data_04src0551
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. Ian Butler
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C30 H52 Fe P2'
_chemical_formula_sum
 'C30 H52 Fe P2'
_chemical_formula_weight          530.51
 
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'
 'Fe'  'Fe'   0.3463   0.8444
 '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   '-C 2yc'
 
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                    24.578(5)
_cell_length_b                    9.3330(19)
_cell_length_c                    15.288(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  123.25(3)
_cell_angle_gamma                 90.00
_cell_volume                      2932.6(14)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3565
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.22
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.202
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1152
_exptl_absorpt_coefficient_mu     0.639
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8216
_exptl_absorpt_correction_T_max   0.9749
_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             25472
_diffrn_reflns_av_R_equivalents   0.0614
_diffrn_reflns_av_sigmaI/netI     0.0407
_diffrn_reflns_limit_h_min        -31
_diffrn_reflns_limit_h_max        31
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.47
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3356
_reflns_number_gt                 2689
_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)+(0.0268P)²+3.5438P] 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          3356
_refine_ls_number_parameters      158
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0524
_refine_ls_R_factor_gt            0.0341
_refine_ls_wR_factor_ref          0.0770
_refine_ls_wR_factor_gt           0.0701
_refine_ls_goodness_of_fit_ref    1.039
_refine_ls_restrained_S_all       1.039
_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 0.07080(8) 0.21397(18) 0.22177(13) 0.0174(4) Uani 1 1 d . . .
C2 C 0.05442(8) 0.36429(19) 0.20448(13) 0.0191(4) Uani 1 1 d . . .
C3 C -0.01271(8) 0.3774(2) 0.12443(13) 0.0213(4) Uani 1 1 d . . .
C4 C -0.03897(8) 0.2373(2) 0.09101(13) 0.0199(4) Uani 1 1 d . . .
C5 C 0.01173(8) 0.13519(19) 0.15046(13) 0.0189(4) Uani 1 1 d . . .
C6 C 0.10009(9) 0.48856(19) 0.25443(15) 0.0258(4) Uani 1 1 d . . .
H6A H 0.1169 0.5159 0.2116 0.039 Uiso 1 1 calc R . .
H6B H 0.1364 0.4612 0.3245 0.039 Uiso 1 1 calc R . .
H6C H 0.0768 0.5699 0.2598 0.039 Uiso 1 1 calc R . .
C7 C -0.04873(9) 0.5148(2) 0.07560(16) 0.0308(5) Uani 1 1 d . . .
H7A H -0.0305 0.5912 0.1282 0.046 Uiso 1 1 calc R . .
H7B H -0.0949 0.5019 0.0491 0.046 Uiso 1 1 calc R . .
H7C H -0.0443 0.5409 0.0177 0.046 Uiso 1 1 calc R . .
C8 C -0.10768(9) 0.2080(2) 0.00096(14) 0.0278(4) Uani 1 1 d . . .
H8A H -0.1128 0.2377 -0.0646 0.042 Uiso 1 1 calc R . .
H8B H -0.1381 0.2619 0.0109 0.042 Uiso 1 1 calc R . .
H8C H -0.1168 0.1053 -0.0019 0.042 Uiso 1 1 calc R . .
C9 C 0.00499(9) -0.02412(19) 0.13547(14) 0.0231(4) Uani 1 1 d . . .
H9A H -0.0412 -0.0502 0.0967 0.035 Uiso 1 1 calc R . .
H9B H 0.0280 -0.0715 0.2039 0.035 Uiso 1 1 calc R . .
H9C H 0.0237 -0.0547 0.0960 0.035 Uiso 1 1 calc R . .
C10 C 0.17152(8) 0.1087(2) 0.20119(13) 0.0225(4) Uani 1 1 d . . .
H10 H 0.1491 0.0153 0.1707 0.027 Uiso 1 1 calc R . .
C11 C 0.24494(9) 0.0886(3) 0.25361(16) 0.0356(5) Uani 1 1 d . . .
H11A H 0.2535 0.0508 0.2025 0.053 Uiso 1 1 calc R . .
