data_test_0m
_publ_contact_author_name 'Prof. Frieder Jaekle'
_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_phone '(973) 353 5064 '
_publ_contact_author_fax '(973) 353 1264'
loop_
_publ_author_name
_publ_author_address
'Prof. Frieder Jaekle'
;Rutgers University, Chemistry Department
73 Warren Street, Newark, NJ 07102, USA
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C68 H76 B2 Fe2 S4, 2(C7 H8)'
_chemical_formula_sum
'C82 H92 B2 Fe2 S4'
_chemical_formula_weight 1339.12
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'
'S' 'S' 0.3331 0.5567
'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'
'B' 'B' 0.0090 0.0039
'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 9.7770(3)
_cell_length_b 11.5826(4)
_cell_length_c 16.0262(5)
_cell_angle_alpha 81.645(2)
_cell_angle_beta 75.3130(10)
_cell_angle_gamma 83.325(2)
_cell_volume 1730.94(10)
_cell_formula_units_Z 1
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4554
_cell_measurement_theta_min 2.87
_cell_measurement_theta_max 66.75
_exptl_crystal_description prism
_exptl_crystal_colour red
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.08
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.285
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 710
_exptl_absorpt_coefficient_mu 4.818
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.6444
_exptl_absorpt_correction_T_max 0.6992
_exptl_absorpt_process_details 'sadabs'
_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 '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 13131
_diffrn_reflns_av_R_equivalents 0.0458
_diffrn_reflns_av_sigmaI/netI 0.0664
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.87
_diffrn_reflns_theta_max 66.97
_reflns_number_total 6157
_reflns_number_gt 4132
_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 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6157
_refine_ls_number_parameters 414
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0761
_refine_ls_R_factor_gt 0.0475
_refine_ls_wR_factor_ref 0.1197
_refine_ls_wR_factor_gt 0.1073
_refine_ls_goodness_of_fit_ref 0.999
_refine_ls_restrained_S_all 0.999
_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 0.62268(6) 0.34588(4) 0.68270(3) 0.02254(16) Uani 1 1 d . . .
S1 S 0.23902(9) 0.90533(7) 0.90267(6) 0.0280(2) Uani 1 1 d . . .
S2 S 0.34870(9) 0.65296(7) 0.98931(5) 0.0236(2) Uani 1 1 d . . .
B1 B 0.3982(4) 0.5742(3) 0.7391(3) 0.0212(8) Uani 1 1 d . . .
C1 C 0.0459(4) 1.0993(3) 0.8826(3) 0.0374(9) Uani 1 1 d . . .
H1A H -0.0374 1.1231 0.8610 0.056 Uiso 1 1 calc R . .
H1B H 0.1211 1.1465 0.8508 0.056 Uiso 1 1 calc R . .
H1C H 0.0254 1.1091 0.9431 0.056 Uiso 1 1 calc R . .
C2 C 0.0905(4) 0.9737(3) 0.8714(2) 0.0268(8) Uani 1 1 d . . .
C3 C 0.0286(4) 0.8982(3) 0.8379(2) 0.0271(8) Uani 1 1 d . . .
H3 H -0.0527 0.9194 0.8174 0.033 Uiso 1 1 calc R . .
C4 C 0.0996(3) 0.7839(3) 0.8372(2) 0.0222(7) Uani 1 1 d . . .
H4 H 0.0691 0.7229 0.8165 0.027 Uiso 1 1 calc R . .
C5 C 0.2171(3) 0.7728(3) 0.8699(2) 0.0226(7) Uani 1 1 d . . .
C6 C 0.3132(3) 0.6706(3) 0.8867(2) 0.0206(7) Uani 1 1 d . . .
C7 C 0.3904(3) 0.5860(3) 0.8364(2) 0.0196(7) Uani 1 1 d . . .
C8 C 0.4746(3) 0.5076(3) 0.8852(2) 0.0201(7) Uani 1 1 d . . .
H8 H 0.5323 0.4447 0.8619 0.024 Uiso 1 1 calc R . .
C9 C 0.4651(3) 0.5305(3) 0.9675(2) 0.0203(7) Uani 1 1 d . . .
