# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Long, Nicholas'
_publ_contact_author_email       n.long@imperial.ac.uk

_publ_section_title              
;
Coordination Chemistry with Phosphine and
Phosphine Oxide-Substituted Hydroxyferrocenes
;
_publ_author_name                'Nicholas Long'

data_6
_database_code_depnum_ccdc_archive 'CCDC 762216'
#TrackingRef 'Dalton 11-07.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H36 Fe2 O4 P2 Rh2'
_chemical_formula_sum            'C46 H36 Fe2 O4 P2 Rh2'
_chemical_formula_weight         1032.21

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'
O O 0.0492 0.0322 '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'
Rh Rh 0.0927 3.6045 '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

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4740(10)
_cell_length_b                   11.3952(16)
_cell_length_c                   12.7781(19)
_cell_angle_alpha                75.487(12)
_cell_angle_beta                 75.467(13)
_cell_angle_gamma                77.507(12)
_cell_volume                     1006.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      4.0588
_cell_measurement_theta_max      70.9715

_exptl_crystal_description       needles
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    13.293
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.23046
_exptl_absorpt_correction_T_max  0.74853
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.24pre2 beta (release 31.07.2004 CrysAlis171 .NET)
(compiled Jul 31 2004,21:19:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;

_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            8337
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.06
_diffrn_reflns_theta_max         71.18
_reflns_number_total             3680
_reflns_number_gt                3230
_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.
;

_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^)+(0.1069P)^2^+2.5856P] 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         3680
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1898
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_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
Rh Rh 0.41026(7) 0.54699(4) 0.88762(4) 0.0331(2) Uani 1 1 d . . .
Fe Fe 0.01095(15) 0.75273(9) 1.07056(9) 0.0312(3) Uani 1 1 d . . .
C C 0.4295(11) 0.4783(6) 0.7713(6) 0.0387(16) Uani 1 1 d . . .
O O 0.4438(9) 0.4269(5) 0.7013(5) 0.0562(15) Uani 1 1 d . . .
P P 0.2302(2) 0.71412(15) 0.81224(15) 0.0314(4) Uani 1 1 d . . .
C1 C 0.0243(9) 0.7656(6) 0.9081(5) 0.0274(13) Uani 1 1 d . . .
C2 C -0.0315(10) 0.8870(6) 0.9337(6) 0.0364(15) Uani 1 1 d . . .
H2A H 0.0335 0.9546 0.9011 0.044 Uiso 1 1 calc R . .
C3 C -0.1983(10) 0.8877(7) 1.0151(6) 0.0372(16) Uani 1 1 d . . .
H3A H -0.2643 0.9554 1.0475 0.045 Uiso 1 1 calc R . .
C4 C -0.2513(10) 0.7678(7) 1.0407(6) 0.0387(16) Uani 1 1 d . . .
H4A H -0.3584 0.7425 1.0928 0.046 Uiso 1 1 calc R . .
C5 C -0.1147(10) 0.6939(7) 0.9742(6) 0.0372(15) Uani 1 1 d . . .
H5A H -0.1158 0.6107 0.9738 0.045 Uiso 1 1 calc R . .
C6 C 0.2630(10) 0.6542(6) 1.1012(6) 0.0356(15) Uani 1 1 d . . .
O6 O 0.4116(6) 0.6049(4) 1.0307(4) 0.0301(10) Uani 1 1 d . . .
C7 C 0.1142(12) 0.5950(6) 1.1707(6) 0.0417(17) Uani 1 1 d . . .
H7A H 0.0979 0.5135 1.1744 0.050 Uiso 1 1 calc R . .
C8 C -0.0069(11) 0.6788(8) 1.2341(6) 0.0428(17) Uani 1 1 d . . .
H8A H -0.1191 0.6638 1.2865 0.051 Uiso 1 1 calc R . .
C9 C 0.0718(11) 0.7900(7) 1.2042(7) 0.0414(17) Uani 1 1 d . . .
H9A H 0.0215 0.8613 1.2344 0.050 Uiso 1 1 calc R . .
C10 C 0.2381(10) 0.7750(6) 1.1216(7) 0.0379(16) Uani 1 1 d . . .
H10A H 0.3179 0.8343 1.0866 0.045 Uiso 1 1 calc R . .
C11 C 0.1390(11) 0.7095(6) 0.6935(6) 0.0365(15) Uani 1 1 d . . .
C12 C 0.2667(12) 0.6881(7) 0.5948(6) 0.0454(18) Uani 1 1 d . . .
H12A H 0.3980 0.6806 0.5883 0.054 Uiso 1 1 calc R . .
C13 C 0.1928(15) 0.6786(9) 0.5069(7) 0.062(2) Uani 1 1 d . . .
H13A H 0.2761 0.6630 0.4404 0.074 Uiso 1 1 calc R . .
C14 C 0.0043(17) 0.6912(11) 0.5146(8) 0.070(3) Uani 1 1 d . . .
H14A H -0.0422 0.6855 0.4536 0.083 Uiso 1 1 calc R . .
C15 C -0.1176(15) 0.7119(11) 0.6101(7) 0.066(3) Uani 1 1 d . . .
H15A H -0.2485 0.7193 0.6156 0.080 Uiso 1 1 calc R . .
C16 C -0.0516(12) 0.7223(8) 0.6993(7) 0.050(2) Uani 1 1 d . . .
H16A H -0.1378 0.7383 0.7647 0.060 Uiso 1 1 calc R . .
C17 C 0.3485(10) 0.8488(6) 0.7633(6) 0.0372(15) Uani 1 1 d . . .
C18 C 0.3005(12) 0.9436(7) 0.6752(7) 0.0453(18) Uani 1 1 d . . .
H18A H 0.2082 0.9378 0.6381 0.054 Uiso 1 1 calc R . .
C19 C 0.3918(14) 1.0470(8) 0.6430(8) 0.058(2) Uani 1 1 d . . .
H19A H 0.3609 1.1111 0.5835 0.069 Uiso 1 1 calc R . .
C20 C 0.5246(13) 1.0567(8) 0.6962(8) 0.055(2) Uani 1 1 d . . .
H20A H 0.5864 1.1263 0.6731 0.066 Uiso 1 1 calc R . .
C21 C 0.5679(13) 0.9640(8) 0.7840(7) 0.0488(19) Uani 1 1 d . . .
H21A H 0.6569 0.9715 0.8226 0.059 Uiso 1 1 calc R . .
C22 C 0.4823(11) 0.8601(7) 0.8163(7) 0.0416(17) Uani 1 1 d . . .
H22A H 0.5160 0.7962 0.8752 0.050 Uiso 1 1 calc R . .

