 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C60 H50 P4 Ru'
_chemical_formula_sum
 'C60 H50 P4 Ru'
_chemical_formula_weight          995.95
 
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'
 'Ru'  'Ru'  -1.2594   0.8363
 '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                    9.2135(2)
_cell_length_b                    11.5649(3)
_cell_length_c                    13.2669(4)
_cell_angle_alpha                 110.990(1)
_cell_angle_beta                  96.126(1)
_cell_angle_gamma                 111.168(1)
_cell_volume                      1184.67(6)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     10657
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.396
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              514
_exptl_absorpt_coefficient_mu     0.507
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9279
_exptl_absorpt_correction_T_max   0.9702
_exptl_absorpt_process_details    'SORTAV (R.H.Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             13634
_diffrn_reflns_av_R_equivalents   0.0600
_diffrn_reflns_av_sigmaI/netI     0.0626
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.11
_diffrn_reflns_theta_max          25.02
_reflns_number_total              4073
_reflns_number_gt                 3420
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'PLATON (Watkin, Pearce 1995)'
_computing_publication_material   SHELXL-97
 
_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 > 2σ(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)+(0.0266P)²+1.7462P] 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      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4073
_refine_ls_number_parameters      299
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0537
_refine_ls_R_factor_gt            0.0407
_refine_ls_wR_factor_ref          0.0927
_refine_ls_wR_factor_gt           0.0852
_refine_ls_goodness_of_fit_ref    1.035
_refine_ls_restrained_S_all       1.035
_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
Ru1 Ru 0.5000 0.0000 0.0000 0.01269(12) Uani 1 2 d S . .
P1 P 0.26601(10) -0.17013(8) -0.14782(7) 0.0167(2) Uani 1 1 d . . .
P2 P 0.32309(9) -0.04186(8) 0.11190(6) 0.01364(19) Uani 1 1 d . . .
C1 C 0.2115(4) -0.1229(4) -0.2590(3) 0.0232(8) Uani 1 1 d . . .
C2 C 0.1187(4) -0.0496(5) -0.2503(3) 0.0378(10) Uani 1 1 d . . .
H2 H 0.0734 -0.0306 -0.1886 0.045 Uiso 1 1 calc R . .
C3 C 0.0916(5) -0.0039(5) -0.3312(4) 0.0475(12) Uani 1 1 d . . .
H3 H 0.0295 0.0473 -0.3237 0.057 Uiso 1 1 calc R . .
C4 C 0.1544(5) -0.0325(5) -0.4218(4) 0.0433(12) Uani 1 1 d . . .
H4 H 0.1348 -0.0018 -0.4772 0.052 Uiso 1 1 calc R . .
C5 C 0.2454(4) -0.1054(4) -0.4325(3) 0.0336(10) Uani 1 1 d . . .
H5 H 0.2889 -0.1248 -0.4951 0.040 Uiso 1 1 calc R . .
C6 C 0.2741(4) -0.1508(4) -0.3518(3) 0.0265(8) Uani 1 1 d . . .
H6 H 0.3370 -0.2015 -0.3599 0.032 Uiso 1 1 calc R . .
C7 C 0.2296(4) -0.3484(4) -0.2304(3) 0.0281(9) Uani 1 1 d . . .
C8 C 0.1114(7) -0.4295(5) -0.3327(4) 0.084(2) Uani 1 1 d . . .
H8 H 0.0532 -0.3906 -0.3625 0.101 Uiso 1 1 calc R . .
C9 C 0.0780(11) -0.5664(5) -0.3913(4) 0.125(4) Uani 1 1 d . . .
H9 H -0.0026 -0.6205 -0.4611 0.150 Uiso 1 1 calc R . .
C10 C 0.1595(9) -0.6238(5) -0.3497(5) 0.093(3) Uani 1 1 d . . .
H10 H 0.1372 -0.7172 -0.3911 0.112 Uiso 1 1 calc R . .
C11 C 0.2728(6) -0.5480(5) -0.2491(6) 0.075(2) Uani 1 1 d . . .