C10 C 0.5330(3) 0.5173(3) 0.6811(2) 0.0207(7) Uani 1 1 d . . .
C11 C 0.6775(3) 0.5086(3) 0.6883(2) 0.0217(7) Uani 1 1 d . . .
H11 H 0.7087 0.5318 0.7365 0.026 Uiso 1 1 calc R . .
C12 C 0.7680(4) 0.4611(3) 0.6153(2) 0.0249(8) Uani 1 1 d . . .
H12 H 0.8714 0.4464 0.6044 0.030 Uiso 1 1 calc R . .
C13 C 0.6826(3) 0.4372(3) 0.5609(2) 0.0235(8) Uani 1 1 d . . .
H13 H 0.7165 0.4034 0.5060 0.028 Uiso 1 1 calc R . .
C14 C 0.5396(4) 0.4716(3) 0.6006(2) 0.0225(8) Uani 1 1 d . . .
H14 H 0.4576 0.4640 0.5777 0.027 Uiso 1 1 calc R . .
C15 C 0.5067(4) 0.2390(3) 0.7834(2) 0.0340(9) Uani 1 1 d . . .
H15 H 0.4214 0.2633 0.8264 0.041 Uiso 1 1 calc R . .
C16 C 0.5110(4) 0.2018(3) 0.7016(2) 0.0329(9) Uani 1 1 d . . .
H16 H 0.4287 0.1958 0.6786 0.040 Uiso 1 1 calc R . .
C17 C 0.6552(4) 0.1750(3) 0.6595(2) 0.0291(8) Uani 1 1 d . . .
H17 H 0.6899 0.1468 0.6024 0.035 Uiso 1 1 calc R . .
C18 C 0.7401(4) 0.1955(3) 0.7150(2) 0.0299(8) Uani 1 1 d . . .
H18 H 0.8439 0.1844 0.7029 0.036 Uiso 1 1 calc R . .
C19 C 0.6483(4) 0.2347(3) 0.7910(2) 0.0316(9) Uani 1 1 d . . .
H19 H 0.6780 0.2564 0.8402 0.038 Uiso 1 1 calc R . .
C20 C 0.2741(3) 0.6270(3) 0.6940(2) 0.0198(7) Uani 1 1 d . . .
C21 C 0.2827(3) 0.7392(3) 0.6452(2) 0.0219(7) Uani 1 1 d . . .
C22 C 0.1696(4) 0.7887(3) 0.6102(2) 0.0247(8) Uani 1 1 d . . .
H22 H 0.1757 0.8625 0.5783 0.030 Uiso 1 1 calc R . .
C23 C 0.0472(3) 0.7309(3) 0.6214(2) 0.0236(8) Uani 1 1 d . . .
C24 C 0.0432(3) 0.6197(3) 0.6663(2) 0.0231(8) Uani 1 1 d . . .
H24 H -0.0362 0.5790 0.6731 0.028 Uiso 1 1 calc R . .
C25 C 0.1550(3) 0.5661(3) 0.7020(2) 0.0208(7) Uani 1 1 d . . .
C26 C 0.4127(4) 0.8054(3) 0.6336(2) 0.0268(8) Uani 1 1 d . . .
H26 H 0.4627 0.7683 0.6776 0.032 Uiso 1 1 calc R . .
C27 C 0.3778(4) 0.9341(3) 0.6477(2) 0.0343(9) Uani 1 1 d . . .
H27A H 0.3357 0.9749 0.6026 0.051 Uiso 1 1 calc R . .
H27B H 0.4633 0.9684 0.6463 0.051 Uiso 1 1 calc R . .
H27C H 0.3124 0.9400 0.7032 0.051 Uiso 1 1 calc R . .
C28 C 0.5149(4) 0.7938(3) 0.5446(2) 0.0343(9) Uani 1 1 d . . .
H28A H 0.5387 0.7124 0.5376 0.051 Uiso 1 1 calc R . .
H28B H 0.5997 0.8306 0.5408 0.051 Uiso 1 1 calc R . .
H28C H 0.4704 0.8311 0.4996 0.051 Uiso 1 1 calc R . .
C29 C -0.0780(4) 0.7853(3) 0.5851(2) 0.0282(8) Uani 1 1 d . . .
