# Copyright The Royal Society of Chemistry, 1998 


# Use of silver oxide in the synthesis of arene ruthenium metallacyclic 
# complexes David L. Davies et al.

data_ks9653_(2b) 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C42 H41 Cl9 N O3 P Ru' 
_chemical_formula_weight          1058.85 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'Ru'  'Ru'  -1.2594   0.8363 
 '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)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    22.593(4) 
_cell_length_b                    11.252(2) 
_cell_length_c                    18.784(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.11(1)
_cell_angle_gamma                 90.00 
_cell_volume                      4587.7(15) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     190(2) 
_cell_measurement_reflns_used     39
_cell_measurement_theta_min       5.2
_cell_measurement_theta_max       12.4
 
_exptl_crystal_description        plate
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.48
_exptl_crystal_size_mid           0.44
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.533 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2144 
_exptl_absorpt_coefficient_mu     0.940 
_exptl_absorpt_correction_type    'semi-empirical based on psi scans data'
_exptl_absorpt_correction_T_min   0.74
_exptl_absorpt_correction_T_max   0.97
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       190(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4 diffractometer'
_diffrn_measurement_method        'omega scans'
_diffrn_standards_number          3
_diffrn_standards_interval_count  100
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <2
_diffrn_reflns_number             8326 
_diffrn_reflns_av_R_equivalents   0.0401 
_diffrn_reflns_av_sigmaI/netI     0.0961 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        26 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        1 
_diffrn_reflns_limit_l_min        -1 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          2.50 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              7022 
_reflns_number_observed           4447 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'XSCANS (Fait, 1991)' 
_computing_cell_refinement        'XSCANS (Fait, 1991)' 
_computing_data_reduction         'XSCANS (Fait, 1991)' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXTL/PC ver5.0(Sheldrick, 1996)'
_computing_molecular_graphics     'SHELXTL/PC ver5.0(Sheldrick, 1996)'
_computing_publication_material   'SHELXTL/PC ver5.0(Sheldrick, 1996)' 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+12.1823P] 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          7022 
_refine_ls_number_parameters      568 
_refine_ls_number_restraints      15 
_refine_ls_R_factor_all           0.1145 
_refine_ls_R_factor_obs           0.0609 
_refine_ls_wR_factor_all          0.1381 
_refine_ls_wR_factor_obs          0.1142 
_refine_ls_goodness_of_fit_all    1.022 
_refine_ls_goodness_of_fit_obs    1.086 
_refine_ls_restrained_S_all       1.030 
_refine_ls_restrained_S_obs       1.099 
_refine_ls_shift/esd_max          -0.113 
_refine_ls_shift/esd_mean         0.003 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ru1 Ru 0.23337(2) 0.17957(4) 0.15232(3) 0.02278(15) Uani 1 d . . 
P1 P 0.34147(7) 0.19065(15) 0.19784(9) 0.0244(4) Uani 1 d . . 
N1 N 0.2274(2) 0.1642(4) 0.2607(3) 0.0260(13) Uani 1 d . . 
O2 O 0.2176(3) 0.4781(4) 0.2679(3) 0.059(2) Uani 1 d . . 
O1 O 0.2401(2) 0.3547(3) 0.1880(3) 0.0302(11) Uani 1 d . . 
O3 O 0.2724(2) -0.0161(4) 0.2846(3) 0.0358(12) Uani 1 d . . 
C1 C 0.2209(3) 0.3767(6) 0.2454(5) 0.038(2) Uani 1 d . . 
C2 C 0.2022(3) 0.2683(6) 0.2816(4) 0.032(2) Uani 1 d . . 
C3 C 0.1587(3) 0.2847(6) 0.3172(4) 0.036(2) Uani 1 d . . 
H3 H 0.1525(3) 0.3672(6) 0.3261(4) 0.043 Uiso 1 d R . 
C5 C 0.2635(4) 0.0900(7) 0.3901(4) 0.045(2) Uani 1 d . . 
H5A H 0.2820(4) 0.0189(7) 0.4147(4) 0.080 Uiso 1 d R . 
H5B H 0.2906(4) 0.1562(7) 0.4073(4) 0.080 Uiso 1 d R . 
H5C H 0.2249(4) 0.1039(7) 0.4007(4) 0.080 Uiso 1 d R . 
C4 C 0.2529(3) 0.0760(6) 0.3075(4) 0.031(2) Uani 1 d . . 
C6 C 0.1179(3) 0.2084(6) 0.3449(4) 0.032(2) Uani 1 d . . 
C7 C 0.1138(4) 0.0845(7) 0.3359(4) 0.044(2) Uani 1 d . . 
H7 H 0.1414(4) 0.0435(7) 0.3137(4) 0.053 Uiso 1 d R . 
C8 C 0.0707(4) 0.0199(7) 0.3588(5) 0.055(2) Uani 1 d . . 
H8 H 0.0685(4) -0.0649(7) 0.3528(5) 0.066 Uiso 1 d R . 
C9 C 0.0301(4) 0.0756(8) 0.3918(5) 0.058(2) Uani 1 d . . 
H9 H 0.0001(4) 0.0307(8) 0.4080(5) 0.069 Uiso 1 d R . 
C10 C 0.0333(4) 0.1980(8) 0.4008(4) 0.054(2) Uani 1 d . . 
H10 H 0.0055(4) 0.2380(8) 0.4233(4) 0.065 Uiso 1 d R . 
C11 C 0.0762(4) 0.2620(7) 0.3770(4) 0.044(2) Uani 1 d . . 
H11 H 0.0784(4) 0.3466(7) 0.3836(4) 0.052 Uiso 1 d R . 
C12 C 0.2831(3) 0.0882(7) 0.0016(4) 0.044(2) Uani 1 d . . 
H12A H 0.2663(3) 0.0505(7) -0.0456(4) 0.053 Uiso 1 d R . 
H12B H 0.2990(3) 0.1650(7) -0.0058(4) 0.053 Uiso 1 d R . 
H12C H 0.3157(3) 0.0402(7) 0.0314(4) 0.053 Uiso 1 d R . 
C13 C 0.2348(3) 0.1036(6) 0.0406(4) 0.031(2) Uani 1 d . . 
C14 C 0.2226(3) 0.0131(6) 0.0879(4) 0.035(2) Uani 1 d . . 
H14 H 0.2520(3) -0.0496(6) 0.1043(4) 0.042 Uiso 1 d R . 
C15 C 0.1734(3) 0.0272(6) 0.1201(4) 0.035(2) Uani 1 d . . 
H15 H 0.1700(3) -0.0281(6) 0.1577(4) 0.043 Uiso 1 d R . 
C16 C 0.1342(3) 0.1288(6) 0.1061(4) 0.034(2) Uani 1 d . . 
C17 C 0.1484(3) 0.2171(6) 0.0616(4) 0.034(2) Uani 1 d . . 
H17 H 0.1291(3) 0.2934(6) 0.0606(4) 0.041 Uiso 1 d R . 
C18 C 0.1986(3) 0.2066(6) 0.0301(4) 0.036(2) Uani 1 d . . 
H18 H 0.2122(3) 0.2746(6) 0.0080(4) 0.043 Uiso 1 d R . 
C19 C 0.0804(4) 0.1376(7) 0.1390(5) 0.049(2) Uani 1 d . . 
H19 H 0.0959(4) 0.1191(7) 0.1907(5) 0.058 Uiso 1 d R . 
C20 C 0.0513(4) 0.2591(9) 0.1336(6) 0.075(3) Uani 1 d . . 
H20A H 0.0820(4) 0.3157(9) 0.1579(6) 0.089 Uiso 1 d R . 
