 
data_2006src1374
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr S. Aldridge
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C36 H40 B4 Fe2 O8'
_chemical_formula_weight          755.62

 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B'  'B'   0.0013   0.0007
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    'P bcn'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y+1/2, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y-1/2, -z-1/2'
 '-x-1/2, y-1/2, z'
 'x, -y, z-1/2'
 
_cell_length_a                    19.6222(11)
_cell_length_b                    7.8609(3)
_cell_length_c                    21.3982(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3300.6(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4105
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Brown
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.521
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1568
_exptl_absorpt_coefficient_mu     0.934
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8425
_exptl_absorpt_correction_T_max   0.9907
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'

 
_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 19154 reflections reduced R(int) from 0.2526 to 0.1054
Ratio of minimum to maximum apparent transmission: 0.669862
The given Tmin and Tmax were generated using the SHELX SIZE command.
;
 
_diffrn_ambient_temperature        120(2)
_diffrn_radiation_wavelength       0.71073
_diffrn_radiation_type             MoK\a
_diffrn_radiation_source           'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
    'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method         'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             25134
_diffrn_reflns_av_R_equivalents   0.1290
_diffrn_reflns_av_sigmaI/netI     0.0793
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.95
_diffrn_reflns_theta_max          26.37
_reflns_number_total              3366
_reflns_number_gt                 2254
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     
'Ortep3 for Windows (Farrugia, L.J., 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'