H29 H -0.1582 0.7389 0.6139 0.034 Uiso 1 1 calc R . .
C30 C -0.1235(4) 0.9100(3) 0.6045(2) 0.0332(9) Uani 1 1 d . . .
H30A H -0.1440 0.9126 0.6660 0.050 Uiso 1 1 calc R . .
H30B H -0.2069 0.9375 0.5838 0.050 Uiso 1 1 calc R . .
H30C H -0.0485 0.9591 0.5758 0.050 Uiso 1 1 calc R . .
C31 C -0.0485(4) 0.7753(3) 0.4880(2) 0.0402(10) Uani 1 1 d . . .
H31A H 0.0351 0.8137 0.4579 0.060 Uiso 1 1 calc R . .
H31B H -0.1278 0.8117 0.4661 0.060 Uiso 1 1 calc R . .
H31C H -0.0342 0.6941 0.4790 0.060 Uiso 1 1 calc R . .
C32 C 0.1438(3) 0.4429(3) 0.7496(2) 0.0238(8) Uani 1 1 d . . .
H32 H 0.2256 0.4233 0.7754 0.029 Uiso 1 1 calc R . .
C33 C 0.0092(4) 0.4338(3) 0.8234(2) 0.0321(9) Uani 1 1 d . . .
H33A H 0.0072 0.4895 0.8627 0.048 Uiso 1 1 calc R . .
H33B H 0.0089 0.3562 0.8540 0.048 Uiso 1 1 calc R . .
H33C H -0.0727 0.4501 0.7996 0.048 Uiso 1 1 calc R . .
C34 C 0.1507(4) 0.3539(3) 0.6861(2) 0.0307(9) Uani 1 1 d . . .
H34A H 0.0687 0.3684 0.6623 0.046 Uiso 1 1 calc R . .
H34B H 0.1529 0.2761 0.7164 0.046 Uiso 1 1 calc R . .
H34C H 0.2349 0.3617 0.6400 0.046 Uiso 1 1 calc R . .
C35 C 0.2575(4) 0.2556(3) 0.0506(2) 0.0284(8) Uani 1 1 d . . .
C36 C 0.3084(4) 0.1432(3) 0.0304(2) 0.0341(9) Uani 1 1 d . . .
H36 H 0.3014 0.1210 -0.0217 0.041 Uiso 1 1 calc R . .
C37 C 0.3695(4) 0.0639(3) 0.0867(3) 0.0370(9) Uani 1 1 d . . .
H37 H 0.4015 -0.0113 0.0726 0.044 Uiso 1 1 calc R . .
C38 C 0.3827(4) 0.0961(3) 0.1634(3) 0.0365(9) Uani 1 1 d . . .
H38 H 0.4231 0.0428 0.2014 0.044 Uiso 1 1 calc R . .
C39 C 0.3360(4) 0.2078(3) 0.1836(2) 0.0355(9) Uani 1 1 d . . .
H39 H 0.3474 0.2305 0.2346 0.043 Uiso 1 1 calc R . .
C40 C 0.2724(4) 0.2862(3) 0.1284(2) 0.0303(8) Uani 1 1 d . . .
H40 H 0.2390 0.3607 0.1435 0.036 Uiso 1 1 calc R . .
C41 C 0.1813(4) 0.3391(3) -0.0064(2) 0.0337(9) Uani 1 1 d . . .
H41A H 0.0822 0.3266 0.0098 0.050 Uiso 1 1 calc R . .
H41B H 0.2199 0.3261 -0.0660 0.050 Uiso 1 1 calc R . .