H20B H 0.0362(4) 0.2790(9) 0.0820(6) 0.089 Uiso 1 d R . 
H20C H 0.0179(4) 0.2605(9) 0.1559(6) 0.089 Uiso 1 d R . 
C21 C 0.0335(5) 0.0420(10) 0.1063(7) 0.103(4) Uani 1 d . . 
H21A H -0.0012(5) 0.0433(10) 0.1265(7) 0.124 Uiso 1 d R . 
H21B H 0.0197(5) 0.0569(10) 0.0539(7) 0.124 Uiso 1 d R . 
H21C H 0.0531(5) -0.0344(10) 0.1150(7) 0.124 Uiso 1 d R . 
C22 C 0.3734(3) 0.2094(6) 0.2984(4) 0.030(2) Uani 1 d . . 
C23 C 0.4042(3) 0.1189(6) 0.3441(4) 0.034(2) Uani 1 d . . 
H23A H 0.4087(3) 0.0421(6) 0.3240(4) 0.080 Uiso 1 d R . 
C24 C 0.4286(4) 0.1405(8) 0.4193(5) 0.050(2) Uani 1 d . . 
H24A H 0.4499(4) 0.0783(8) 0.4513(5) 0.080 Uiso 1 d R . 
C25 C 0.4230(4) 0.2493(9) 0.4495(5) 0.055(2) Uani 1 d . . 
H25A H 0.4402(4) 0.2636(9) 0.5016(5) 0.080 Uiso 1 d R . 
C26 C 0.3926(3) 0.3393(7) 0.4044(5) 0.045(2) Uani 1 d . . 
H26A H 0.3882(3) 0.4156(7) 0.4251(5) 0.080 Uiso 1 d R . 
C27 C 0.3677(3) 0.3209(6) 0.3302(4) 0.038(2) Uani 1 d . . 
H27A H 0.3464(3) 0.3841(6) 0.2991(4) 0.080 Uiso 1 d R . 
C28 C 0.3849(3) 0.0670(6) 0.1738(4) 0.028(2) Uani 1 d . . 
C29 C 0.3694(3) -0.0484(6) 0.1872(4) 0.033(2) Uani 1 d . . 
H29A H 0.3374(3) -0.0627(6) 0.2108(4) 0.080 Uiso 1 d R . 
C30 C 0.4000(3) -0.1443(6) 0.1658(4) 0.038(2) Uani 1 d . . 
H30A H 0.3897(3) -0.2244(6) 0.1754(4) 0.080 Uiso 1 d R . 
C31 C 0.4460(4) -0.1236(7) 0.1311(4) 0.043(2) Uani 1 d . . 
H31A H 0.4668(4) -0.1894(7) 0.1162(4) 0.080 Uiso 1 d R . 
C32 C 0.4617(3) -0.0093(7) 0.1180(4) 0.042(2) Uani 1 d . . 
H32A H 0.4934(3) 0.0041(7) 0.0938(4) 0.080 Uiso 1 d R . 
C33 C 0.4316(3) 0.0861(6) 0.1400(4) 0.033(2) Uani 1 d . . 
H33A H 0.4432(3) 0.1655(6) 0.1310(4) 0.080 Uiso 1 d R . 
C34 C 0.3737(3) 0.3223(6) 0.1643(4) 0.0274(14) Uani 1 d . . 
C35 C 0.4327(3) 0.3610(6) 0.2010(4) 0.041(2) Uani 1 d . . 
H35A H 0.4564(3) 0.3190(6) 0.2440(4) 0.080 Uiso 1 d R . 
C36 C 0.4571(4) 0.4598(7) 0.1759(5) 0.053(2) Uani 1 d . . 
H36A H 0.4977(4) 0.4866(7) 0.2019(5) 0.080 Uiso 1 d R . 
C37 C 0.4236(4) 0.5195(7) 0.1136(5) 0.044(2) Uani 1 d . . 
H37A H 0.4411(4) 0.5871(7) 0.0957(5) 0.080 Uiso 1 d R . 
C38 C 0.3655(4) 0.4818(6) 0.0774(4) 0.039(2) Uani 1 d . . 
H38A H 0.3420(4) 0.5240(6) 0.0344(4) 0.080 Uiso 1 d R . 
C39 C 0.3398(3) 0.3844(6) 0.1025(4) 0.033(2) Uani 1 d . . 
H39A H 0.2990(3) 0.3585(6) 0.0768(4) 0.080 Uiso 1 d R . 
C1S C 0.1503(2) 0.6588(5) 0.3312(3) 0.054(2) Uani 1 d D . 
H1A H 0.1732(2) 0.5943(5) 0.3183(3) 0.080 Uiso 1 d R . 
Cl1 Cl 0.14853(15) 0.6374(3) 0.4231(2) 0.0924(9) Uani 1 d D . 
Cl2 Cl 0.18321(14) 0.7964(2) 0.3199(2) 0.0888(9) Uani 1 d D . 
Cl3 Cl 0.07542(12) 0.6467(4) 0.2724(2) 0.1106(12) Uani 1 d D . 
C2S C 0.3527(2) 0.7729(5) 0.3717(3) 0.064(3) Uani 1 d D . 
H2A H 0.3268(2) 0.8394(5) 0.3515(3) 0.080 Uiso 1 d R . 
Cl4 Cl 0.4312(2) 0.8003(9) 0.3819(7) 0.112(3) Uani 0.66 d PD . 
Cl5 Cl 0.3411(7) 0.7433(8) 0.4586(3) 0.099(3) Uani 0.66 d PD . 
Cl6 Cl 0.3290(3) 0.6506(6) 0.3139(5) 0.102(2) Uani 0.66 d PD . 
Cl4' Cl 0.4313(4) 0.8094(19) 0.4086(16) 0.170(13) Uani 0.34 d PD . 
Cl5' Cl 0.3374(16) 0.7035(20) 0.4488(11) 0.156(11) Uani 0.34 d PD . 
Cl6' Cl 0.3688(10) 0.6557(13) 0.3171(9) 0.212(12) Uani 0.34 d PD . 
C3S C 0.1973(2) 0.6061(5) 0.1096(3) 0.055(2) Uani 1 d D . 
H3A H 0.2082(2) 0.5495(5) 0.1494(3) 0.080 Uiso 1 d R . 
Cl7 Cl 0.2601(2) 0.6962(3) 0.1081(3) 0.0886(14) Uani 0.75 d PD . 
Cl8 Cl 0.1730(3) 0.5333(3) 0.0230(2) 0.093(2) Uani 0.75 d PD . 
Cl9 Cl 0.1362(2) 0.7021(4) 0.1138(3) 0.1037(15) Uani 0.75 d PD . 
Cl7' Cl 0.2053(12) 0.5903(24) 0.0199(6) 0.261(20) Uani 0.25 d PD . 
Cl8' Cl 0.1214(4) 0.5978(15) 0.1153(10) 0.134(6) Uani 0.25 d PD . 
Cl9' Cl 0.2339(10) 0.7265(9) 0.1649(9) 0.181(10) Uani 0.25 d PD . 