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
Rh 0.0353(3) 0.0248(3) 0.0366(3) -0.0073(2) -0.0089(2) 0.0033(2)
Fe 0.0310(6) 0.0275(6) 0.0341(6) -0.0089(4) -0.0073(4) 0.0009(4)
C 0.040(4) 0.028(3) 0.041(4) 0.000(3) -0.006(3) 0.000(3)
O 0.071(4) 0.046(3) 0.053(3) -0.024(3) -0.017(3) 0.010(3)
P 0.0302(9) 0.0240(8) 0.0366(9) -0.0063(7) -0.0084(7) 0.0044(6)
C1 0.022(3) 0.025(3) 0.035(3) -0.003(3) -0.012(3) 0.003(2)
C2 0.039(4) 0.028(3) 0.040(4) -0.003(3) -0.011(3) -0.001(3)
C3 0.031(4) 0.035(4) 0.042(4) -0.016(3) -0.017(3) 0.021(3)
C4 0.035(4) 0.039(4) 0.042(4) -0.011(3) -0.009(3) -0.004(3)
C5 0.038(4) 0.031(3) 0.040(4) -0.008(3) -0.009(3) 0.001(3)
C6 0.041(4) 0.029(3) 0.037(4) -0.005(3) -0.018(3) 0.002(3)
O6 0.024(2) 0.026(2) 0.039(3) -0.0080(19) -0.0139(19) 0.0089(17)
C7 0.063(5) 0.023(3) 0.039(4) 0.001(3) -0.020(4) -0.005(3)
C8 0.038(4) 0.053(5) 0.031(4) -0.005(3) -0.003(3) -0.004(3)
C9 0.041(4) 0.039(4) 0.044(4) -0.018(3) -0.010(3) 0.006(3)
C10 0.035(4) 0.024(3) 0.057(5) -0.010(3) -0.021(3) 0.005(3)
C11 0.044(4) 0.024(3) 0.036(4) -0.008(3) -0.007(3) 0.005(3)
C12 0.048(5) 0.046(4) 0.036(4) -0.004(3) -0.007(3) -0.001(3)
C13 0.078(7) 0.060(6) 0.038(4) -0.011(4) -0.011(4) 0.005(5)
C14 0.085(8) 0.093(8) 0.043(5) -0.026(5) -0.024(5) -0.017(6)
C15 0.056(6) 0.103(8) 0.040(5) -0.015(5) -0.021(4) -0.002(5)
C16 0.043(5) 0.059(5) 0.043(4) -0.016(4) -0.008(3) 0.005(4)
C17 0.030(4) 0.030(3) 0.046(4) -0.008(3) -0.004(3) 0.002(3)
C18 0.047(4) 0.035(4) 0.052(5) 0.000(3) -0.015(4) -0.009(3)
C19 0.071(6) 0.036(4) 0.058(5) 0.007(4) -0.020(5) -0.004(4)
C20 0.051(5) 0.035(4) 0.074(6) -0.003(4) -0.006(4) -0.014(4)
C21 0.050(5) 0.042(4) 0.053(5) -0.011(4) -0.004(4) -0.011(4)
C22 0.039(4) 0.036(4) 0.047(4) -0.010(3) -0.010(3) 0.001(3)