H41C H 0.1931 0.4181 0.0004 0.050 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0268(3) 0.0242(3) 0.0179(3) -0.0048(2) -0.0078(2) 0.0007(2)
S1 0.0320(5) 0.0252(4) 0.0298(5) -0.0069(4) -0.0120(4) 0.0009(4)
S2 0.0287(5) 0.0275(4) 0.0159(5) -0.0061(4) -0.0090(4) 0.0044(4)
B1 0.023(2) 0.0175(18) 0.023(2) -0.0004(16) -0.0050(17) -0.0061(16)
C1 0.048(3) 0.0288(19) 0.035(2) 0.0003(17) -0.0153(19) 0.0042(18)
C2 0.029(2) 0.0286(18) 0.020(2) -0.0030(16) -0.0030(15) -0.0001(15)
C3 0.0207(19) 0.038(2) 0.021(2) 0.0017(16) -0.0055(15) 0.0024(15)
C4 0.0241(19) 0.0266(17) 0.0163(19) -0.0068(15) -0.0045(14) 0.0013(14)
C5 0.0258(19) 0.0255(17) 0.0150(18) -0.0016(14) -0.0028(14) -0.0025(14)
C6 0.0234(19) 0.0253(17) 0.0150(18) -0.0018(14) -0.0067(14) -0.0053(14)
C7 0.0226(18) 0.0229(17) 0.0156(18) -0.0011(14) -0.0074(14) -0.0065(14)
C8 0.0252(19) 0.0208(16) 0.0161(18) -0.0044(14) -0.0069(14) -0.0018(14)
C9 0.0262(19) 0.0198(16) 0.0163(18) -0.0043(14) -0.0059(14) -0.0034(14)
C10 0.0278(19) 0.0186(16) 0.0155(18) 0.0010(14) -0.0071(14) -0.0010(14)
C11 0.0238(19) 0.0239(17) 0.0204(19) -0.0066(15) -0.0087(14) -0.0014(14)
C12 0.0179(18) 0.0284(18) 0.027(2) -0.0019(15) -0.0038(15) -0.0018(14)
C13 0.029(2) 0.0266(18) 0.0144(19) -0.0024(15) -0.0063(15) 0.0002(15)
C14 0.029(2) 0.0256(17) 0.0137(18) -0.0004(14) -0.0080(15) -0.0006(15)
C15 0.043(2) 0.0254(18) 0.026(2) 0.0022(16) 0.0024(17) -0.0031(17)
C16 0.038(2) 0.0186(17) 0.045(3) -0.0037(17) -0.0148(19) -0.0033(16)
C17 0.042(2) 0.0223(18) 0.025(2) -0.0085(16) -0.0102(17) 0.0029(16)
C18 0.034(2) 0.0247(18) 0.031(2) -0.0038(16) -0.0123(17) 0.0078(16)
C19 0.050(3) 0.0242(18) 0.020(2) -0.0025(16) -0.0106(17) 0.0036(17)
C20 0.0231(19) 0.0249(17) 0.0114(18) -0.0072(14) -0.0031(13) 0.0020(14)
C21 0.0234(19) 0.0266(17) 0.0162(19) -0.0069(15) -0.0045(14) 0.0004(14)
C22 0.037(2) 0.0216(17) 0.0156(19) -0.0034(14) -0.0071(15) 0.0006(15)
C23 0.0249(19) 0.0282(18) 0.0197(19) -0.0122(15) -0.0068(15) 0.0052(15)
C24 0.0216(19) 0.0273(18) 0.023(2) -0.0104(15) -0.0063(14) -0.0002(14)
C25 0.0235(19) 0.0230(16) 0.0183(19) -0.0090(14) -0.0075(14) 0.0017(14)
C26 0.032(2) 0.0278(18) 0.023(2) -0.0007(15) -0.0124(16) -0.0044(15)
C27 0.044(2) 0.0305(19) 0.031(2) -0.0027(17) -0.0098(18) -0.0130(17)
C28 0.029(2) 0.040(2) 0.033(2) -0.0055(18) -0.0027(17) -0.0079(17)
C29 0.025(2) 0.0307(19) 0.031(2) -0.0048(16) -0.0130(16) 0.0043(15)
C30 0.037(2) 0.033(2) 0.030(2) -0.0026(17) -0.0110(17) 0.0035(17)
C31 0.042(2) 0.049(2) 0.033(2) -0.0129(19) -0.0181(19) 0.0123(19)
C32 0.0223(19) 0.0273(18) 0.024(2) -0.0023(15) -0.0109(15) -0.0015(15)
C33 0.039(2) 0.0263(19) 0.030(2) 0.0000(17) -0.0093(18) -0.0006(16)
C34 0.037(2) 0.0247(18) 0.032(2) -0.0025(16) -0.0130(17) -0.0019(16)
C35 0.0206(19) 0.038(2) 0.025(2) -0.0023(16) -0.0024(15) -0.0042(16)
C36 0.035(2) 0.040(2) 0.025(2) -0.0053(18) -0.0022(17) -0.0052(18)
C37 0.030(2) 0.034(2) 0.040(3) -0.0014(18) 0.0005(18) 0.0023(17)
C38 0.026(2) 0.046(2) 0.033(2) 0.0006(19) -0.0028(17) -0.0003(17)
C39 0.033(2) 0.043(2) 0.031(2) -0.0082(19) -0.0053(17) -0.0094(18)
C40 0.030(2) 0.0300(19) 0.032(2) -0.0072(17) -0.0059(16) -0.0033(16)
C41 0.035(2) 0.039(2) 0.026(2) -0.0012(17) -0.0063(17) -0.0058(17)
_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 C11 2.039(3) . ?