 
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 
Ru1 0.0205(3) 0.0229(2) 0.0254(3) 0.0016(3) 0.0071(2) 0.0006(3) 
P1 0.0214(9) 0.0261(8) 0.0264(9) 0.0005(8) 0.0079(7) 0.0027(7) 
N1 0.026(3) 0.026(3) 0.028(3) 0.001(2) 0.011(3) -0.002(2) 
O2 0.078(5) 0.027(3) 0.094(5) -0.020(3) 0.061(4) -0.011(3) 
O1 0.034(3) 0.020(2) 0.042(3) 0.003(2) 0.020(2) 0.002(2) 
O3 0.036(3) 0.032(3) 0.043(3) 0.011(2) 0.016(3) 0.007(2) 
C1 0.026(4) 0.031(4) 0.061(6) -0.001(4) 0.019(4) -0.005(3) 
C2 0.032(4) 0.029(3) 0.037(4) -0.006(3) 0.015(4) -0.001(3) 
C3 0.037(4) 0.035(4) 0.042(5) -0.008(3) 0.020(4) 0.003(3) 
C5 0.042(5) 0.067(5) 0.032(5) 0.012(4) 0.020(4) 0.010(4) 
C4 0.024(4) 0.037(4) 0.036(4) 0.004(3) 0.015(3) -0.004(3) 
C6 0.020(4) 0.043(4) 0.034(4) -0.003(3) 0.009(3) 0.001(3) 
C7 0.033(5) 0.050(5) 0.050(5) -0.002(4) 0.013(4) -0.003(4) 
C8 0.045(5) 0.053(5) 0.073(7) 0.018(5) 0.024(5) 0.007(4) 
C9 0.043(6) 0.072(6) 0.065(6) 0.013(5) 0.028(5) -0.007(4) 
C10 0.036(5) 0.089(7) 0.045(5) 0.008(5) 0.023(4) 0.008(5) 
C11 0.040(5) 0.059(5) 0.038(5) -0.008(4) 0.021(4) -0.001(4) 
C12 0.038(5) 0.062(5) 0.035(5) -0.009(4) 0.015(4) 0.000(4) 
C13 0.026(4) 0.045(4) 0.021(4) -0.007(3) 0.003(3) -0.002(3) 
C14 0.038(4) 0.030(4) 0.034(4) -0.002(3) 0.006(4) 0.001(3) 
C15 0.039(5) 0.034(4) 0.032(4) -0.006(3) 0.006(4) -0.017(3) 
C16 0.026(4) 0.045(4) 0.029(4) -0.009(3) 0.006(3) -0.005(3) 
C17 0.023(4) 0.044(4) 0.033(4) 0.003(3) 0.004(3) 0.001(3) 
C18 0.033(4) 0.044(4) 0.026(4) 0.006(3) 0.003(3) -0.001(3) 
C19 0.032(5) 0.072(6) 0.048(5) -0.017(4) 0.020(4) -0.018(4) 
C20 0.043(6) 0.111(8) 0.077(8) -0.009(6) 0.030(6) 0.020(5) 
C21 0.056(7) 0.140(10) 0.131(11) -0.063(9) 0.053(8) -0.054(7) 
C22 0.016(3) 0.042(4) 0.032(4) -0.002(3) 0.009(3) -0.004(3) 
C23 0.018(4) 0.051(4) 0.033(4) 0.005(4) 0.011(3) 0.010(3) 
C24 0.028(4) 0.084(6) 0.039(5) 0.004(4) 0.011(4) 0.009(4) 
C25 0.038(5) 0.095(7) 0.035(5) -0.015(5) 0.014(4) -0.008(5) 
C26 0.024(4) 0.066(6) 0.048(5) -0.017(4) 0.014(4) -0.012(4) 
C27 0.035(4) 0.039(4) 0.043(5) -0.009(4) 0.016(4) -0.011(4) 
C28 0.021(4) 0.034(4) 0.026(4) 0.001(3) 0.004(3) 0.005(3) 
C29 0.033(4) 0.035(4) 0.035(4) -0.004(3) 0.014(4) 0.000(3) 
C30 0.033(4) 0.037(4) 0.040(5) -0.008(3) 0.003(4) 0.004(3) 
C31 0.037(5) 0.050(5) 0.042(5) -0.011(4) 0.009(4) 0.015(4) 
C32 0.037(5) 0.053(5) 0.041(5) 0.001(4) 0.018(4) 0.009(4) 
C33 0.029(4) 0.041(4) 0.033(4) 0.002(3) 0.012(3) 0.007(3) 
C34 0.026(4) 0.030(3) 0.030(4) -0.001(3) 0.014(3) 0.000(3) 
C35 0.027(4) 0.049(4) 0.046(5) 0.001(4) 0.009(4) -0.007(3) 
C36 0.039(5) 0.056(5) 0.064(6) -0.011(5) 0.016(5) -0.022(4) 
C37 0.046(5) 0.042(4) 0.049(5) -0.006(4) 0.021(4) -0.015(4) 
C38 0.041(5) 0.039(4) 0.040(5) 0.004(4) 0.014(4) -0.004(4) 
C39 0.029(4) 0.034(4) 0.038(5) 0.002(3) 0.012(4) -0.006(3) 
C1S 0.045(5) 0.053(5) 0.067(6) -0.018(4) 0.018(5) 0.006(4) 
Cl1 0.093(2) 0.125(2) 0.057(2) 0.003(2) 0.017(2) 0.008(2) 
Cl2 0.098(2) 0.0504(15) 0.111(2) -0.0034(14) 0.016(2) 0.0046(13) 
Cl3 0.0513(15) 0.222(4) 0.058(2) -0.013(2) 0.0145(14) -0.015(2) 
C2S 0.068(7) 0.058(5) 0.056(6) 0.008(5) -0.001(5) 0.001(5) 
Cl4 0.046(3) 0.117(7) 0.165(8) 0.075(6) 0.014(4) 0.023(3) 
Cl5 0.171(7) 0.071(5) 0.049(3) 0.012(3) 0.023(4) -0.003(4) 
Cl6 0.114(5) 0.063(3) 0.098(4) -0.041(3) -0.021(4) 0.006(3) 
Cl4' 0.129(14) 0.085(10) 0.226(26) -0.016(12) -0.069(13) -0.045(9) 
Cl5' 0.209(21) 0.125(18) 0.178(19) 0.092(14) 0.128(18) 0.043(15) 
Cl6' 0.348(33) 0.106(11) 0.113(12) 0.026(8) -0.050(18) -0.010(16) 
C3S 0.063(6) 0.045(5) 0.057(6) -0.005(4) 0.018(5) -0.006(4) 
Cl7 0.059(2) 0.053(2) 0.156(5) 0.015(2) 0.034(3) 0.000(2) 
Cl8 0.175(5) 0.048(2) 0.043(2) -0.009(2) 0.009(3) 0.000(2) 
Cl9 0.073(3) 0.130(4) 0.129(4) -0.025(3) 0.063(3) 0.003(3) 
Cl7' 0.327(34) 0.364(33) 0.176(20) 0.186(23) 0.211(24) 0.308(30) 
Cl8' 0.048(7) 0.158(14) 0.197(18) 0.069(13) 0.034(9) -0.007(8) 
Cl9' 0.183(20) 0.058(8) 0.229(24) 0.064(11) -0.064(16) -0.047(10) 
 
_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 
Ru1 O1 2.073(4) . ? 
Ru1 N1 2.084(5) . ? 
Ru1 C15 2.164(6) . ? 
Ru1 C14 2.207(7) . ? 
Ru1 C17 2.226(7) . ? 
Ru1 C18 2.231(7) . ? 
Ru1 C16 2.241(7) . ? 
Ru1 C13 2.274(7) . ? 
Ru1 P1 2.356(2) . ? 
P1 C28 1.829(6) . ? 
P1 C34 1.837(7) . ? 
P1 C22 1.838(7) . ? 
N1 C4 1.345(8) . ? 
N1 C2 1.406(8) . ? 
O2 C1 1.226(8) . ? 
O1 C1 1.292(8) . ? 
O3 C4 1.248(8) . ? 
C1 C2 1.512(9) . ? 
C2 C3 1.346(9) . ? 
C3 C6 1.458(9) . ? 
