Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222

_publ_section_title              
;In vitro DNA Scission Activity of Heterometallocenes
;
_publ_contact_author_name        'Prof. Nicholas Long'
_publ_contact_author_email       N.LONG@IMPERIAL.AC.UK
loop_
_publ_author_name
'Nicholas Long'
'Konrad Kowalski'
'David J. Mann'
'Natsuko Suwaki'
'Andrew J. P. White'
'Janusz Zakrzewski'

# Attachment 'B616191J_Dalton__cif_.cif'

data_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 617967'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 F6 Fe N P'
_chemical_formula_weight         375.08

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.7720(16)
_cell_length_b                   14.610(3)
_cell_length_c                   7.809(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.73(3)
_cell_angle_gamma                90.00
_cell_volume                     736.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5589
_cell_measurement_theta_min      3.0221
_cell_measurement_theta_max      70.7980

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             380
_exptl_absorpt_coefficient_mu    9.819
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
(compiled Mar 17 2006,10:57:34)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54248
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9537
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         5.95
_diffrn_reflns_theta_max         70.89
_reflns_number_total             1467
_reflns_number_gt                1316
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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.

Refinements in the non-centrosymmetric space group P2(1) gave the following
results

refine_ls_R_factor_obs+ 0.0275
refine_ls_wR_factor_obs+ 0.0671
refine_ls_abs_structure_Flack+ 0.498(13)
refine_ls_R_factor_obs- 0.0274
refine_ls_wR_factor_obs- 0.0674
refine_ls_abs_structure_Flack- 0.502(13)

Additionally, use of P2(1) did not remove the disorder in the PF6 anion.
Therefore, with no good reason to remove the centre of symmetry, the
centrosymmetric space group P2(1)/m was used.

;

_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^)+(0.0698P)^2^+0.2567P] 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         1467
_refine_ls_number_parameters     129
_refine_ls_number_restraints     409
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1059
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.857
_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
Fe Fe 0.09195(13) 0.2500 1.00043(11) 0.0277(3) Uani 1 2 d S . .
N1 N 0.3735(8) 0.2500 1.1756(7) 0.0310(11) Uani 1 2 d S . .
C2 C 0.3498(6) 0.3294(3) 1.0678(6) 0.0329(9) Uani 1 1 d . . .
C3 C 0.3125(7) 0.2986(3) 0.8897(6) 0.0361(10) Uani 1 1 d . . .
H3A H 0.2847 0.3385 0.7808 0.043 Uiso 1 1 calc R . .
C4 C 0.4392(11) 0.2500 1.3741(8) 0.0418(16) Uani 1 2 d S . .
H4A H 0.4173 0.1890 1.4174 0.063 Uiso 0.50 1 calc PR . .
H4B H 0.3574 0.2950 1.4164 0.063 Uiso 0.50 1 calc PR . .
H4C H 0.5865 0.2659 1.4202 0.063 Uiso 0.50 1 calc PR . .
C5 C 0.3823(8) 0.4236(4) 1.1441(7) 0.0437(12) Uani 1 1 d . . .
H5A H 0.5308 0.4344 1.1999 0.066 Uiso 1 1 calc R . .
H5B H 0.3101 0.4301 1.2348 0.066 Uiso 1 1 calc R . .
H5C H 0.3272 0.4683 1.0478 0.066 Uiso 1 1 calc R . .
C6 C -0.1270(10) 0.2500 1.1330(9) 0.0486(19) Uani 1 2 d S . .
H6A H -0.0992 0.2500 1.2664 0.058 Uiso 1 2 calc SR . .
C7 C -0.1509(7) 0.3274(4) 1.0228(8) 0.0482(13) Uani 1 1 d . . .
H7A H -0.1418 0.3924 1.0646 0.058 Uiso 1 1 calc R . .
C8 C -0.1875(7) 0.2989(4) 0.8442(7) 0.0421(11) Uani 1 1 d . . .
H8A H -0.2115 0.3395 0.7367 0.051 Uiso 1 1 calc R . .
P P 0.0160(15) 0.4953(7) 0.5017(8) 0.028(3) Uiso 0.356(6) 1 d PDU A -1
F1 F 0.051(3) 0.4848(13) 0.7135(17) 0.056(11) Uiso 0.356(6) 1 d PDU A -1
F2 F -0.2105(19) 0.5389(10) 0.4758(18) 0.060(5) Uiso 0.356(6) 1 d PDU A -1
F3 F 0.1414(18) 0.5892(7) 0.5368(11) 0.031(2) Uiso 0.356(6) 1 d PDU A -1
F4 F 0.2233(19) 0.4416(10) 0.5256(16) 0.042(3) Uiso 0.356(6) 1 d PDU A -1
F5 F -0.0858(19) 0.3964(7) 0.4674(13) 0.049(3) Uiso 0.356(6) 1 d PDU A -1
F6 F -0.013(2) 0.5066(7) 0.2907(11) 0.032(3) Uiso 0.356(6) 1 d PDU A -1
P' P 0.020(3) 0.5088(11) 0.4993(13) 0.026(8) Uiso 0.144(6) 1 d PDU A -2
F1' F 0.099(3) 0.5003(12) 0.7172(17) 0.020(5) Uiso 0.144(6) 1 d PDU A -2
F2' F -0.085(4) 0.6037(14) 0.522(3) 0.054(7) Uiso 0.144(6) 1 d PDU A -2
F3' F 0.223(3) 0.5682(17) 0.512(3) 0.064(8) Uiso 0.144(6) 1 d PDU A -2
F4' F 0.149(4) 0.4198(13) 0.492(2) 0.017(4) Uiso 0.144(6) 1 d PDU A -2
F5' F -0.185(3) 0.4546(18) 0.495(3) 0.066(8) Uiso 0.144(6) 1 d PDU A -2
F6' F -0.059(4) 0.5200(17) 0.288(2) 0.023(10) Uiso 0.144(6) 1 d PDU A -2