_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
Rh C 1.808(8) . ?
Rh O6 2.096(5) . ?
Rh O6 2.157(4) 2_667 ?
Rh P 2.2334(17) . ?
Fe C1 2.023(7) . ?
Fe C5 2.029(8) . ?
Fe C8 2.030(7) . ?
Fe C9 2.035(8) . ?
Fe C6 2.048(7) . ?
Fe C10 2.049(7) . ?
Fe C7 2.051(7) . ?
Fe C4 2.053(8) . ?
Fe C2 2.056(7) . ?
Fe C3 2.070(6) . ?
C O 1.159(10) . ?
P C1 1.799(7) . ?
P C11 1.829(8) . ?
P C17 1.832(7) . ?
C1 C5 1.429(10) . ?
C1 C2 1.450(9) . ?
C2 C3 1.409(10) . ?
C3 C4 1.441(11) . ?
C4 C5 1.423(10) . ?
C6 O6 1.357(9) . ?
C6 C7 1.418(11) . ?
C6 C10 1.429(10) . ?
O6 Rh 2.157(4) 2_667 ?
C7 C8 1.426(11) . ?
C8 C9 1.437(11) . ?
C9 C10 1.424(11) . ?
C11 C16 1.385(11) . ?
C11 C12 1.418(10) . ?
C12 C13 1.407(12) . ?
C13 C14 1.366(15) . ?
C14 C15 1.367(14) . ?
C15 C16 1.389(12) . ?
C17 C22 1.384(11) . ?
C17 C18 1.410(11) . ?
C18 C19 1.410(12) . ?
C19 C20 1.372(13) . ?
C20 C21 1.385(13) . ?
C21 C22 1.390(11) . ?