C5 C4 1.510(9) . ? 
C6 C11 1.388(9) . ? 
C6 C7 1.404(9) . ? 
C7 C8 1.377(10) . ? 
C8 C9 1.390(11) . ? 
C9 C10 1.387(11) . ? 
C10 C11 1.379(10) . ? 
C12 C13 1.483(9) . ? 
C13 C18 1.401(9) . ? 
C13 C14 1.428(9) . ? 
C14 C15 1.413(9) . ? 
C15 C16 1.426(10) . ? 
C16 C17 1.392(9) . ? 
C16 C19 1.511(9) . ? 
C17 C18 1.422(9) . ? 
C19 C20 1.508(11) . ? 
C19 C21 1.516(11) . ? 
C22 C23 1.387(9) . ? 
C22 C27 1.411(9) . ? 
C23 C24 1.388(10) . ? 
C24 C25 1.370(11) . ? 
C25 C26 1.375(11) . ? 
C26 C27 1.366(10) . ? 
C28 C29 1.386(9) . ? 
C28 C33 1.392(9) . ? 
C29 C30 1.400(9) . ? 
C30 C31 1.390(10) . ? 
C31 C32 1.375(10) . ? 
C32 C33 1.393(9) . ? 
C34 C39 1.388(9) . ? 
C34 C35 1.390(9) . ? 
C35 C36 1.382(10) . ? 
C36 C37 1.378(11) . ? 
C37 C38 1.368(11) . ? 
C38 C39 1.384(9) . ? 
C1S Cl3 1.751(4) . ? 
C1S Cl2 1.755(4) . ? 
C1S Cl1 1.755(4) . ? 
C2S Cl6 1.742(5) . ? 
C2S Cl5 1.757(5) . ? 
C2S Cl4 1.757(5) . ? 
C2S Cl5' 1.762(5) . ? 
C2S Cl4' 1.765(5) . ? 
C2S Cl6' 1.768(5) . ? 
Cl4 Cl4' 0.51(4) . ? 
Cl4 Cl6' 2.27(2) . ? 
Cl6 Cl6' 0.89(2) . ? 
C3S Cl8' 1.748(5) . ? 
C3S Cl7 1.750(4) . ? 
C3S Cl7' 1.753(5) . ? 
C3S Cl9' 1.767(5) . ? 
C3S Cl8 1.767(4) . ? 
C3S Cl9 1.771(4) . ? 
Cl7 Cl9' 1.40(2) . ? 
Cl7 Cl7' 2.13(3) . ? 
Cl8 Cl7' 0.98(3) . ? 
Cl8 Cl8' 2.45(2) . ? 
Cl9 Cl8' 1.22(2) . ? 
Cl9 Cl9' 2.17(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 
O1 Ru1 N1 77.4(2) . . ? 
O1 Ru1 C15 145.8(2) . . ? 
N1 Ru1 C15 90.2(2) . . ? 
O1 Ru1 C14 166.2(2) . . ? 
N1 Ru1 C14 116.0(2) . . ? 
C15 Ru1 C14 37.7(2) . . ? 
O1 Ru1 C17 92.1(2) . . ? 
N1 Ru1 C17 119.2(2) . . ? 
C15 Ru1 C17 66.2(3) . . ? 
C14 Ru1 C17 78.5(3) . . ? 
O1 Ru1 C18 100.2(2) . . ? 
N1 Ru1 C18 156.4(2) . . ? 
C15 Ru1 C18 78.8(3) . . ? 
C14 Ru1 C18 66.3(3) . . ? 
C17 Ru1 C18 37.2(2) . . ? 
O1 Ru1 C16 110.1(2) . . ? 
N1 Ru1 C16 91.7(2) . . ? 
C15 Ru1 C16 37.7(3) . . ? 
C14 Ru1 C16 67.9(3) . . ? 
C17 Ru1 C16 36.3(2) . . ? 
C18 Ru1 C16 66.9(3) . . ? 
O1 Ru1 C13 129.6(2) . . ? 
N1 Ru1 C13 153.0(2) . . ? 
C15 Ru1 C13 67.2(3) . . ? 
C14 Ru1 C13 37.1(2) . . ? 
C17 Ru1 C13 66.1(3) . . ? 
C18 Ru1 C13 36.2(2) . . ? 
C16 Ru1 C13 79.4(2) . . ? 
O1 Ru1 P1 81.78(13) . . ? 
N1 Ru1 P1 89.5(2) . . ? 
C15 Ru1 P1 130.4(2) . . ? 
C14 Ru1 P1 100.9(2) . . ? 
C17 Ru1 P1 148.7(2) . . ? 
C18 Ru1 P1 113.5(2) . . ? 
C16 Ru1 P1 168.1(2) . . ? 
C13 Ru1 P1 94.3(2) . . ? 
C28 P1 C34 103.8(3) . . ? 
C28 P1 C22 104.8(3) . . ? 
C34 P1 C22 100.4(3) . . ? 
C28 P1 Ru1 116.3(2) . . ? 
C34 P1 Ru1 112.8(2) . . ? 
C22 P1 Ru1 116.8(2) . . ? 
C4 N1 C2 124.4(6) . . ? 
C4 N1 Ru1 124.7(4) . . ? 
C2 N1 Ru1 110.2(4) . . ? 
C1 O1 Ru1 116.1(4) . . ? 
O2 C1 O1 122.1(6) . . ? 
O2 C1 C2 123.0(7) . . ? 
O1 C1 C2 114.9(6) . . ? 
C3 C2 N1 131.5(6) . . ? 
C3 C2 C1 116.5(6) . . ? 
N1 C2 C1 111.1(6) . . ? 
C2 C3 C6 135.9(6) . . ? 
O3 C4 N1 121.0(7) . . ? 
O3 C4 C5 118.0(7) . . ? 
N1 C4 C5 120.8(6) . . ? 
C11 C6 C7 117.0(7) . . ? 
C11 C6 C3 118.1(6) . . ? 
C7 C6 C3 124.7(6) . . ? 
C8 C7 C6 121.0(7) . . ? 
C7 C8 C9 120.8(8) . . ? 
C10 C9 C8 119.0(8) . . ? 
C11 C10 C9 119.7(7) . . ? 
C10 C11 C6 122.5(7) . . ? 
C18 C13 C14 118.1(6) . . ? 
C18 C13 C12 120.5(6) . . ? 
C14 C13 C12 121.4(6) . . ? 
C18 C13 Ru1 70.2(4) . . ? 
C14 C13 Ru1 68.9(4) . . ? 
C12 C13 Ru1 134.5(5) . . ? 
C15 C14 C13 119.8(6) . . ? 
C15 C14 Ru1 69.5(4) . . ? 
C13 C14 Ru1 74.0(4) . . ? 
C14 C15 C16 122.3(6) . . ? 
C14 C15 Ru1 72.8(4) . . ? 
C16 C15 Ru1 74.1(4) . . ? 
C17 C16 C15 116.6(6) . . ? 
C17 C16 C19 123.0(7) . . ? 
C15 C16 C19 120.4(7) . . ? 
C17 C16 Ru1 71.2(4) . . ? 
C15 C16 Ru1 68.2(4) . . ? 
C19 C16 Ru1 130.9(5) . . ? 
C16 C17 C18 122.3(6) . . ? 
C16 C17 Ru1 72.5(4) . . ? 
C18 C17 Ru1 71.6(4) . . ? 
C13 C18 C17 120.8(6) . . ? 
C13 C18 Ru1 73.6(4) . . ? 
C17 C18 Ru1 71.2(4) . . ? 
C20 C19 C16 114.7(7) . . ? 
C20 C19 C21 111.9(8) . . ? 