 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0000P)²+18.2477P] where P=(Fo²+2Fc²)/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          3366
_refine_ls_number_parameters      226
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1451
_refine_ls_R_factor_gt            0.0905
_refine_ls_wR_factor_ref          0.1676
_refine_ls_wR_factor_gt           0.1459
_refine_ls_goodness_of_fit_ref    1.219
_refine_ls_restrained_S_all       1.219
_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
C1 C 0.5953(3) 0.2405(8) 0.4634(3) 0.0303(15) Uani 1 1 d . . .
C2 C 0.6610(3) 0.1926(8) 0.4393(3) 0.0313(15) Uani 1 1 d . . .
H2 H 0.6702 0.0933 0.4155 0.038 Uiso 1 1 calc R . .
C3 C 0.7095(4) 0.3159(8) 0.4566(3) 0.0387(17) Uani 1 1 d . . .
H3 H 0.7565 0.3157 0.4459 0.046 Uiso 1 1 calc R . .
C4 C 0.6756(4) 0.4399(8) 0.4928(3) 0.0342(16) Uani 1 1 d . . .
H4 H 0.6962 0.5368 0.5115 0.041 Uiso 1 1 calc R . .
C5 C 0.6055(4) 0.3954(8) 0.4966(3) 0.0320(15) Uani 1 1 d . . .
H5 H 0.5713 0.4584 0.5178 0.038 Uiso 1 1 calc R . .
C6 C 0.6293(3) 0.4174(8) 0.3101(2) 0.0302(14) Uani 1 1 d . . .
C7 C 0.6692(4) 0.5590(8) 0.3318(3) 0.0336(15) Uani 1 1 d . . .
H7 H 0.7160 0.5791 0.3231 0.040 Uiso 1 1 calc R . .
C8 C 0.6256(4) 0.6638(8) 0.3688(3) 0.0367(17) Uani 1 1 d . . .
H8 H 0.6386 0.7666 0.3888 0.044 Uiso 1 1 calc R . .
C9 C 0.5609(4) 0.5916(8) 0.3708(3) 0.0382(17) Uani 1 1 d . . .
H9 H 0.5226 0.6358 0.3926 0.046 Uiso 1 1 calc R . .
C10 C 0.5621(3) 0.4419(8) 0.3350(3) 0.0326(15) Uani 1 1 d . . .
H10 H 0.5243 0.3684 0.3283 0.039 Uiso 1 1 calc R . .
C11 C 0.4505(3) -0.0236(7) 0.4009(3) 0.0298(14) Uani 1 1 d . . .
H11 H 0.4295 -0.1284 0.4192 0.036 Uiso 1 1 calc R . .
C12 C 0.4122(3) 0.1345(8) 0.4264(3) 0.0301(15) Uani 1 1 d . . .
H12 H 0.3854 0.1008 0.4642 0.036 Uiso 1 1 calc R . .
C13 C 0.3660(3) 0.2235(8) 0.3813(3) 0.0321(14) Uani 1 1 d . . .
H13A H 0.3915 0.2484 0.3425 0.039 Uiso 1 1 calc R . .
H13B H 0.3514 0.3334 0.3996 0.039 Uiso 1 1 calc R . .
C14 C 0.3024(3) 0.1176(8) 0.3651(3) 0.0330(15) Uani 1 1 d . . .
H14A H 0.3058 0.0066 0.3868 0.040 Uiso 1 1 calc R . .
H14B H 0.2618 0.1769 0.3816 0.040 Uiso 1 1 calc R . .
C15 C 0.2919(3) 0.0850(8) 0.2955(3) 0.0310(14) Uani 1 1 d . . .
H15 H 0.2470 0.0272 0.2894 0.037 Uiso 1 1 calc R . .
C16 C 0.3476(3) -0.0168(8) 0.2604(3) 0.0325(15) Uani 1 1 d . . .
H16 H 0.3239 -0.0903 0.2290 0.039 Uiso 1 1 calc R . .
C17 C 0.3968(4) -0.1314(8) 0.2968(3) 0.0339(15) Uani 1 1 d . . .
H17A H 0.3701 -0.1939 0.3286 0.041 Uiso 1 1 calc R . .
H17B H 0.4154 -0.2169 0.2673 0.041 Uiso 1 1 calc R . .
C18 C 0.4567(3) -0.0464(7) 0.3298(3) 0.0269(14) Uani 1 1 d . . .
H18A H 0.4637 0.0671 0.3108 0.032 Uiso 1 1 calc R . .
H18B H 0.4982 -0.1144 0.3212 0.032 Uiso 1 1 calc R . .
O1 O 0.5194(2) -0.0051(5) 0.42534(18) 0.0335(11) Uani 1 1 d . . .
O2 O 0.4665(2) 0.2486(5) 0.44525(18) 0.0315(10) Uani 1 1 d . . .
O3 O 0.2909(2) 0.2472(5) 0.26278(19) 0.0332(10) Uani 1 1 d . . .
O4 O 0.3857(2) 0.1106(5) 0.22565(17) 0.0325(11) Uani 1 1 d . . .
Fe1 Fe 0.63157(5) 0.42479(10) 0.40583(4) 0.0275(2) Uani 1 1 d . . .
B1 B 0.5271(4) 0.1592(9) 0.4453(3) 0.0286(17) Uani 1 1 d . . .
B2 B 0.3486(4) 0.2561(9) 0.2260(3) 0.0301(16) Uani 1 1 d . . .
 