Fe1 C17 2.041(3) . ?
Fe1 C16 2.044(3) . ?
Fe1 C18 2.049(3) . ?
Fe1 C12 2.052(3) . ?
Fe1 C14 2.054(3) . ?
Fe1 C19 2.056(3) . ?
Fe1 C13 2.058(3) . ?
Fe1 C15 2.059(3) . ?
Fe1 C10 2.075(3) . ?
S1 C2 1.724(3) . ?
S1 C5 1.745(3) . ?
S2 C9 1.731(3) . ?
S2 C6 1.744(3) . ?
B1 C10 1.546(5) . ?
B1 C7 1.566(5) . ?
B1 C20 1.584(5) . ?
C1 C2 1.493(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.356(5) . ?
C3 C4 1.423(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.461(4) . ?
C6 C7 1.389(4) . ?
C7 C8 1.436(4) . ?
C8 C9 1.361(4) . ?
C8 H8 0.9300 . ?
C9 C9 1.445(6) 2_667 ?
C10 C11 1.438(4) . ?
C10 C14 1.448(4) . ?
C11 C12 1.416(4) . ?
C11 H11 0.9800 . ?
C12 C13 1.423(4) . ?
C12 H12 0.9800 . ?
C13 C14 1.419(4) . ?
C13 H13 0.9800 . ?
C14 H14 0.9800 . ?
C15 C19 1.414(5) . ?
C15 C16 1.427(5) . ?
C15 H15 0.9800 . ?
C16 C17 1.420(5) . ?
C16 H16 0.9800 . ?
C17 C18 1.422(5) . ?
C17 H17 0.9800 . ?
C18 C19 1.416(5) . ?
C18 H18 0.9800 . ?
C19 H19 0.9800 . ?
C20 C25 1.400(4) . ?
C20 C21 1.415(4) . ?
C21 C22 1.393(4) . ?
C21 C26 1.518(4) . ?
C22 C23 1.398(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(4) . ?
C23 C29 1.520(4) . ?
C24 C25 1.401(4) . ?
C24 H24 0.9300 . ?
C25 C32 1.520(4) . ?
C26 C27 1.527(4) . ?
C26 C28 1.534(5) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.513(4) . ?
C29 C31 1.528(5) . ?
C29 H29 0.9800 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.532(5) . ?
C32 C34 1.535(4) . ?
C32 H32 0.9800 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C40 1.390(5) . ?
C35 C36 1.391(5) . ?
C35 C41 1.499(5) . ?
C36 C37 1.385(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.376(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.377(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.381(5) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
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
C11 Fe1 C17 156.61(14) . . ?
C11 Fe1 C16 162.26(14) . . ?
C17 Fe1 C16 40.68(14) . . ?
C11 Fe1 C18 122.80(14) . . ?
C17 Fe1 C18 40.69(13) . . ?
C16 Fe1 C18 68.26(14) . . ?
C11 Fe1 C12 40.50(13) . . ?
C17 Fe1 C12 119.28(14) . . ?
C16 Fe1 C12 155.68(15) . . ?
C18 Fe1 C12 105.41(14) . . ?
C11 Fe1 C14 68.06(12) . . ?
C17 Fe1 C14 120.68(13) . . ?
C16 Fe1 C14 107.80(14) . . ?
C18 Fe1 C14 155.83(14) . . ?
