data_2005src0348

_exptl_special_details
;
 Crystals were twinned (-180deg about 0 -1 0 direct axis)
 at 48.4%
;


 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. R. B. Bedford
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H28 Cl4 Fe P'
_chemical_formula_weight          497.04
 
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'
 'P'  'P'   0.1023   0.0942
 '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                    9.298(2)
_cell_length_b                    11.4767(16)
_cell_length_c                    11.5814(7)
_cell_angle_alpha                 90.229(10)
_cell_angle_beta                  99.187(8)
_cell_angle_gamma                 95.194(15)
_cell_volume                      1214.7(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5349
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Blade
_exptl_crystal_colour             'Light Yellow'
_exptl_crystal_size_max           0.33
_exptl_crystal_size_mid           0.17
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.359
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              514
_exptl_absorpt_coefficient_mu     1.129
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7069
_exptl_absorpt_correction_T_max   0.9778
 _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    'graphite'
_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             16853
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0840
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          4.89
_diffrn_reflns_theta_max          27.48
_reflns_number_total              16853
_reflns_number_gt                 11859
_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)+(0.0962P)²+15.3879P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0
_refine_ls_number_reflns          16853
_refine_ls_number_parameters      247
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1614
_refine_ls_R_factor_gt            0.1092
_refine_ls_wR_factor_ref          0.2889
_refine_ls_wR_factor_gt           0.2440
_refine_ls_goodness_of_fit_ref    1.128
_refine_ls_restrained_S_all       1.128
_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 0.0502(6) 0.2416(5) 0.1308(4) 0.0182(12) Uani 1 1 d . . .
C2 C 0.0845(6) 0.2251(5) 0.0197(5) 0.0238(13) Uani 1 1 d . . .
H2 H 0.1788 0.2040 0.0110 0.029 Uiso 1 1 calc R . .
C3 C -0.0189(7) 0.2393(5) -0.0783(5) 0.0278(14) Uani 1 1 d . . .
H3 H 0.0054 0.2295 -0.1541 0.033 Uiso 1 1 calc R . .
C4 C -0.1580(7) 0.2680(6) -0.0665(5) 0.0307(15) Uani 1 1 d . . .
H4 H -0.2299 0.2738 -0.1339 0.037 Uiso 1 1 calc R . .
C5 C -0.1914(6) 0.2880(6) 0.0431(5) 0.0283(14) Uani 1 1 d . . .
H5 H -0.2849 0.3117 0.0501 0.034 Uiso 1 1 calc R . .
C6 C -0.0902(6) 0.2741(6) 0.1451(5) 0.0219(12) Uani 1 1 d . . .
C7 C -0.1321(6) 0.2986(6) 0.2612(5) 0.0240(13) Uani 1 1 d . . .
C8 C -0.1771(6) 0.2100(6) 0.3297(5) 0.0294(14) Uani 1 1 d . . .
H8 H -0.1847 0.1312 0.3023 0.035 Uiso 1 1 calc R . .
C9 C -0.2121(7) 0.2351(7) 0.4405(6) 0.0345(17) Uani 1 1 d . . .
H9 H -0.2411 0.1733 0.4887 0.041 Uiso 1 1 calc R . .
C10 C -0.2040(7) 0.3498(7) 0.4786(6) 0.0366(17) Uani 1 1 d . . .
H10 H -0.2285 0.3673 0.5529 0.044 Uiso 1 1 calc R . .
C11 C -0.1607(8) 0.4385(7) 0.4095(7) 0.0390(18) Uani 1 1 d . . .
H11 H -0.1552 0.5174 0.4361 0.047 Uiso 1 1 calc R . .
C12 C -0.1250(7) 0.4135(6) 0.3011(6) 0.0332(16) Uani 1 1 d . . .
H12 H -0.0953 0.4756 0.2536 0.040 Uiso 1 1 calc R . .
C13 C 0.3383(6) 0.3552(5) 0.2529(5) 0.0199(12) Uani 1 1 d . . .
C14 C 0.4571(6) 0.3215(6) 0.1856(5) 0.0281(14) Uani 1 1 d . . .
H14A H 0.5288 0.3891 0.1829 0.042 Uiso 1 1 calc R . .
H14B H 0.4128 0.2967 0.1058 0.042 Uiso 1 1 calc R . .
H14C H 0.5060 0.2570 0.2250 0.042 Uiso 1 1 calc R . .
C15 C 0.4058(7) 0.3892(6) 0.3807(5) 0.0255(14) Uani 1 1 d . . .
H15A H 0.4445 0.3208 0.4204 0.038 Uiso 1 1 calc R . .
H15B H 0.3304 0.4170 0.4214 0.038 Uiso 1 1 calc R . .