 
_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
C1 C5 1.424(8) . ?
C1 C2 1.439(9) . ?
C1 B1 1.533(10) . ?
C1 Fe1 2.031(6) . ?
C2 C3 1.408(9) . ?
C2 Fe1 2.044(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.412(9) . ?
C3 Fe1 2.063(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.421(9) . ?
C4 Fe1 2.056(6) . ?
C4 H4 0.9500 . ?
C5 Fe1 2.023(6) . ?
C5 H5 0.9500 . ?
C6 C10 1.434(9) . ?
C6 C7 1.438(9) . ?
C6 B2 1.547(9) 4_655 ?
C6 Fe1 2.049(5) . ?
C7 C8 1.427(9) . ?
C7 Fe1 2.042(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.391(9) . ?
C8 Fe1 2.043(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(9) . ?
C9 Fe1 2.050(7) . ?
C9 H9 0.9500 . ?
C10 Fe1 2.043(6) . ?
C10 H10 0.9500 . ?
C11 O1 1.457(7) . ?
C11 C18 1.538(7) . ?
C11 C12 1.551(8) . ?
C11 H11 1.0000 . ?
C12 O2 1.450(7) . ?
C12 C13 1.498(8) . ?
C12 H12 1.0000 . ?
C13 C14 1.539(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.525(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O3 1.455(7) . ?
C15 C16 1.550(8) . ?
C15 H15 1.0000 . ?
C16 O4 1.454(7) . ?
C16 C17 1.532(9) . ?
C16 H16 1.0000 . ?
C17 C18 1.526(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
O1 B1 1.369(8) . ?
O2 B1 1.382(9) . ?
O3 B2 1.380(8) . ?
O4 B2 1.356(8) . ?
B2 C6 1.547(9) 4_655 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C5 C1 C2 106.1(6) . . ?
C5 C1 B1 127.3(6) . . ?
C2 C1 B1 125.6(6) . . ?
C5 C1 Fe1 69.1(3) . . ?
C2 C1 Fe1 69.8(3) . . ?
B1 C1 Fe1 116.7(4) . . ?
C3 C2 C1 109.3(6) . . ?
C3 C2 Fe1 70.7(4) . . ?
C1 C2 Fe1 68.8(3) . . ?
C3 C2 H2 125.3 . . ?
C1 C2 H2 125.3 . . ?
Fe1 C2 H2 126.8 . . ?
C2 C3 C4 107.5(6) . . ?
C2 C3 Fe1 69.2(4) . . ?
C4 C3 Fe1 69.7(4) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
Fe1 C3 H3 126.4 . . ?
C3 C4 C5 108.5(6) . . ?
C3 C4 Fe1 70.2(4) . . ?
C5 C4 Fe1 68.4(3) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Fe1 C4 H4 127.3 . . ?
C4 C5 C1 108.5(6) . . ?
C4 C5 Fe1 70.9(4) . . ?
C1 C5 Fe1 69.7(3) . . ?
C4 C5 H5 125.7 . . ?
C1 C5 H5 125.7 . . ?
Fe1 C5 H5 125.3 . . ?
C10 C6 C7 106.1(5) . . ?
C10 C6 B2 123.6(6) . 4_655 ?
C7 C6 B2 129.9(6) . 4_655 ?
C10 C6 Fe1 69.3(3) . . ?
C7 C6 Fe1 69.1(3) . . ?
B2 C6 Fe1 121.0(4) 4_655 . ?
C8 C7 C6 107.3(6) . . ?
C8 C7 Fe1 69.6(3) . . ?
C6 C7 Fe1 69.7(3) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
Fe1 C7 H7 126.0 . . ?
C9 C8 C7 109.2(6) . . ?
C9 C8 Fe1 70.4(4) . . ?
C7 C8 Fe1 69.5(3) . . ?
C9 C8 H8 125.4 . . ?
C7 C8 H8 125.4 . . ?
Fe1 C8 H8 126.3 . . ?
C8 C9 C10 108.1(6) . . ?
C8 C9 Fe1 69.8(4) . . ?
C10 C9 Fe1 69.7(4) . . ?
C8 C9 H9 126.0 . . ?
C10 C9 H9 126.0 . . ?
Fe1 C9 H9 126.1 . . ?
C9 C10 C6 109.2(6) . . ?
C9 C10 Fe1 70.2(4) . . ?
C6 C10 Fe1 69.7(3) . . ?
C9 C10 H10 125.4 . . ?
