data_05src0094
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. R. B. Bedford
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C26 H22 Cl Fe N2 O2, C H2 Cl2'
_chemical_formula_sum
 'C27 H24 Cl3 Fe N2 O2'
_chemical_formula_weight          570.68
 
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'
 'N'  'N'   0.0061   0.0033
 '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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            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                    10.9613(6)
_cell_length_b                    11.0481(8)
_cell_length_c                    11.1915(7)
_cell_angle_alpha                 109.102(5)
_cell_angle_beta                  100.330(5)
_cell_angle_gamma                 96.187(6)
_cell_volume                      1239.56(14)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5303
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             'Dark Red'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.529
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              586
_exptl_absorpt_coefficient_mu     0.961
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6999
_exptl_absorpt_correction_T_max   0.8311
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             18761
_diffrn_reflns_av_R_equivalents   0.0310
_diffrn_reflns_av_sigmaI/netI     0.0355
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.00
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5641
_reflns_number_gt                 4701
_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, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_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)+(0.0375P)²+0.7101P] 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          5641
_refine_ls_number_parameters      318
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0455
_refine_ls_R_factor_gt            0.0336
_refine_ls_wR_factor_ref          0.0850
_refine_ls_wR_factor_gt           0.0792
_refine_ls_goodness_of_fit_ref    1.041
_refine_ls_restrained_S_all       1.041
_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
C1 C 0.34198(17) 0.5234(2) 0.7355(2) 0.0268(4) Uani 1 1 d . . .
H1A H 0.3227 0.5983 0.7101 0.032 Uiso 1 1 calc R . .
H1B H 0.2787 0.5033 0.7825 0.032 Uiso 1 1 calc R . .
C2 C 0.33603(19) 0.4067(2) 0.6158(2) 0.0318(5) Uani 1 1 d . . .
H2A H 0.2470 0.3686 0.5707 0.038 Uiso 1 1 calc R . .
H2B H 0.3785 0.4339 0.5553 0.038 Uiso 1 1 calc R . .
C3 C 0.50335(18) 0.66899(19) 0.91408(18) 0.0222(4) Uani 1 1 d . . .
C4 C 0.62893(18) 0.70734(18) 1.00106(18) 0.0219(4) Uani 1 1 d . . .
C5 C 0.70571(17) 0.61539(17) 1.01137(17) 0.0184(4) Uani 1 1 d . . .
C6 C 0.82935(17) 0.65856(18) 1.09820(17) 0.0211(4) Uani 1 1 d . . .
C7 C 0.90850(17) 0.5679(2) 1.10840(18) 0.0242(4) Uani 1 1 d . . .
H7 H 0.8797 0.4780 1.0591 0.029 Uiso 1 1 calc R . .
C8 C 1.02685(18) 0.6088(2) 1.18902(19) 0.0306(5) Uani 1 1 d . . .
H8 H 1.0796 0.5472 1.1949 0.037 Uiso 1 1 calc R . .
C9 C 1.0700(2) 0.7414(2) 1.2627(2) 0.0373(5) Uani 1 1 d . . .
H9 H 1.1516 0.7691 1.3190 0.045 Uiso 1 1 calc R . .
C10 C 0.9953(2) 0.8304(2) 1.2539(2) 0.0371(5) Uani 1 1 d . . .
H10 H 1.0257 0.9197 1.3047 0.045 Uiso 1 1 calc R . .
C11 C 0.87316(19) 0.7926(2) 1.17042(19) 0.0273(4) Uani 1 1 d . . .
C12 C 0.7943(2) 0.8829(2) 1.1566(2) 0.0330(5) Uani 1 1 d . . .
H12 H 0.8232 0.9732 1.2041 0.040 Uiso 1 1 calc R . .
C13 C 0.6782(2) 0.84175(19) 1.07618(19) 0.0297(5) Uani 1 1 d . . .
H13 H 0.6273 0.9046 1.0693 0.036 Uiso 1 1 calc R . .
C14 C 0.4128(2) 0.7634(2) 0.9339(2) 0.0319(5) Uani 1 1 d . . .
H14A H 0.4056 0.8009 0.8653 0.048 Uiso 1 1 calc R . .
H14B H 0.4441 0.8331 1.0187 0.048 Uiso 1 1 calc R . .