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
Fe 0.0221(5) 0.0337(6) 0.0269(5) 0.000 0.0071(3) 0.000
N1 0.025(2) 0.040(3) 0.028(2) 0.000 0.0078(19) 0.000
C2 0.024(2) 0.039(2) 0.036(2) 0.0041(18) 0.0095(16) -0.0019(18)
C3 0.025(2) 0.050(3) 0.034(2) 0.004(2) 0.0118(16) -0.002(2)
C4 0.041(4) 0.052(4) 0.028(3) 0.000 0.005(3) 0.000
C5 0.039(3) 0.040(3) 0.050(3) -0.001(2) 0.012(2) -0.008(2)
C6 0.026(3) 0.087(6) 0.036(3) 0.000 0.014(3) 0.000
C7 0.024(2) 0.049(3) 0.072(3) -0.019(3) 0.014(2) 0.002(2)
C8 0.023(2) 0.052(3) 0.047(3) 0.014(2) 0.0056(18) 0.004(2)

_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
Fe N1 1.979(5) . ?
Fe C2 2.028(4) . ?
Fe C2 2.028(4) 4_565 ?
Fe C8 2.043(5) 4_565 ?
Fe C8 2.043(5) . ?
Fe C7 2.047(5) 4_565 ?
Fe C7 2.047(5) . ?
Fe C6 2.051(7) . ?
Fe C3 2.066(4) . ?
Fe C3 2.066(4) 4_565 ?
N1 C2 1.413(5) 4_565 ?
N1 C2 1.413(5) . ?
N1 C4 1.477(8) . ?
C2 C3 1.410(6) . ?
C2 C5 1.489(7) . ?
C3 C3 1.419(10) 4_565 ?
C6 C7 1.401(7) 4_565 ?
C6 C7 1.401(7) . ?
C7 C8 1.403(7) . ?
C8 C8 1.430(11) 4_565 ?
P F4 1.569(12) . ?
P F5 1.588(13) . ?
P F3 1.592(12) . ?
P F1 1.606(13) . ?
P F6 1.607(9) . ?
P F2 1.615(13) . ?
P' F4' 1.577(17) . ?
P' F6' 1.581(16) . ?
P' F5' 1.592(19) . ?
P' F2' 1.595(18) . ?
P' F3' 1.602(19) . ?
P' F1' 1.626(14) . ?