C6 C10 H10 125.4 . . ?
Fe1 C10 H10 126.3 . . ?
O1 C11 C18 107.0(5) . . ?
O1 C11 C12 104.1(5) . . ?
C18 C11 C12 118.7(5) . . ?
O1 C11 H11 108.9 . . ?
C18 C11 H11 108.9 . . ?
C12 C11 H11 108.9 . . ?
O2 C12 C13 109.6(5) . . ?
O2 C12 C11 103.8(5) . . ?
C13 C12 C11 116.2(5) . . ?
O2 C12 H12 109.0 . . ?
C13 C12 H12 109.0 . . ?
C11 C12 H12 109.0 . . ?
C12 C13 C14 112.5(5) . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 114.9(5) . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
O3 C15 C14 109.0(5) . . ?
O3 C15 C16 103.1(4) . . ?
C14 C15 C16 117.7(5) . . ?
O3 C15 H15 108.9 . . ?
C14 C15 H15 108.9 . . ?
C16 C15 H15 108.9 . . ?
O4 C16 C17 109.9(5) . . ?
O4 C16 C15 104.8(4) . . ?
C17 C16 C15 120.1(5) . . ?
O4 C16 H16 107.1 . . ?
C17 C16 H16 107.1 . . ?
C15 C16 H16 107.1 . . ?
C18 C17 C16 117.6(5) . . ?
C18 C17 H17A 107.9 . . ?
C16 C17 H17A 107.9 . . ?
C18 C17 H17B 107.9 . . ?
C16 C17 H17B 107.9 . . ?
H17A C17 H17B 107.2 . . ?
C17 C18 C11 116.6(5) . . ?
C17 C18 H18A 108.1 . . ?
C11 C18 H18A 108.1 . . ?
C17 C18 H18B 108.1 . . ?
C11 C18 H18B 108.1 . . ?
H18A C18 H18B 107.3 . . ?
B1 O1 C11 108.0(5) . . ?
B1 O2 C12 108.6(5) . . ?
B2 O3 C15 108.0(5) . . ?
B2 O4 C16 107.6(5) . . ?
C5 Fe1 C1 41.1(2) . . ?
C5 Fe1 C7 153.6(2) . . ?
C1 Fe1 C7 165.1(2) . . ?
C5 Fe1 C8 117.6(2) . . ?
C1 Fe1 C8 150.7(3) . . ?
C7 Fe1 C8 40.9(2) . . ?
C5 Fe1 C10 123.5(3) . . ?
C1 Fe1 C10 105.3(3) . . ?
C7 Fe1 C10 68.4(3) . . ?
C8 Fe1 C10 67.2(3) . . ?
C5 Fe1 C2 68.4(2) . . ?
C1 Fe1 C2 41.3(2) . . ?
C7 Fe1 C2 129.1(3) . . ?
C8 Fe1 C2 166.8(3) . . ?
C10 Fe1 C2 120.5(3) . . ?
C5 Fe1 C6 162.1(3) . . ?
C1 Fe1 C6 125.4(3) . . ?
C7 Fe1 C6 41.2(2) . . ?
C8 Fe1 C6 68.7(2) . . ?
C10 Fe1 C6 41.0(2) . . ?
C2 Fe1 C6 109.4(2) . . ?
C5 Fe1 C9 104.7(3) . . ?
C1 Fe1 C9 116.2(3) . . ?
C7 Fe1 C9 68.3(3) . . ?
C8 Fe1 C9 39.7(3) . . ?
C10 Fe1 C9 40.1(3) . . ?
C2 Fe1 C9 152.9(3) . . ?
C6 Fe1 C9 68.8(3) . . ?
C5 Fe1 C4 40.8(2) . . ?
C1 Fe1 C4 68.8(3) . . ?
C7 Fe1 C4 121.4(3) . . ?
C8 Fe1 C4 108.8(3) . . ?
C10 Fe1 C4 161.5(3) . . ?
C2 Fe1 C4 67.4(2) . . ?
C6 Fe1 C4 156.3(3) . . ?
C9 Fe1 C4 125.3(3) . . ?
C5 Fe1 C3 68.5(3) . . ?
C1 Fe1 C3 69.1(3) . . ?
C7 Fe1 C3 110.8(3) . . ?
C8 Fe1 C3 129.0(3) . . ?
C10 Fe1 C3 155.9(3) . . ?
C2 Fe1 C3 40.1(3) . . ?
C6 Fe1 C3 122.1(3) . . ?
C9 Fe1 C3 163.7(3) . . ?
C4 Fe1 C3 40.1(3) . . ?
O1 B1 O2 112.6(6) . . ?
O1 B1 C1 124.7(6) . . ?
O2 B1 C1 122.7(6) . . ?
O4 B2 O3 113.6(6) . . ?
O4 B2 C6 122.5(6) . 4_655 ?
O3 B2 C6 123.9(6) . 4_655 ?
 
_diffrn_measured_fraction_theta_max    0.995
_diffrn_reflns_theta_full              26.37
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.546
_refine_diff_density_min   -0.476
_refine_diff_density_rms    0.109