H11B H 0.2613 0.0212 0.3120 0.053 Uiso 1 1 calc R . .
H11C H 0.2669 0.1811 0.2799 0.053 Uiso 1 1 calc R . .
C12 C 0.14536(9) 0.2201(2) 0.11413(14) 0.0266(4) Uani 1 1 d . . .
H12A H 0.1642 0.3139 0.1444 0.040 Uiso 1 1 calc R . .
H12B H 0.0979 0.2251 0.0773 0.040 Uiso 1 1 calc R . .
H12C H 0.1572 0.1927 0.0648 0.040 Uiso 1 1 calc R . .
C13 C 0.16486(8) -0.00708(19) 0.37286(13) 0.0210(4) Uani 1 1 d . . .
H13 H 0.1286 -0.0095 0.3845 0.025 Uiso 1 1 calc R . .
C14 C 0.22879(9) 0.0010(2) 0.48165(14) 0.0277(4) Uani 1 1 d . . .
H14A H 0.2323 -0.0831 0.5229 0.042 Uiso 1 1 calc R . .
H14B H 0.2290 0.0881 0.5175 0.042 Uiso 1 1 calc R . .
H14C H 0.2657 0.0030 0.4737 0.042 Uiso 1 1 calc R . .
C15 C 0.16318(10) -0.1495(2) 0.32242(15) 0.0293(4) Uani 1 1 d . . .
H15A H 0.2021 -0.1580 0.3200 0.044 Uiso 1 1 calc R . .
H15B H 0.1242 -0.1534 0.2512 0.044 Uiso 1 1 calc R . .
H15C H 0.1621 -0.2285 0.3637 0.044 Uiso 1 1 calc R . .
P1 P 0.15665(2) 0.16510(5) 0.30333(3) 0.01731(11) Uani 1 1 d . . .
Fe1 Fe 0.0000 0.26191(4) 0.2500 0.01556(10) Uani 1 2 d S . .
 
 
_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 1.443(2) . ?
C1 C5 1.450(2) . ?
C1 P1 1.8247(18) . ?
C1 Fe1 2.0585(17) . ?
C2 C3 1.422(2) . ?
C2 C6 1.499(2) . ?
C2 Fe1 2.0511(17) . ?
C3 C4 1.423(3) . ?
C3 C7 1.504(3) . ?
C3 Fe1 2.0702(17) . ?
C4 C5 1.430(2) . ?
C4 C8 1.507(2) . ?
C4 Fe1 2.0796(17) . ?
C5 C9 1.500(2) . ?
C5 Fe1 2.0685(17) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.525(2) . ?
C10 C11 1.532(3) . ?
C10 P1 1.8640(18) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.526(3) . ?
C13 C14 1.541(2) . ?
C13 P1 1.8755(18) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
Fe1 C2 2.0511(17) 2 ?
Fe1 C1 2.0585(17) 2 ?
Fe1 C5 2.0685(17) 2 ?
Fe1 C3 2.0702(17) 2 ?
Fe1 C4 2.0796(17) 2 ?
 
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 C5 106.95(14) . . ?
C2 C1 P1 118.03(12) . . ?
C5 C1 P1 133.88(13) . . ?
C2 C1 Fe1 69.16(9) . . ?
C5 C1 Fe1 69.81(9) . . ?
P1 C1 Fe1 134.81(9) . . ?
C3 C2 C1 108.45(15) . . ?
C3 C2 C6 124.30(16) . . ?
C1 C2 C6 127.08(15) . . ?
C3 C2 Fe1 70.55(10) . . ?
C1 C2 Fe1 69.71(9) . . ?
C6 C2 Fe1 129.27(13) . . ?
C2 C3 C4 108.32(15) . . ?
C2 C3 C7 126.16(17) . . ?
C4 C3 C7 125.28(16) . . ?
C2 C3 Fe1 69.10(10) . . ?
C4 C3 Fe1 70.30(10) . . ?
C7 C3 Fe1 130.74(13) . . ?
C3 C4 C5 108.57(15) . . ?