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 Fe C2 41.28(14) . . ?
N1 Fe C2 41.28(14) . 4_565 ?
C2 Fe C2 69.8(3) . 4_565 ?
N1 Fe C8 159.19(16) . 4_565 ?
C2 Fe C8 157.4(2) . 4_565 ?
C2 Fe C8 121.5(2) 4_565 4_565 ?
N1 Fe C8 159.19(16) . . ?
C2 Fe C8 121.51(19) . . ?
C2 Fe C8 157.4(2) 4_565 . ?
C8 Fe C8 41.0(3) 4_565 . ?
N1 Fe C7 124.83(19) . 4_565 ?
C2 Fe C7 160.9(2) . 4_565 ?
C2 Fe C7 108.2(2) 4_565 4_565 ?
C8 Fe C7 40.1(2) 4_565 4_565 ?
C8 Fe C7 67.8(2) . 4_565 ?
N1 Fe C7 124.83(19) . . ?
C2 Fe C7 108.2(2) . . ?
C2 Fe C7 160.9(2) 4_565 . ?
C8 Fe C7 67.8(2) 4_565 . ?
C8 Fe C7 40.1(2) . . ?
C7 Fe C7 67.1(3) 4_565 . ?
N1 Fe C6 110.1(2) . . ?
C2 Fe C6 124.52(19) . . ?
C2 Fe C6 124.52(19) 4_565 . ?
C8 Fe C6 67.7(2) 4_565 . ?
C8 Fe C6 67.7(2) . . ?
C7 Fe C6 40.0(2) 4_565 . ?
C7 Fe C6 40.0(2) . . ?
N1 Fe C3 67.80(19) . . ?
C2 Fe C3 40.28(18) . . ?
C2 Fe C3 68.28(19) 4_565 . ?
C8 Fe C3 121.8(2) 4_565 . ?
C8 Fe C3 106.63(19) . . ?
C7 Fe C3 158.0(2) 4_565 . ?
C7 Fe C3 123.2(2) . . ?
C6 Fe C3 159.61(14) . . ?
N1 Fe C3 67.80(18) . 4_565 ?
C2 Fe C3 68.28(19) . 4_565 ?
C2 Fe C3 40.28(18) 4_565 4_565 ?
C8 Fe C3 106.63(19) 4_565 4_565 ?
C8 Fe C3 121.8(2) . 4_565 ?
C7 Fe C3 123.2(2) 4_565 4_565 ?
C7 Fe C3 158.0(2) . 4_565 ?
C6 Fe C3 159.61(14) . 4_565 ?
C3 Fe C3 40.2(3) . 4_565 ?
C2 N1 C2 110.3(5) 4_565 . ?
C2 N1 C4 124.6(2) 4_565 . ?
C2 N1 C4 124.6(2) . . ?
C2 N1 Fe 71.2(3) 4_565 . ?
C2 N1 Fe 71.2(3) . . ?
C4 N1 Fe 130.1(4) . . ?
C3 C2 N1 106.2(4) . . ?
C3 C2 C5 130.6(4) . . ?
N1 C2 C5 123.0(4) . . ?
C3 C2 Fe 71.3(3) . . ?
N1 C2 Fe 67.5(3) . . ?
C5 C2 Fe 130.0(3) . . ?
C2 C3 C3 108.6(3) . 4_565 ?
C2 C3 Fe 68.4(2) . . ?
C3 C3 Fe 69.92(14) 4_565 . ?
C7 C6 C7 107.7(6) 4_565 . ?
C7 C6 Fe 69.9(3) 4_565 . ?
C7 C6 Fe 69.9(3) . . ?
C6 C7 C8 108.9(5) . . ?
C6 C7 Fe 70.2(3) . . ?
C8 C7 Fe 69.8(3) . . ?
C7 C8 C8 107.2(3) . 4_565 ?
C7 C8 Fe 70.1(3) . . ?
C8 C8 Fe 69.52(15) 4_565 . ?
F4 P F5 83.8(7) . . ?
F4 P F3 90.0(8) . . ?
F5 P F3 173.7(8) . . ?
F4 P F1 89.1(8) . . ?
F5 P F1 90.4(9) . . ?
F3 P F1 90.1(8) . . ?
F4 P F6 89.9(7) . . ?
F5 P F6 90.5(6) . . ?
F3 P F6 88.9(7) . . ?
F1 P F6 178.6(12) . . ?
F4 P F2 173.2(12) . . ?
F5 P F2 89.5(8) . . ?
F3 P F2 96.8(8) . . ?
F1 P F2 90.1(9) . . ?
F6 P F2 90.9(7) . . ?
F4' P' F6' 93.7(11) . . ?
F4' P' F5' 94.5(12) . . ?
F6' P' F5' 90.9(12) . . ?
F4' P' F2' 173.2(13) . . ?
F6' P' F2' 90.3(11) . . ?
F5' P' F2' 90.9(12) . . ?
F4' P' F3' 88.6(12) . . ?
F6' P' F3' 91.1(12) . . ?
F5' P' F3' 176.2(15) . . ?
F2' P' F3' 85.8(11) . . ?
F4' P' F1' 87.9(10) . . ?
F6' P' F1' 178.3(14) . . ?
F5' P' F1' 89.4(11) . . ?
F2' P' F1' 88.1(10) . . ?
F3' P' F1' 88.6(11) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        70.89
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.070

#===END