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
C Rh O6 172.2(2) . . ?
C Rh O6 94.5(3) . 2_667 ?
O6 Rh O6 77.75(19) . 2_667 ?
C Rh P 90.3(2) . . ?
O6 Rh P 97.52(13) . . ?
O6 Rh P 175.02(13) 2_667 . ?
C1 Fe C5 41.3(3) . . ?
C1 Fe C8 160.1(3) . . ?
C5 Fe C8 122.8(3) . . ?
C1 Fe C9 156.2(3) . . ?
C5 Fe C9 162.1(3) . . ?
C8 Fe C9 41.4(3) . . ?
C1 Fe C6 105.8(3) . . ?
C5 Fe C6 117.8(3) . . ?
C8 Fe C6 68.8(3) . . ?
C9 Fe C6 68.6(3) . . ?
C1 Fe C10 119.9(3) . . ?
C5 Fe C10 153.9(3) . . ?
C8 Fe C10 69.3(3) . . ?
C9 Fe C10 40.8(3) . . ?
C6 Fe C10 40.8(3) . . ?
C1 Fe C7 122.8(3) . . ?
C5 Fe C7 104.5(3) . . ?
C8 Fe C7 40.9(3) . . ?
C9 Fe C7 68.8(3) . . ?
C6 Fe C7 40.5(3) . . ?
C10 Fe C7 68.6(3) . . ?
C1 Fe C4 69.3(3) . . ?
C5 Fe C4 40.8(3) . . ?
C8 Fe C4 106.3(3) . . ?
C9 Fe C4 126.5(3) . . ?
C6 Fe C4 152.7(3) . . ?
C10 Fe C4 164.7(3) . . ?
C7 Fe C4 118.3(3) . . ?
C1 Fe C2 41.6(3) . . ?
C5 Fe C2 69.0(3) . . ?
C8 Fe C2 156.4(3) . . ?
C9 Fe C2 122.2(3) . . ?
C6 Fe C2 126.7(3) . . ?
C10 Fe C2 109.5(3) . . ?
C7 Fe C2 162.2(3) . . ?
C4 Fe C2 68.3(3) . . ?
C1 Fe C3 69.1(3) . . ?
C5 Fe C3 68.8(3) . . ?
C8 Fe C3 121.1(3) . . ?
C9 Fe C3 109.8(3) . . ?
C6 Fe C3 164.3(3) . . ?
C10 Fe C3 127.8(3) . . ?
C7 Fe C3 154.8(3) . . ?
C4 Fe C3 40.9(3) . . ?
C2 Fe C3 40.0(3) . . ?
O C Rh 175.5(6) . . ?
C1 P C11 103.6(3) . . ?
C1 P C17 102.8(3) . . ?
C11 P C17 103.4(3) . . ?
C1 P Rh 113.5(2) . . ?
C11 P Rh 119.0(2) . . ?
C17 P Rh 112.7(2) . . ?
C5 C1 C2 107.0(6) . . ?
C5 C1 P 126.3(5) . . ?
C2 C1 P 126.7(5) . . ?
C5 C1 Fe 69.6(4) . . ?
C2 C1 Fe 70.4(4) . . ?
P C1 Fe 124.7(3) . . ?
C3 C2 C1 108.5(6) . . ?
C3 C2 Fe 70.5(4) . . ?
C1 C2 Fe 67.9(4) . . ?
C2 C3 C4 108.1(6) . . ?
C2 C3 Fe 69.5(4) . . ?
C4 C3 Fe 68.9(4) . . ?
C5 C4 C3 107.9(7) . . ?
C5 C4 Fe 68.7(4) . . ?
C3 C4 Fe 70.2(4) . . ?
C4 C5 C1 108.6(6) . . ?
C4 C5 Fe 70.5(4) . . ?
C1 C5 Fe 69.1(4) . . ?
O6 C6 C7 126.9(6) . . ?
O6 C6 C10 124.4(7) . . ?
C7 C6 C10 108.6(7) . . ?
O6 C6 Fe 129.1(5) . . ?
C7 C6 Fe 69.9(4) . . ?
C10 C6 Fe 69.6(4) . . ?
C6 O6 Rh 127.9(4) . . ?
C6 O6 Rh 113.5(4) . 2_667 ?
Rh O6 Rh 102.25(19) . 2_667 ?
C6 C7 C8 108.2(6) . . ?
C6 C7 Fe 69.7(4) . . ?
C8 C7 Fe 68.8(4) . . ?
C7 C8 C9 107.4(7) . . ?
C7 C8 Fe 70.3(4) . . ?
C9 C8 Fe 69.5(4) . . ?
C10 C9 C8 108.3(6) . . ?
C10 C9 Fe 70.1(4) . . ?
C8 C9 Fe 69.1(4) . . ?
C9 C10 C6 107.5(7) . . ?
C9 C10 Fe 69.1(4) . . ?
C6 C10 Fe 69.6(4) . . ?
C16 C11 C12 119.5(7) . . ?
C16 C11 P 121.4(6) . . ?
C12 C11 P 119.1(6) . . ?
C13 C12 C11 117.8(8) . . ?
C14 C13 C12 121.7(9) . . ?
C13 C14 C15 120.0(9) . . ?
C14 C15 C16 120.6(9) . . ?
C11 C16 C15 120.5(8) . . ?
C22 C17 C18 119.3(7) . . ?
C22 C17 P 119.5(6) . . ?
C18 C17 P 121.1(6) . . ?
C17 C18 C19 118.8(8) . . ?
C20 C19 C18 121.1(8) . . ?
C19 C20 C21 119.5(8) . . ?
C20 C21 C22 120.6(9) . . ?
C17 C22 C21 120.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.167

#===END