe1 C4 H4 125.7 . . ?
C4 C5 C1 107.16(18) . . ?
C4 C5 B1 129.81(18) . 5_776 ?
C1 C5 B1 121.38(18) . 5_776 ?
C4 C5 Fe1 69.94(11) . . ?
C1 C5 Fe1 69.16(11) . . ?
B1 C5 Fe1 114.58(13) 5_776 . ?
C7 C6 C10 107.7(2) . . ?
C7 C6 Fe1 69.92(12) . . ?
C10 C6 Fe1 69.58(12) . . ?
C7 C6 H6 126.2 . . ?
C10 C6 H6 126.2 . . ?
Fe1 C6 H6 126.2 . . ?
C6 C7 C8 108.4(2) . . ?
C6 C7 Fe1 69.63(12) . . ?
C8 C7 Fe1 70.00(11) . . ?
C6 C7 H7 125.8 . . ?
C8 C7 H7 125.8 . . ?
Fe1 C7 H7 125.8 . . ?
C7 C8 C9 107.8(2) . . ?
C7 C8 Fe1 69.50(12) . . ?
C9 C8 Fe1 69.79(12) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 H8 126.1 . . ?
Fe1 C8 H8 126.1 . . ?
C10 C9 C8 107.94(19) . . ?
C10 C9 Fe1 69.31(12) . . ?
C8 C9 Fe1 69.76(12) . . ?
C10 C9 H9 126.0 . . ?
C8 C9 H9 126.0 . . ?
Fe1 C9 H9 126.0 . . ?
C9 C10 C6 108.2(2) . . ?
C9 C10 Fe1 70.25(12) . . ?
C6 C10 Fe1 69.70(13) . . ?
C9 C10 H10 125.9 . . ?
C6 C10 H10 125.9 . . ?
Fe1 C10 H10 125.9 . . ?
C12 C11 C16 114.44(18) . . ?
C12 C11 B1 122.08(18) . . ?
C16 C11 B1 123.48(18) . . ?
F1 C12 C13 116.80(18) . . ?
F1 C12 C11 119.76(18) . . ?
C13 C12 C11 123.4(2) . . ?
F2 C13 C12 120.7(2) . . ?
F2 C13 C14 119.44(18) . . ?
C12 C13 C14 119.8(2) . . ?
F3 C14 C13 120.24(19) . . ?
F3 C14 C15 120.6(2) . . ?
C13 C14 C15 119.17(19) . . ?
F4 C15 C16 120.8(2) . . ?
F4 C15 C14 119.72(19) . . ?
C16 C15 C14 119.4(2) . . ?
F5 C16 C15 116.87(19) . . ?
F5 C16 C11 119.39(18) . . ?
C15 C16 C11 123.69(19) . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 67.89
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.493
_refine_diff_density_min -0.268
_refine_diff_density_rms 0.066
#===END