C16 C19 C21 109.8(7) . . ? 
C23 C22 C27 118.7(7) . . ? 
C23 C22 P1 122.5(5) . . ? 
C27 C22 P1 118.7(5) . . ? 
C22 C23 C24 119.4(7) . . ? 
C25 C24 C23 121.5(8) . . ? 
C24 C25 C26 119.3(8) . . ? 
C27 C26 C25 120.8(8) . . ? 
C26 C27 C22 120.4(8) . . ? 
C29 C28 C33 119.2(6) . . ? 
C29 C28 P1 119.2(5) . . ? 
C33 C28 P1 121.5(5) . . ? 
C28 C29 C30 120.1(6) . . ? 
C31 C30 C29 119.9(7) . . ? 
C32 C31 C30 120.3(6) . . ? 
C31 C32 C33 119.7(7) . . ? 
C28 C33 C32 120.8(7) . . ? 
C39 C34 C35 119.2(6) . . ? 
C39 C34 P1 120.9(5) . . ? 
C35 C34 P1 119.9(5) . . ? 
C36 C35 C34 120.1(7) . . ? 
C37 C36 C35 120.3(8) . . ? 
C38 C37 C36 119.8(7) . . ? 
C37 C38 C39 120.8(7) . . ? 
C38 C39 C34 119.9(7) . . ? 
Cl3 C1S Cl2 111.1(3) . . ? 
Cl3 C1S Cl1 109.1(3) . . ? 
Cl2 C1S Cl1 111.5(3) . . ? 
Cl6 C2S Cl5 109.3(5) . . ? 
Cl6 C2S Cl4 109.4(6) . . ? 
Cl5 C2S Cl4 109.8(7) . . ? 
Cl6 C2S Cl5' 93.8(9) . . ? 
Cl5 C2S Cl5' 15.8(10) . . ? 
Cl4 C2S Cl5' 114.2(12) . . ? 
Cl6 C2S Cl4' 122.0(9) . . ? 
Cl5 C2S Cl4' 94.1(11) . . ? 
Cl4 C2S Cl4' 16.7(13) . . ? 
Cl5' C2S Cl4' 100.7(15) . . ? 
Cl6 C2S Cl6' 29.2(8) . . ? 
Cl5 C2S Cl6' 120.4(9) . . ? 
Cl4 C2S Cl6' 80.2(9) . . ? 
Cl5' C2S Cl6' 105.3(11) . . ? 
Cl4' C2S Cl6' 93.2(11) . . ? 
Cl4' Cl4 C2S 82.5(11) . . ? 
Cl4' Cl4 Cl6' 120.0(23) . . ? 
C2S Cl4 Cl6' 50.1(5) . . ? 
Cl6' Cl6 C2S 77.0(6) . . ? 
Cl4 Cl4' C2S 80.7(10) . . ? 
Cl6 Cl6' C2S 73.7(6) . . ? 
Cl6 Cl6' Cl4 123.4(6) . . ? 
C2S Cl6' Cl4 49.7(4) . . ? 
Cl8' C3S Cl7 147.6(7) . . ? 
Cl8' C3S Cl7' 114.7(11) . . ? 
Cl7 C3S Cl7' 75.1(11) . . ? 
Cl8' C3S Cl9' 108.2(11) . . ? 
Cl7 C3S Cl9' 46.8(8) . . ? 
Cl7' C3S Cl9' 119.1(13) . . ? 
Cl8' C3S Cl8 88.5(7) . . ? 
Cl7 C3S Cl8 107.4(4) . . ? 
Cl7' C3S Cl8 32.5(11) . . ? 
Cl9' C3S Cl8 150.6(8) . . ? 
Cl8' C3S Cl9 40.7(5) . . ? 
Cl7 C3S Cl9 107.0(3) . . ? 
Cl7' C3S Cl9 113.2(6) . . ? 
Cl9' C3S Cl9 75.5(8) . . ? 
Cl8 C3S Cl9 106.1(4) . . ? 
Cl9' Cl7 C3S 67.2(4) . . ? 
Cl9' Cl7 Cl7' 116.9(8) . . ? 
C3S Cl7 Cl7' 52.5(6) . . ? 
Cl7' Cl8 C3S 73.0(7) . . ? 
Cl7' Cl8 Cl8' 110.8(9) . . ? 
C3S Cl8 Cl8' 45.5(4) . . ? 
Cl8' Cl9 C3S 68.7(4) . . ? 
Cl8' Cl9 Cl9' 111.2(6) . . ? 
C3S Cl9 Cl9' 52.2(4) . . ? 
Cl8 Cl7' C3S 74.5(6) . . ? 
Cl8 Cl7' Cl7 126.6(5) . . ? 
C3S Cl7' Cl7 52.4(6) . . ? 
Cl9 Cl8' C3S 70.7(4) . . ? 
Cl9 Cl8' Cl8 94.7(7) . . ? 
C3S Cl8' Cl8 46.1(4) . . ? 
Cl7 Cl9' C3S 66.0(5) . . ? 
Cl7 Cl9' Cl9 103.1(6) . . ? 
C3S Cl9' Cl9 52.4(4) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
 O3 C4 N1 C2 177.3(6) . . . . ? 
 
_refine_diff_density_max    0.571 
_refine_diff_density_min   -0.573 
_refine_diff_density_rms    0.091 
#=END
 
data_rk9424_(3a) 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C34 H34 Cl6 N O3 P Ru' 
_chemical_formula_weight          849.36 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 '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            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/n
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    10.667(3) 
_cell_length_b                    11.154(2) 
_cell_length_c                    30.814(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.36(2)
_cell_angle_gamma                 90.00 
_cell_volume                      3665.2(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     52
_cell_measurement_theta_min       5.6
_cell_measurement_theta_max       11.4
 
_exptl_crystal_description        block
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid           0.33 
_exptl_crystal_size_min           0.18 
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.539 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1720 
_exptl_absorpt_coefficient_mu     0.944 
_exptl_absorpt_correction_type    'semi-empirical based on psi scan data'
_exptl_absorpt_correction_T_min   0.65
_exptl_absorpt_correction_T_max   0.81
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4 diffractometer'
_diffrn_measurement_method        'omega scans'
_diffrn_standards_number          3
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         <1
_diffrn_reflns_number             7577 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0725 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        38 
_diffrn_reflns_theta_min          2.64 
_diffrn_reflns_theta_max          29.99 
_reflns_number_total              7577 
_reflns_number_observed           4629 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'XSCANS (Fait, 1991)' 
_computing_cell_refinement        'XSCANS (Fait, 1991)' 
_computing_data_reduction         'XSCANS (Fait, 1991)' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXLTL/PC ver5.0(Sheldrick, 1996)' 
_computing_molecular_graphics     'SHELXLTL/PC ver5.0(Sheldrick, 1996)' 
_computing_publication_material   'SHELXLTL/PC ver5.0(Sheldrick, 1996)' 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+2.3300P] 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          7577 
_refine_ls_number_parameters      415 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0943 
_refine_ls_R_factor_obs           0.0519 
_refine_ls_wR_factor_all          0.1218 
_refine_ls_wR_factor_obs          0.1046 
_refine_ls_goodness_of_fit_all    1.031 
_refine_ls_goodness_of_fit_obs    1.151 
_refine_ls_restrained_S_all       1.031 
_refine_ls_restrained_S_obs       1.151 
_refine_ls_shift/esd_max          0.002 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Ru1 Ru 0.13951(4) 0.17895(3) 0.153300(11) 0.03597(11) Uani 1 d . . 
P1 P 0.30804(13) 0.19385(11) 0.10561(4) 0.0421(3) Uani 1 d . . 