C3 C4 C8 123.72(16) . . ?
C5 C4 C8 127.50(17) . . ?
C3 C4 Fe1 69.60(10) . . ?
C5 C4 Fe1 69.42(10) . . ?
C8 C4 Fe1 130.91(13) . . ?
C4 C5 C1 107.71(15) . . ?
C4 C5 C9 125.38(15) . . ?
C1 C5 C9 126.80(15) . . ?
C4 C5 Fe1 70.25(10) . . ?
C1 C5 Fe1 69.07(9) . . ?
C9 C5 Fe1 129.12(12) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C11 110.59(16) . . ?
C12 C10 P1 110.87(13) . . ?
C11 C10 P1 108.19(13) . . ?
C12 C10 H10 109.0 . . ?
C11 C10 H10 109.1 . . ?
P1 C10 H10 109.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C14 108.47(15) . . ?
C15 C13 P1 119.69(13) . . ?
C14 C13 P1 107.41(12) . . ?
C15 C13 H13 106.9 . . ?
C14 C13 H13 106.9 . . ?
P1 C13 H13 106.9 . . ?
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 . . ?
C1 P1 C10 100.52(8) . . ?
C1 P1 C13 109.04(8) . . ?
C10 P1 C13 102.90(8) . . ?
C2 Fe1 C2 124.47(10) 2 . ?
C2 Fe1 C1 41.12(7) 2 2 ?
C2 Fe1 C1 162.90(7) . 2 ?
C2 Fe1 C1 162.90(7) 2 . ?
C2 Fe1 C1 41.12(7) . . ?
C1 Fe1 C1 154.90(10) 2 . ?
C2 Fe1 C5 153.61(7) 2 . ?
C2 Fe1 C5 68.71(7) . . ?
C1 Fe1 C5 120.31(7) 2 . ?
C1 Fe1 C5 41.13(7) . . ?
C2 Fe1 C5 68.71(7) 2 2 ?
C2 Fe1 C5 153.61(7) . 2 ?
C1 Fe1 C5 41.13(7) 2 2 ?
C1 Fe1 C5 120.31(7) . 2 ?
C5 Fe1 C5 110.25(10) . 2 ?
C2 Fe1 C3 40.35(7) 2 2 ?
C2 Fe1 C3 106.09(7) . 2 ?
C1 Fe1 C3 68.52(7) 2 2 ?
C1 Fe1 C3 126.32(7) . 2 ?
C5 Fe1 C3 165.63(7) . 2 ?
C5 Fe1 C3 68.07(7) 2 2 ?
C2 Fe1 C3 106.09(7) 2 . ?
C2 Fe1 C3 40.35(7) . . ?
C1 Fe1 C3 126.32(7) 2 . ?
C1 Fe1 C3 68.52(7) . . ?
C5 Fe1 C3 68.07(7) . . ?
C5 Fe1 C3 165.63(7) 2 . ?
C3 Fe1 C3 117.28(10) 2 . ?
C2 Fe1 C4 118.67(7) 2 . ?
C2 Fe1 C4 67.85(7) . . ?
C1 Fe1 C4 108.69(7) 2 . ?
C1 Fe1 C4 68.38(7) . . ?
C5 Fe1 C4 40.33(7) . . ?
C5 Fe1 C4 129.50(7) 2 . ?
C3 Fe1 C4 151.62(7) 2 . ?
C3 Fe1 C4 40.10(7) . . ?
C2 Fe1 C4 67.85(7) 2 2 ?
C2 Fe1 C4 118.67(7) . 2 ?
C1 Fe1 C4 68.38(7) 2 2 ?
C1 Fe1 C4 108.69(7) . 2 ?
C5 Fe1 C4 129.50(7) . 2 ?
C5 Fe1 C4 40.33(7) 2 2 ?
C3 Fe1 C4 40.10(7) 2 2 ?
C3 Fe1 C4 151.62(7) . 2 ?
C4 Fe1 C4 167.33(10) . 2 ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.364
_refine_diff_density_min   -0.299
_refine_diff_density_rms    0.058