H15C H 0.4853 0.4516 0.3811 0.038 Uiso 1 1 calc R . .
C16 C 0.2658(7) 0.4607(6) 0.1956(6) 0.0306(16) Uani 1 1 d . . .
H16A H 0.1891 0.4813 0.2389 0.046 Uiso 1 1 calc R . .
H16B H 0.2225 0.4404 0.1144 0.046 Uiso 1 1 calc R . .
H16C H 0.3396 0.5275 0.1969 0.046 Uiso 1 1 calc R . .
C17 C 0.2468(7) 0.0845(5) 0.2768(5) 0.0229(13) Uani 1 1 d . . .
C18 C 0.2925(8) 0.0333(6) 0.1689(6) 0.0305(16) Uani 1 1 d . . .
H18A H 0.3233 -0.0451 0.1859 0.046 Uiso 1 1 calc R . .
H18B H 0.3741 0.0837 0.1466 0.046 Uiso 1 1 calc R . .
H18C H 0.2098 0.0283 0.1045 0.046 Uiso 1 1 calc R . .
C19 C 0.3723(7) 0.0838(6) 0.3807(5) 0.0264(15) Uani 1 1 d . . .
H19A H 0.3420 0.1164 0.4504 0.040 Uiso 1 1 calc R . .
H19B H 0.4585 0.1313 0.3625 0.040 Uiso 1 1 calc R . .
H19C H 0.3963 0.0032 0.3955 0.040 Uiso 1 1 calc R . .
C20 C 0.1114(7) 0.0120(6) 0.3086(6) 0.0309(15) Uani 1 1 d . . .
H20A H 0.0296 0.0135 0.2439 0.046 Uiso 1 1 calc R . .
H20B H 0.0846 0.0453 0.3794 0.046 Uiso 1 1 calc R . .
H20C H 0.1340 -0.0690 0.3227 0.046 Uiso 1 1 calc R . .
P1 P 0.19233(15) 0.23558(14) 0.25542(12) 0.0177(3) Uani 1 1 d . . .
H1P H 0.132(5) 0.259(5) 0.348(4) 0.008(13) Uiso 1 1 d . . .
Cl1 Cl 0.84905(17) 0.77830(18) 0.39202(14) 0.0380(4) Uani 1 1 d . . .
Cl2 Cl 0.6713(2) 0.93360(15) 0.14920(16) 0.0377(4) Uani 1 1 d . . .
Cl3 Cl 0.45604(15) 0.76380(15) 0.33382(12) 0.0271(4) Uani 1 1 d . . .
Cl4 Cl 0.6465(2) 0.62261(15) 0.13807(15) 0.0368(4) Uani 1 1 d . . .
Fe1 Fe 0.65592(9) 0.77549(8) 0.25284(7) 0.0238(3) 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 C2 1.391(8) . ?
C1 C6 1.423(8) . ?
C1 P1 1.801(5) . ?
C2 C3 1.386(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.491(8) . ?
C7 C8 1.368(10) . ?
C7 C12 1.388(9) . ?
C8 C9 1.409(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.368(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.525(8) . ?
C13 C16 1.540(8) . ?
C13 C15 1.547(8) . ?
C13 P1 1.844(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.515(8) . ?
C17 C19 1.538(8) . ?
C17 C20 1.541(9) . ?
C17 P1 1.856(6) . ?
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 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
P1 H1P 1.33(5) . ?
Cl1 Fe1 2.2110(17) . ?
Cl2 Fe1 2.186(2) . ?
Cl3 Fe1 2.2053(17) . ?
Cl4 Fe1 2.1839(18) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 C1 C6 120.6(5) . . ?
C2 C1 P1 118.6(4) . . ?
C6 C1 P1 120.5(4) . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 120.6(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.6(5) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 117.4(5) . . ?
C5 C6 C7 119.0(5) . . ?
C1 C6 C7 123.5(4) . . ?
C8 C7 C12 119.2(6) . . ?
C8 C7 C6 121.4(6) . . ?
C12 C7 C6 119.5(6) . . ?
C7 C8 C9 120.3(7) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.5(7) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C9 120.1(6) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.2(7) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.6(7) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
C14 C13 C16 110.0(5) . . ?
C14 C13 C15 110.0(5) . . ?
C16 C13 C15 108.5(5) . . ?
C14 C13 P1 112.6(4) . . ?
C16 C13 P1 107.3(4) . . ?
C15 C13 P1 108.2(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C19 109.7(5) . . ?
C18 C17 C20 110.6(5) . . ?
C19 C17 C20 108.5(5) . . ?
C18 C17 P1 112.9(4) . . ?
C19 C17 P1 109.5(4) . . ?
C20 C17 P1 105.4(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 P1 C13 110.9(3) . . ?
C1 P1 C17 111.0(3) . . ?
C13 P1 C17 117.9(3) . . ?
C1 P1 H1P 106(2) . . ?
C13 P1 H1P 105(2) . . ?
C17 P1 H1P 105(2) . . ?
Cl4 Fe1 Cl2 108.93(7) . . ?
Cl4 Fe1 Cl3 108.40(8) . . ?
Cl2 Fe1 Cl3 110.81(8) . . ?
Cl4 Fe1 Cl1 110.05(8) . . ?
Cl2 Fe1 Cl1 109.57(8) . . ?
Cl3 Fe1 Cl1 109.06(7) . . ?
 
_diffrn_measured_fraction_theta_max    0.883
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.883
_refine_diff_density_max    1.042
_refine_diff_density_min   -0.842
_refine_diff_density_rms    0.207