O1 O 0.2777(3) 0.1806(3) 0.20253(9) 0.0401(7) Uani 1 d . . 
C1 C 0.2806(4) 0.0846(4) 0.22571(14) 0.0394(11) Uani 1 d . . 
O2 O 0.3404(3) 0.0744(3) 0.26014(10) 0.0565(9) Uani 1 d . . 
C2 C 0.2045(4) -0.0179(4) 0.20708(14) 0.0404(11) Uani 1 d . . 
C3 C 0.1600(5) -0.1015(5) 0.2323(2) 0.0605(15) Uani 1 d . . 
H3A H 0.1760(5) -0.0991(5) 0.2630(2) 0.080 Uiso 1 d R . 
H3B H 0.1111(5) -0.1656(5) 0.2197(2) 0.080 Uiso 1 d R . 
N1 N 0.1784(4) -0.0030(3) 0.16227(11) 0.0380(9) Uani 1 d . . 
C4 C 0.1815(5) -0.0916(4) 0.1334(2) 0.0475(12) Uani 1 d . . 
O3 O 0.1509(4) -0.0774(3) 0.09439(10) 0.0599(10) Uani 1 d . . 
C5 C 0.2324(6) -0.2133(4) 0.1462(2) 0.067(2) Uani 1 d . . 
H5A H 0.2266(6) -0.2660(4) 0.1216(2) 0.080 Uiso 1 d R . 
H5B H 0.3186(6) -0.2056(4) 0.1555(2) 0.080 Uiso 1 d R . 
H5C H 0.1846(6) -0.2457(4) 0.1694(2) 0.080 Uiso 1 d R . 
C11 C 0.4170(5) 0.3167(5) 0.11866(15) 0.0523(12) Uani 1 d . . 
C12 C 0.3822(6) 0.4095(5) 0.1448(2) 0.0594(14) Uani 1 d . . 
H12A H 0.3038(6) 0.4116(5) 0.1565(2) 0.080 Uiso 1 d R . 
C13 C 0.4644(7) 0.5035(5) 0.1531(2) 0.078(2) Uani 1 d . . 
H13A H 0.4390(7) 0.5679(5) 0.1716(2) 0.080 Uiso 1 d R . 
C14 C 0.5802(8) 0.5034(7) 0.1358(2) 0.093(2) Uani 1 d . . 
H14A H 0.6363(8) 0.5689(7) 0.1417(2) 0.080 Uiso 1 d R . 
C15 C 0.6177(7) 0.4113(7) 0.1107(3) 0.104(3) Uani 1 d . . 
H15A H 0.6992(7) 0.4124(7) 0.0981(3) 0.080 Uiso 1 d R . 
C16 C 0.5364(6) 0.3180(6) 0.1020(2) 0.085(2) Uani 1 d . . 
H16A H 0.5618(6) 0.2535(6) 0.0836(2) 0.080 Uiso 1 d R . 
C21 C 0.4174(5) 0.0671(4) 0.10428(14) 0.0426(11) Uani 1 d . . 
C22 C 0.4446(5) 0.0056(5) 0.0666(2) 0.0574(14) Uani 1 d . . 
H22A H 0.4015(5) 0.0307(5) 0.0395(2) 0.080 Uiso 1 d R . 
C23 C 0.5289(5) -0.0872(5) 0.0675(2) 0.0626(15) Uani 1 d . . 
H23A H 0.5464(5) -0.1287(5) 0.0410(2) 0.080 Uiso 1 d R . 
C24 C 0.5855(5) -0.1221(5) 0.1058(2) 0.065(2) Uani 1 d . . 
H24A H 0.6439(5) -0.1876(5) 0.1061(2) 0.080 Uiso 1 d R . 
C25 C 0.5614(5) -0.0626(6) 0.1433(2) 0.068(2) Uani 1 d . . 
H25A H 0.6024(5) -0.0865(6) 0.1700(2) 0.080 Uiso 1 d R . 
C26 C 0.4787(5) 0.0333(5) 0.1426(2) 0.0576(14) Uani 1 d . . 
H26A H 0.4612(5) 0.0748(5) 0.1690(2) 0.080 Uiso 1 d R . 
C31 C 0.2623(5) 0.2197(4) 0.04865(14) 0.0491(13) Uani 1 d . . 
C32 C 0.1760(6) 0.1415(5) 0.0293(2) 0.061(2) Uani 1 d . . 
H32A H 0.1432(6) 0.0743(5) 0.0469(2) 0.080 Uiso 1 d R . 
C33 C 0.1344(7) 0.1590(6) -0.0130(2) 0.077(2) Uani 1 d . . 
H33A H 0.0741(7) 0.1052(6) -0.0261(2) 0.080 Uiso 1 d R . 
C34 C 0.1784(8) 0.2538(8) -0.0360(2) 0.090(2) Uani 1 d . . 
H34A H 0.1497(8) 0.2662(8) -0.0655(2) 0.080 Uiso 1 d R . 
C35 C 0.2635(8) 0.3303(6) -0.0182(2) 0.086(2) Uani 1 d . . 
H35A H 0.2950(8) 0.3965(6) -0.0346(2) 0.080 Uiso 1 d R . 
C36 C 0.3078(6) 0.3146(5) 0.0249(2) 0.069(2) Uani 1 d . . 
H36A H 0.3680(6) 0.3684(5) 0.0380(2) 0.080 Uiso 1 d R . 
C41 C -0.0580(5) 0.1430(5) 0.1344(2) 0.0533(13) Uani 1 d . . 
C42 C -0.0154(5) 0.2383(5) 0.10953(15) 0.0493(12) Uani 1 d . . 
H42A H -0.0120(5) 0.2247(5) 0.07732(15) 0.080 Uiso 1 d R . 
C43 C 0.0368(5) 0.3434(4) 0.1289(2) 0.0501(12) Uani 1 d . . 
C44 C 0.0480(5) 0.3491(5) 0.1740(2) 0.0521(13) Uani 1 d . . 
H44A H 0.0978(5) 0.4119(5) 0.1870(2) 0.080 Uiso 1 d R . 
C45 C 0.0034(5) 0.2553(5) 0.20015(15) 0.0509(13) Uani 1 d . . 
C46 C -0.0508(5) 0.1546(5) 0.1807(2) 0.0521(13) Uani 1 d . . 
H46A H -0.0675(5) 0.0855(5) 0.1982(2) 0.080 Uiso 1 d R . 
C47 C -0.1153(6) 0.0333(5) 0.1146(2) 0.075(2) Uani 1 d . . 
H47A H -0.2041(6) 0.0444(5) 0.1106(2) 0.080 Uiso 1 d R . 
H47B H -0.0780(6) 0.0201(5) 0.0870(2) 0.080 Uiso 1 d R . 
H47C H -0.0999(6) -0.0350(5) 0.1330(2) 0.080 Uiso 1 d R . 
C48 C 0.0734(6) 0.4484(5) 0.1001(2) 0.072(2) Uani 1 d . . 
H48A H 0.0032(6) 0.5015(5) 0.0963(2) 0.080 Uiso 1 d R . 
H48B H 0.1418(6) 0.4908(5) 0.1139(2) 0.080 Uiso 1 d R . 
H48C H 0.0988(6) 0.4195(5) 0.0724(2) 0.080 Uiso 1 d R . 
C49 C 0.0194(6) 0.2635(6) 0.2487(2) 0.071(2) Uani 1 d . . 
H49A H -0.0525(6) 0.3008(6) 0.2612(2) 0.080 Uiso 1 d R . 
H49B H 0.0293(6) 0.1841(6) 0.2603(2) 0.080 Uiso 1 d R . 