H14C H 0.3299 0.7175 0.9305 0.048 Uiso 1 1 calc R . .
C15 C 0.34931(16) 0.18634(19) 0.60801(17) 0.0207(4) Uani 1 1 d . . .
C16 C 0.41847(17) 0.08937(18) 0.63717(17) 0.0203(4) Uani 1 1 d . . .
C17 C 0.54084(17) 0.12269(17) 0.71622(16) 0.0179(4) Uani 1 1 d . . .
C18 C 0.60496(17) 0.02189(17) 0.73992(17) 0.0197(4) Uani 1 1 d . . .
C19 C 0.72725(18) 0.05411(18) 0.82095(18) 0.0219(4) Uani 1 1 d . . .
H19 H 0.7678 0.1426 0.8606 0.026 Uiso 1 1 calc R . .
C20 C 0.7878(2) -0.0420(2) 0.84273(19) 0.0276(4) Uani 1 1 d . . .
H20 H 0.8702 -0.0195 0.8971 0.033 Uiso 1 1 calc R . .
C21 C 0.7286(2) -0.1732(2) 0.7850(2) 0.0309(5) Uani 1 1 d . . .
H21 H 0.7710 -0.2390 0.8006 0.037 Uiso 1 1 calc R . .
C22 C 0.6102(2) -0.20654(19) 0.7063(2) 0.0298(5) Uani 1 1 d . . .
H22 H 0.5714 -0.2957 0.6671 0.036 Uiso 1 1 calc R . .
C23 C 0.54457(19) -0.11027(18) 0.68240(19) 0.0244(4) Uani 1 1 d . . .
C24 C 0.4205(2) -0.1409(2) 0.6035(2) 0.0297(5) Uani 1 1 d . . .
H24 H 0.3785 -0.2290 0.5650 0.036 Uiso 1 1 calc R . .
C25 C 0.36179(19) -0.0457(2) 0.58280(19) 0.0280(4) Uani 1 1 d . . .
H25 H 0.2788 -0.0695 0.5296 0.034 Uiso 1 1 calc R . .
C26 C 0.21883(18) 0.1363(2) 0.5203(2) 0.0320(5) Uani 1 1 d . . .
H26A H 0.1738 0.2093 0.5258 0.048 Uiso 1 1 calc R . .
H26B H 0.1725 0.0731 0.5478 0.048 Uiso 1 1 calc R . .
H26C H 0.2256 0.0942 0.4305 0.048 Uiso 1 1 calc R . .
N1 N 0.46926(14) 0.55654(15) 0.82045(15) 0.0200(3) Uani 1 1 d . . .
N2 N 0.39839(14) 0.30931(16) 0.65373(15) 0.0230(3) Uani 1 1 d . . .
O1 O 0.67100(11) 0.48947(12) 0.94785(12) 0.0195(3) Uani 1 1 d . . .
O2 O 0.60324(11) 0.24228(12) 0.77331(12) 0.0205(3) Uani 1 1 d . . .
Cl1 Cl 0.68460(4) 0.46679(4) 0.64599(4) 0.02086(11) Uani 1 1 d . . .
Fe1 Fe 0.57377(2) 0.40744(2) 0.77521(2) 0.01586(8) Uani 1 1 d . . .
C31 C 0.9962(2) 0.3552(3) 1.3173(2) 0.0499(7) Uani 1 1 d . . .
H31A H 1.0893 0.3664 1.3399 0.060 Uiso 1 1 calc R . .
H31B H 0.9739 0.4402 1.3194 0.060 Uiso 1 1 calc R . .
Cl31 Cl 0.93931(7) 0.24111(7) 1.15939(7) 0.0591(2) Uani 1 1 d . . .
Cl32 Cl 0.93581(7) 0.30979(8) 1.43408(9) 0.0673(2) 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 N1 1.473(2) . ?
C1 C2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.470(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.299(2) . ?
C3 C4 1.465(3) . ?
C3 C14 1.508(3) . ?
C4 C5 1.407(3) . ?
C4 C13 1.432(3) . ?
C5 O1 1.314(2) . ?
C5 C6 1.447(3) . ?
C6 C7 1.413(3) . ?
C6 C11 1.415(3) . ?
C7 C8 1.374(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.362(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.420(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.416(3) . ?