C12 Fe1 C14 67.84(13) . . ?
C11 Fe1 C19 110.43(14) . . ?
C17 Fe1 C19 68.10(14) . . ?
C16 Fe1 C19 67.94(15) . . ?
C18 Fe1 C19 40.35(13) . . ?
C12 Fe1 C19 123.31(14) . . ?
C14 Fe1 C19 162.32(14) . . ?
C11 Fe1 C13 68.27(13) . . ?
C17 Fe1 C13 103.56(14) . . ?
C16 Fe1 C13 120.56(14) . . ?
C18 Fe1 C13 119.50(14) . . ?
C12 Fe1 C13 40.51(12) . . ?
C14 Fe1 C13 40.36(12) . . ?
C19 Fe1 C13 156.92(14) . . ?
C11 Fe1 C15 126.59(14) . . ?
C17 Fe1 C15 68.43(14) . . ?
C16 Fe1 C15 40.71(14) . . ?
C18 Fe1 C15 68.08(15) . . ?
C12 Fe1 C15 160.70(14) . . ?
C14 Fe1 C15 125.49(14) . . ?
C19 Fe1 C15 40.19(14) . . ?
C13 Fe1 C15 158.66(14) . . ?
C11 Fe1 C10 40.90(12) . . ?
C17 Fe1 C10 158.65(13) . . ?
C16 Fe1 C10 124.66(14) . . ?
C18 Fe1 C10 160.39(13) . . ?
C12 Fe1 C10 68.83(13) . . ?
C14 Fe1 C10 41.06(12) . . ?
C19 Fe1 C10 126.11(13) . . ?
C13 Fe1 C10 69.06(13) . . ?
C15 Fe1 C10 110.87(14) . . ?
C2 S1 C5 92.46(16) . . ?
C9 S2 C6 92.66(15) . . ?
C10 B1 C7 120.8(3) . . ?
C10 B1 C20 117.0(3) . . ?
C7 B1 C20 122.1(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 128.7(3) . . ?
C3 C2 S1 110.6(3) . . ?
C1 C2 S1 120.7(3) . . ?
C2 C3 C4 113.8(3) . . ?
C2 C3 H3 123.1 . . ?
C4 C3 H3 123.1 . . ?
C5 C4 C3 113.1(3) . . ?
C5 C4 H4 123.5 . . ?
C3 C4 H4 123.5 . . ?
C4 C5 C6 131.0(3) . . ?
C4 C5 S1 110.0(2) . . ?
C6 C5 S1 118.8(2) . . ?
C7 C6 C5 133.6(3) . . ?
C7 C6 S2 111.5(2) . . ?
C5 C6 S2 114.7(2) . . ?
C6 C7 C8 110.0(3) . . ?
C6 C7 B1 128.4(3) . . ?
C8 C7 B1 121.5(3) . . ?
C9 C8 C7 116.2(3) . . ?
C9 C8 H8 121.9 . . ?
C7 C8 H8 121.9 . . ?
C8 C9 C9 129.9(4) . 2_667 ?
C8 C9 S2 109.6(2) . . ?
C9 C9 S2 120.5(3) 2_667 . ?
C11 C10 C14 105.1(3) . . ?
C11 C10 B1 129.3(3) . . ?
C14 C10 B1 125.4(3) . . ?
C11 C10 Fe1 68.19(17) . . ?
C14 C10 Fe1 68.72(17) . . ?
B1 C10 Fe1 131.8(2) . . ?
C12 C11 C10 109.7(3) . . ?
C12 C11 Fe1 70.26(18) . . ?
C10 C11 Fe1 70.91(17) . . ?
C12 C11 H11 125.2 . . ?
C10 C11 H11 125.2 . . ?
Fe1 C11 H11 125.2 . . ?
C11 C12 C13 108.2(3) . . ?
C11 C12 Fe1 69.25(18) . . ?
C13 C12 Fe1 69.98(19) . . ?
C11 C12 H12 125.9 . . ?
C13 C12 H12 125.9 . . ?
Fe1 C12 H12 125.9 . . ?
C14 C13 C12 107.5(3) . . ?
C14 C13 Fe1 69.68(18) . . ?