H49C H 0.0929(6) 0.3100(6) 0.2557(2) 0.080 Uiso 1 d R . 
C6 C 0.2346(6) 0.7298(6) 0.0230(2) 0.074(2) Uani 1 d . . 
H6A H 0.2050(6) 0.7727(6) 0.0477(2) 0.080 Uiso 1 d R . 
Cl1 Cl 0.2717(2) 0.8332(2) -0.01748(5) 0.0997(6) Uani 1 d . . 
Cl2 Cl 0.3665(2) 0.6454(2) 0.03903(7) 0.1092(7) Uani 1 d . . 
Cl3 Cl 0.1176(2) 0.6330(2) 0.00426(7) 0.1113(7) Uani 1 d . . 
C7 C 0.8889(6) 0.6670(6) 0.2322(2) 0.077(2) Uani 1 d . . 
H7A H 0.9764(6) 0.6468(6) 0.2335(2) 0.080 Uiso 1 d R . 
Cl4 Cl 0.8019(2) 0.5357(2) 0.23579(7) 0.1044(6) Uani 1 d . . 
Cl5 Cl 0.8560(2) 0.7599(2) 0.27608(9) 0.1309(8) Uani 1 d . . 
Cl6 Cl 0.8558(2) 0.7388(3) 0.18350(9) 0.1627(12) Uani 1 d . . 
 
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 
Ru1 0.0446(2) 0.0326(2) 0.0308(2) -0.0012(2) 0.00213(14) -0.0008(2) 
P1 0.0570(8) 0.0363(6) 0.0334(5) -0.0007(5) 0.0089(5) -0.0029(6) 
O1 0.043(2) 0.038(2) 0.0395(15) -0.0037(15) 0.0001(13) 0.001(2) 
C1 0.039(3) 0.044(3) 0.035(2) -0.003(2) 0.005(2) 0.000(2) 
O2 0.064(2) 0.059(2) 0.046(2) 0.004(2) -0.017(2) 0.000(2) 
C2 0.047(3) 0.039(2) 0.034(2) -0.001(2) 0.000(2) 0.001(2) 
C3 0.083(4) 0.053(3) 0.045(3) 0.006(2) 0.001(3) -0.014(3) 
N1 0.047(2) 0.031(2) 0.036(2) -0.0007(15) 0.002(2) -0.005(2) 
C4 0.059(3) 0.038(3) 0.046(3) -0.001(2) 0.005(3) -0.009(2) 
O3 0.090(3) 0.047(2) 0.043(2) -0.007(2) -0.005(2) 0.002(2) 
C5 0.096(5) 0.040(3) 0.064(3) -0.003(2) 0.000(3) 0.005(3) 
C11 0.066(3) 0.046(3) 0.045(2) 0.005(2) 0.011(2) -0.010(3) 
C12 0.074(4) 0.050(3) 0.054(3) -0.005(3) -0.006(3) -0.010(3) 
C13 0.109(6) 0.058(4) 0.067(4) -0.011(3) -0.016(4) -0.015(4) 
C14 0.101(6) 0.079(5) 0.099(5) 0.012(4) -0.016(5) -0.050(5) 
C15 0.088(6) 0.094(6) 0.130(7) 0.009(5) 0.034(5) -0.041(5) 
C16 0.086(5) 0.068(4) 0.103(5) -0.016(4) 0.037(4) -0.020(4) 
C21 0.047(3) 0.041(3) 0.041(2) 0.002(2) 0.011(2) -0.006(2) 
C22 0.072(4) 0.048(3) 0.052(3) -0.007(2) 0.007(3) 0.010(3) 
C23 0.069(4) 0.053(3) 0.066(3) -0.016(3) 0.008(3) 0.008(3) 
C24 0.056(4) 0.058(3) 0.082(4) -0.001(3) 0.008(3) 0.011(3) 
C25 0.046(3) 0.097(5) 0.062(3) 0.019(3) 0.009(3) 0.013(3) 
C26 0.051(3) 0.076(4) 0.047(3) -0.005(3) 0.012(3) 0.003(3) 
C31 0.074(4) 0.040(3) 0.034(2) -0.001(2) 0.013(2) 0.013(3) 
C32 0.088(4) 0.056(3) 0.038(3) -0.003(2) 0.000(3) 0.020(3) 
C33 0.105(5) 0.086(5) 0.040(3) -0.013(3) -0.010(3) 0.028(4) 
C34 0.130(7) 0.106(6) 0.034(3) -0.003(3) 0.008(4) 0.055(5) 
C35 0.137(7) 0.068(4) 0.055(4) 0.022(3) 0.039(4) 0.042(5) 
C36 0.109(5) 0.047(3) 0.053(3) 0.015(3) 0.024(3) 0.014(4) 
C41 0.045(3) 0.056(3) 0.058(3) -0.004(3) -0.003(3) -0.003(3) 
C42 0.055(3) 0.054(3) 0.039(2) 0.002(2) -0.003(2) 0.010(3) 
C43 0.053(3) 0.040(3) 0.058(3) 0.008(2) 0.000(2) 0.010(2) 
C44 0.054(3) 0.048(3) 0.055(3) -0.014(2) 0.000(3) 0.011(3) 
C45 0.045(3) 0.068(3) 0.039(2) -0.008(2) 0.006(2) 0.018(3) 
C46 0.048(3) 0.058(3) 0.051(3) 0.006(2) 0.009(2) 0.006(3) 
C47 0.064(4) 0.077(4) 0.084(4) 0.000(3) -0.012(3) -0.022(4) 
C48 0.084(4) 0.053(3) 0.078(4) 0.018(3) -0.005(3) 0.008(3) 
C49 0.067(4) 0.100(5) 0.047(3) -0.012(3) 0.013(3) 0.015(4) 
C6 0.104(5) 0.067(4) 0.053(3) -0.001(3) 0.003(3) 0.020(4) 
Cl1 0.154(2) 0.0793(12) 0.0661(9) 0.0046(9) 0.0058(11) -0.0100(13) 
Cl2 0.1010(14) 0.0754(12) 0.149(2) -0.0106(12) -0.0398(13) 0.0166(11) 
Cl3 0.0856(13) 0.110(2) 0.138(2) 0.0348(14) -0.0091(12) -0.0039(12) 
C7 0.053(3) 0.072(4) 0.106(5) 0.013(4) -0.007(3) 0.004(3) 
Cl4 0.0957(14) 0.0731(12) 0.145(2) 0.0102(12) 0.0038(13) -0.0101(11) 
Cl5 0.098(2) 0.106(2) 0.188(2) -0.039(2) 0.011(2) 0.0070(13) 
Cl6 0.141(2) 0.182(3) 0.162(2) 0.098(2) -0.066(2) -0.058(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 
Ru1 N1 2.088(4) . ? 
Ru1 O1 2.090(3) . ? 
Ru1 C41 2.209(5) . ? 
Ru1 C42 2.210(5) . ? 
Ru1 C46 2.233(5) . ? 
Ru1 C44 2.235(5) . ? 
Ru1 C45 2.239(5) . ? 
Ru1 C43 2.257(5) . ? 
Ru1 P1 2.3545(13) . ? 
P1 C31 1.833(5) . ? 
P1 C21 1.834(5) . ? 
P1 C11 1.835(5) . ? 
O1 C1 1.287(5) . ? 
C1 O2 1.230(5) . ? 
C1 C2 1.507(6) . ? 
C2 C3 1.310(6) . ? 
C2 N1 1.412(5) . ? 
N1 C4 1.331(6) . ? 
C4 O3 1.248(5) . ? 
C4 C5 1.511(7) . ? 
C11 C12 1.368(7) . ? 
C11 C16 1.384(8) . ? 