C12 C13 1.354(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N2 1.298(2) . ?
C15 C16 1.464(3) . ?
C15 C26 1.512(2) . ?
C16 C17 1.404(3) . ?
C16 C25 1.433(3) . ?
C17 O2 1.311(2) . ?
C17 C18 1.449(3) . ?
C18 C19 1.413(3) . ?
C18 C23 1.417(3) . ?
C19 C20 1.375(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.405(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.368(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.415(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.420(3) . ?
C24 C25 1.352(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N1 Fe1 2.0860(15) . ?
N2 Fe1 2.0900(15) . ?
O1 Fe1 1.8968(12) . ?
O2 Fe1 1.8811(13) . ?
Cl1 Fe1 2.2530(5) . ?
C31 Cl32 1.750(3) . ?
C31 Cl31 1.755(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
 
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
N1 C1 C2 109.23(15) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 109.40(16) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 121.50(16) . . ?
N1 C3 C14 119.73(18) . . ?
C4 C3 C14 118.76(18) . . ?
C5 C4 C13 118.04(18) . . ?
C5 C4 C3 121.76(17) . . ?
C13 C4 C3 120.18(18) . . ?
O1 C5 C4 123.73(16) . . ?
O1 C5 C6 116.71(16) . . ?
C4 C5 C6 119.54(17) . . ?
C7 C6 C11 119.60(18) . . ?
C7 C6 C5 120.35(17) . . ?
C11 C6 C5 120.03(18) . . ?
C8 C7 C6 120.52(19) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 120.2(2) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 121.5(2) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C6 C11 C12 119.07(19) . . ?
C6 C11 C10 118.0(2) . . ?
C12 C11 C10 122.9(2) . . ?
C13 C12 C11 120.63(19) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C4 122.7(2) . . ?
C12 C13 H13 118.7 . . ?
C4 C13 H13 118.7 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 121.60(16) . . ?
N2 C15 C26 121.52(18) . . ?
C16 C15 C26 116.88(17) . . ?
C17 C16 C25 117.54(18) . . ?
C17 C16 C15 122.61(17) . . ?
C25 C16 C15 119.85(17) . . ?
O2 C17 C16 124.00(17) . . ?
O2 C17 C18 116.05(15) . . ?
C16 C17 C18 119.95(16) . . ?
C19 C18 C23 119.43(17) . . ?
C19 C18 C17 120.59(16) . . ?
C23 C18 C17 119.97(17) . . ?
C20 C19 C18 120.34(18) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 120.3(2) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 120.29(19) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 120.95(19) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C18 118.63(19) . . ?
C22 C23 C24 122.58(19) . . ?
C18 C23 C24 118.80(18) . . ?
C25 C24 C23 120.50(18) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C24 C25 C16 123.24(19) . . ?
C24 C25 H25 118.4 . . ?
C16 C25 H25 118.4 . . ?
C15 C26 H26A 109.5 . . ?
C15 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C15 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 N1 C1 119.17(15) . . ?
C3 N1 Fe1 127.41(12) . . ?
C1 N1 Fe1 113.40(12) . . ?
C15 N2 C2 122.57(16) . . ?
C15 N2 Fe1 130.58(13) . . ?
C2 N2 Fe1 106.70(12) . . ?
C5 O1 Fe1 126.55(11) . . ?
C17 O2 Fe1 135.51(11) . . ?
O2 Fe1 O1 91.93(5) . . ?
O2 Fe1 N1 149.74(6) . . ?
O1 Fe1 N1 85.92(6) . . ?
O2 Fe1 N2 85.66(6) . . ?
O1 Fe1 N2 147.18(6) . . ?
N1 Fe1 N2 80.18(6) . . ?
O2 Fe1 Cl1 108.26(4) . . ?
O1 Fe1 Cl1 106.72(4) . . ?
N1 Fe1 Cl1 101.23(4) . . ?
N2 Fe1 Cl1 105.10(5) . . ?
Cl32 C31 Cl31 113.07(15) . . ?
Cl32 C31 H31A 109.0 . . ?
Cl31 C31 H31A 109.0 . . ?
Cl32 C31 H31B 109.0 . . ?
Cl31 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.528
_refine_diff_density_min   -0.593
_refine_diff_density_rms    0.062