H11 H 0.3284 -0.5888 -0.2196 0.090 Uiso 1 1 calc R . .
C12 C 0.3072(5) -0.4111(4) -0.1896(4) 0.0459(12) Uani 1 1 d . . .
H12 H 0.3861 -0.3591 -0.1191 0.055 Uiso 1 1 calc R . .
C13 C 0.0883(4) -0.2029(4) -0.0891(3) 0.0231(8) Uani 1 1 d . . .
H13A H -0.0041 -0.2108 -0.1410 0.028 Uiso 1 1 calc R . .
H13B H 0.0572 -0.2912 -0.0834 0.028 Uiso 1 1 calc R . .
C14 C 0.1232(4) -0.0891(3) 0.0262(3) 0.0191(7) Uani 1 1 d . . .
H14A H 0.0396 -0.1210 0.0634 0.023 Uiso 1 1 calc R . .
H14B H 0.1203 -0.0081 0.0182 0.023 Uiso 1 1 calc R . .
C15 C 0.2937(4) -0.1816(3) 0.1538(3) 0.0172(7) Uani 1 1 d . . .
C16 C 0.1399(4) -0.2750(4) 0.1455(3) 0.0243(8) Uani 1 1 d . . .
H16 H 0.0463 -0.2727 0.1104 0.029 Uiso 1 1 calc R . .
C17 C 0.1237(5) -0.3704(4) 0.1882(4) 0.0391(10) Uani 1 1 d . . .
H17 H 0.0190 -0.4331 0.1827 0.047 Uiso 1 1 calc R . .
C18 C 0.2593(5) -0.3748(5) 0.2388(4) 0.0478(12) Uani 1 1 d . . .
H18 H 0.2479 -0.4405 0.2681 0.057 Uiso 1 1 calc R . .
C19 C 0.4115(5) -0.2837(4) 0.2470(3) 0.0343(9) Uani 1 1 d . . .
H19 H 0.5046 -0.2865 0.2825 0.041 Uiso 1 1 calc R . .
C20 C 0.4291(4) -0.1891(4) 0.2040(3) 0.0219(8) Uani 1 1 d . . .
H20 H 0.5342 -0.1283 0.2085 0.026 Uiso 1 1 calc R . .
C21 C 0.3365(4) 0.0950(3) 0.2424(3) 0.0205(7) Uani 1 1 d . . .
C22 C 0.3411(5) 0.0828(4) 0.3430(3) 0.0387(10) Uani 1 1 d . . .
H22 H 0.3339 0.0000 0.3457 0.046 Uiso 1 1 calc R . .
C23 C 0.3562(6) 0.1919(5) 0.4400(4) 0.0643(17) Uani 1 1 d . . .
H23 H 0.3617 0.1836 0.5088 0.077 Uiso 1 1 calc R . .
C24 C 0.3632(6) 0.3115(5) 0.4375(4) 0.0658(17) Uani 1 1 d . . .
H24 H 0.3721 0.3847 0.5040 0.079 Uiso 1 1 calc R . .
C25 C 0.3575(5) 0.3249(4) 0.3387(4) 0.0466(12) Uani 1 1 d . . .
H25 H 0.3624 0.4075 0.3366 0.056 Uiso 1 1 calc R . .
C26 C 0.3445(4) 0.2175(3) 0.2419(3) 0.0292(9) Uani 1 1 d . . .
H26 H 0.3409 0.2276 0.1738 0.035 Uiso 1 1 calc R . .
C27 C 0.4078(4) 0.1316(3) -0.0150(3) 0.0193(7) Uani 1 1 d . . .
C28 C 0.3534(4) 0.2095(4) -0.0212(3) 0.0230(8) Uani 1 1 d . . .
C29 C 0.3074(4) 0.3131(4) -0.0161(4) 0.0365(10) Uani 1 1 d . . .
C30 C 0.2735(6) 0.4060(5) -0.0078(5) 0.0638(17) Uani 1 1 d . . .
H30 H 0.247(7) 0.474(6) -0.001(5) 0.10(2) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Ru1 C27 2.047(4) 2_655 ?