C12 C13 1.387(8) . ? 
C13 C14 1.357(9) . ? 
C14 C15 1.353(10) . ? 
C15 C16 1.376(9) . ? 
C21 C22 1.386(6) . ? 
C21 C26 1.388(7) . ? 
C22 C23 1.371(7) . ? 
C23 C24 1.371(7) . ? 
C24 C25 1.361(8) . ? 
C25 C26 1.386(8) . ? 
C31 C36 1.381(7) . ? 
C31 C32 1.392(7) . ? 
C32 C33 1.381(7) . ? 
C33 C34 1.363(9) . ? 
C34 C35 1.353(10) . ? 
C35 C36 1.412(8) . ? 
C41 C42 1.393(7) . ? 
C41 C46 1.432(6) . ? 
C41 C47 1.492(7) . ? 
C42 C43 1.422(7) . ? 
C43 C44 1.394(6) . ? 
C43 C48 1.525(7) . ? 
C44 C45 1.411(7) . ? 
C45 C46 1.393(7) . ? 
C45 C49 1.506(6) . ? 
C6 Cl3 1.739(7) . ? 
C6 Cl1 1.750(6) . ? 
C6 Cl2 1.754(6) . ? 
C7 Cl6 1.730(6) . ? 
C7 Cl4 1.738(6) . ? 
C7 Cl5 1.746(7) . ? 
 
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 Ru1 O1 77.15(13) . . ? 
N1 Ru1 C41 92.5(2) . . ? 
O1 Ru1 C41 147.6(2) . . ? 
N1 Ru1 C42 121.0(2) . . ? 
O1 Ru1 C42 160.9(2) . . ? 
C41 Ru1 C42 36.7(2) . . ? 
N1 Ru1 C46 90.7(2) . . ? 
O1 Ru1 C46 111.04(15) . . ? 
C41 Ru1 C46 37.6(2) . . ? 
C42 Ru1 C46 66.0(2) . . ? 
N1 Ru1 C44 151.0(2) . . ? 
O1 Ru1 C44 95.2(2) . . ? 
C41 Ru1 C44 79.0(2) . . ? 
C42 Ru1 C44 66.1(2) . . ? 
C46 Ru1 C44 65.7(2) . . ? 
N1 Ru1 C45 114.5(2) . . ? 
O1 Ru1 C45 89.19(15) . . ? 
C41 Ru1 C45 67.1(2) . . ? 
C42 Ru1 C45 78.0(2) . . ? 
C46 Ru1 C45 36.3(2) . . ? 
C44 Ru1 C45 36.8(2) . . ? 
N1 Ru1 C43 158.0(2) . . ? 
O1 Ru1 C43 124.3(2) . . ? 
C41 Ru1 C43 66.9(2) . . ? 
C42 Ru1 C43 37.1(2) . . ? 
C46 Ru1 C43 77.6(2) . . ? 
C44 Ru1 C43 36.2(2) . . ? 
C45 Ru1 C43 65.7(2) . . ? 
N1 Ru1 P1 89.93(10) . . ? 
O1 Ru1 P1 85.20(9) . . ? 
C41 Ru1 P1 125.86(14) . . ? 
C42 Ru1 P1 99.73(13) . . ? 
C46 Ru1 P1 163.45(13) . . ? 
C44 Ru1 P1 117.61(14) . . ? 
C45 Ru1 P1 153.1(2) . . ? 
C43 Ru1 P1 96.12(13) . . ? 
C31 P1 C21 104.7(2) . . ? 
C31 P1 C11 104.2(2) . . ? 
C21 P1 C11 100.4(2) . . ? 
C31 P1 Ru1 114.8(2) . . ? 
C21 P1 Ru1 117.08(15) . . ? 
C11 P1 Ru1 113.9(2) . . ? 
C1 O1 Ru1 113.7(3) . . ? 
O2 C1 O1 124.1(4) . . ? 
O2 C1 C2 121.5(4) . . ? 
O1 C1 C2 114.5(4) . . ? 
C3 C2 N1 126.7(4) . . ? 
C3 C2 C1 120.9(4) . . ? 
N1 C2 C1 112.0(4) . . ? 
C4 N1 C2 124.0(4) . . ? 
C4 N1 Ru1 129.9(3) . . ? 
C2 N1 Ru1 106.1(3) . . ? 
O3 C4 N1 122.6(4) . . ? 
O3 C4 C5 116.7(4) . . ? 
N1 C4 C5 120.5(4) . . ? 
C12 C11 C16 118.3(5) . . ? 
C12 C11 P1 121.0(4) . . ? 
C16 C11 P1 120.7(4) . . ? 
C11 C12 C13 120.1(6) . . ? 
C14 C13 C12 120.2(6) . . ? 
C15 C14 C13 120.7(7) . . ? 
C14 C15 C16 119.4(7) . . ? 
C15 C16 C11 121.2(6) . . ? 
C22 C21 C26 118.3(5) . . ? 
C22 C21 P1 123.1(4) . . ? 
C26 C21 P1 118.5(4) . . ? 
C23 C22 C21 120.5(5) . . ? 
C24 C23 C22 120.4(5) . . ? 
C25 C24 C23 120.3(6) . . ? 
C24 C25 C26 119.7(5) . . ? 
C25 C26 C21 120.7(5) . . ? 
C36 C31 C32 119.4(5) . . ? 
C36 C31 P1 122.6(4) . . ? 
C32 C31 P1 118.0(4) . . ? 
C33 C32 C31 120.7(6) . . ? 
C34 C33 C32 119.6(7) . . ? 
C35 C34 C33 121.0(6) . . ? 
C34 C35 C36 120.7(6) . . ? 
C31 C36 C35 118.6(6) . . ? 
C42 C41 C46 117.9(5) . . ? 
C42 C41 C47 122.5(5) . . ? 
C46 C41 C47 119.5(5) . . ? 
C42 C41 Ru1 71.6(3) . . ? 
C46 C41 Ru1 72.1(3) . . ? 
C47 C41 Ru1 129.5(4) . . ? 
C41 C42 C43 121.8(4) . . ? 
C41 C42 Ru1 71.6(3) . . ? 
C43 C42 Ru1 73.2(3) . . ? 
C44 C43 C42 118.7(4) . . ? 
C44 C43 C48 121.8(5) . . ? 
C42 C43 C48 119.5(5) . . ? 
C44 C43 Ru1 71.1(3) . . ? 
C42 C43 Ru1 69.7(3) . . ? 
C48 C43 Ru1 133.5(4) . . ? 
C43 C44 C45 120.9(5) . . ? 
C43 C44 Ru1 72.8(3) . . ? 
C45 C44 Ru1 71.8(3) . . ? 
C46 C45 C44 119.6(4) . . ? 
C46 C45 C49 121.0(5) . . ? 
C44 C45 C49 119.4(5) . . ? 
C46 C45 Ru1 71.6(3) . . ? 
C44 C45 Ru1 71.4(3) . . ? 
C49 C45 Ru1 127.2(4) . . ? 
C45 C46 C41 121.0(5) . . ? 
C45 C46 Ru1 72.1(3) . . ? 
C41 C46 Ru1 70.3(3) . . ? 
Cl3 C6 Cl1 110.2(3) . . ? 
Cl3 C6 Cl2 109.0(3) . . ? 
Cl1 C6 Cl2 111.2(4) . . ? 
Cl6 C7 Cl4 110.3(4) . . ? 
Cl6 C7 Cl5 110.9(4) . . ? 
Cl4 C7 Cl5 109.5(4) . . ? 
 
_refine_diff_density_max    0.709 
_refine_diff_density_min   -0.574 
_refine_diff_density_rms    0.082