C12 C13 Fe1 69.51(18) . . ?
C14 C13 H13 126.3 . . ?
C12 C13 H13 126.3 . . ?
Fe1 C13 H13 126.3 . . ?
C13 C14 C10 109.6(3) . . ?
C13 C14 Fe1 69.96(18) . . ?
C10 C14 Fe1 70.23(17) . . ?
C13 C14 H14 125.2 . . ?
C10 C14 H14 125.2 . . ?
Fe1 C14 H14 125.2 . . ?
C19 C15 C16 107.5(3) . . ?
C19 C15 Fe1 69.8(2) . . ?
C16 C15 Fe1 69.1(2) . . ?
C19 C15 H15 126.3 . . ?
C16 C15 H15 126.3 . . ?
Fe1 C15 H15 126.3 . . ?
C17 C16 C15 108.2(3) . . ?
C17 C16 Fe1 69.5(2) . . ?
C15 C16 Fe1 70.2(2) . . ?
C17 C16 H16 125.9 . . ?
C15 C16 H16 125.9 . . ?
Fe1 C16 H16 125.9 . . ?
C16 C17 C18 107.8(3) . . ?
C16 C17 Fe1 69.78(19) . . ?
C18 C17 Fe1 69.94(19) . . ?
C16 C17 H17 126.1 . . ?
C18 C17 H17 126.1 . . ?
Fe1 C17 H17 126.1 . . ?
C19 C18 C17 107.9(3) . . ?
C19 C18 Fe1 70.11(19) . . ?
C17 C18 Fe1 69.36(19) . . ?
C19 C18 H18 126.1 . . ?
C17 C18 H18 126.1 . . ?
Fe1 C18 H18 126.1 . . ?
C15 C19 C18 108.7(3) . . ?
C15 C19 Fe1 70.0(2) . . ?
C18 C19 Fe1 69.5(2) . . ?
C15 C19 H19 125.7 . . ?
C18 C19 H19 125.7 . . ?
Fe1 C19 H19 125.7 . . ?
C25 C20 C21 118.9(3) . . ?
C25 C20 B1 121.7(3) . . ?
C21 C20 B1 119.4(3) . . ?
C22 C21 C20 119.4(3) . . ?
C22 C21 C26 120.8(3) . . ?
C20 C21 C26 119.8(3) . . ?
C21 C22 C23 122.1(3) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
C24 C23 C22 117.7(3) . . ?
C24 C23 C29 119.9(3) . . ?
C22 C23 C29 122.4(3) . . ?
C23 C24 C25 122.1(3) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C20 C25 C24 119.7(3) . . ?
C20 C25 C32 121.2(3) . . ?
C24 C25 C32 119.1(3) . . ?
C21 C26 C27 113.7(3) . . ?
C21 C26 C28 111.1(3) . . ?
C27 C26 C28 110.5(3) . . ?
C21 C26 H26 107.1 . . ?
C27 C26 H26 107.1 . . ?
C28 C26 H26 107.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C23 113.4(3) . . ?
C30 C29 C31 111.8(3) . . ?
C23 C29 C31 110.8(3) . . ?
C30 C29 H29 106.8 . . ?
C23 C29 H29 106.8 . . ?
C31 C29 H29 106.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C32 C33 112.0(3) . . ?
C25 C32 C34 110.8(3) . . ?
C33 C32 C34 110.6(3) . . ?
C25 C32 H32 107.7 . . ?
C33 C32 H32 107.7 . . ?
C34 C32 H32 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C40 C35 C36 117.7(3) . . ?
C40 C35 C41 120.6(3) . . ?
C36 C35 C41 121.6(3) . . ?
C37 C36 C35 121.1(3) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C38 C37 C36 120.1(4) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C39 119.7(4) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C38 C39 C40 120.3(4) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C39 C40 C35 121.1(3) . . ?
C39 C40 H40 119.5 . . ?
C35 C40 H40 119.5 . . ?
C35 C41 H41A 109.5 . . ?
C35 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C35 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.914
_diffrn_reflns_theta_full 66.97
_diffrn_measured_fraction_theta_full 0.914
_refine_diff_density_max 0.500
_refine_diff_density_min -0.273
_refine_diff_density_rms 0.065