Ru1 C27 2.047(4) . ?
Ru1 P2 2.3573(11) 2_655 ?
Ru1 P2 2.3573(11) . ?
Ru1 P1 2.3739(11) 2_655 ?
Ru1 P1 2.3739(11) . ?
P1 C1 1.828(3) . ?
P1 C7 1.835(4) . ?
P1 C13 1.862(3) . ?
P2 C15 1.831(3) . ?
P2 C14 1.834(3) . ?
P2 C21 1.835(3) . ?
C1 C2 1.393(5) . ?
C1 C6 1.398(5) . ?
C2 C3 1.392(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.379(6) . ?
C7 C8 1.394(6) . ?
C8 C9 1.386(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.357(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.358(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.524(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.396(5) . ?
C15 C16 1.402(5) . ?
C16 C17 1.381(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.374(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.389(5) . ?
C21 C26 1.395(5) . ?
C22 C23 1.392(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.373(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.200(5) . ?
C28 C29 1.390(5) . ?
C29 C30 1.196(6) . ?
C30 H30 0.88(6) . ?
 
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
C27 Ru1 C27 180.0(3) 2_655 . ?
C27 Ru1 P2 85.79(9) 2_655 2_655 ?
C27 Ru1 P2 94.21(9) . 2_655 ?
C27 Ru1 P2 94.21(9) 2_655 . ?
C27 Ru1 P2 85.79(9) . . ?
P2 Ru1 P2 180.00(6) 2_655 . ?
C27 Ru1 P1 83.93(10) 2_655 2_655 ?
C27 Ru1 P1 96.07(10) . 2_655 ?
P2 Ru1 P1 82.54(4) 2_655 2_655 ?
P2 Ru1 P1 97.46(4) . 2_655 ?
C27 Ru1 P1 96.07(10) 2_655 . ?
C27 Ru1 P1 83.93(10) . . ?
P2 Ru1 P1 97.46(4) 2_655 . ?
P2 Ru1 P1 82.54(4) . . ?
P1 Ru1 P1 180.00(4) 2_655 . ?
C1 P1 C7 100.92(16) . . ?
C1 P1 C13 104.42(16) . . ?
C7 P1 C13 98.83(16) . . ?
C1 P1 Ru1 115.50(11) . . ?
C7 P1 Ru1 125.70(13) . . ?
C13 P1 Ru1 108.60(11) . . ?
C15 P2 C14 104.67(15) . . ?
C15 P2 C21 101.52(15) . . ?
C14 P2 C21 101.05(15) . . ?
C15 P2 Ru1 119.80(10) . . ?
C14 P2 Ru1 105.06(11) . . ?
C21 P2 Ru1 122.07(11) . . ?
C2 C1 C6 118.2(3) . . ?
C2 C1 P1 121.8(3) . . ?
C6 C1 P1 119.9(3) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C12 C7 C8 117.2(4) . . ?
C12 C7 P1 121.6(3) . . ?
C8 C7 P1 120.9(4) . . ?
C9 C8 C7 120.6(6) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.5(6) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.2(5) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 121.6(5) . . ?
C7 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C14 C13 P1 112.1(2) . . ?
C14 C13 H13A 109.2 . . ?
P1 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
P1 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 P2 109.6(2) . . ?
C13 C14 H14A 109.7 . . ?
P2 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
P2 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C20 C15 C16 118.5(3) . . ?
C20 C15 P2 119.0(2) . . ?
C16 C15 P2 122.2(2) . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C22 C21 C26 118.1(3) . . ?
C22 C21 P2 122.8(3) . . ?
C26 C21 P2 119.1(3) . . ?
C21 C22 C23 120.0(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.7(4) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 121.4(4) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C28 C27 Ru1 178.4(3) . . ?
C27 C28 C29 172.4(4) . . ?
C30 C29 C28 177.2(5) . . ?
C29 C30 H30 179(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.974
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.974
_refine_diff_density_max    0.670
_refine_diff_density_min   -0.719
_refine_diff_density_rms    0.088
