# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1676 data_3b #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 10 10:25:20 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 873.69 _chemical_formula_analytical ? _chemical_formula_sum 'C29 H43 Cl4 O7 P S3 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural [RuCl3(dmso)3][BDMPP-CH2Cl2] _cell_length_a 13.824(3) _cell_length_b 9.671(3) _cell_length_c 15.292(2) _cell_angle_alpha 90 _cell_angle_beta 112.35(1) _cell_angle_gamma 90 _cell_volume 1890.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 297.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 12.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 896.00 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 297.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.12 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 3 2 -2 1 2 -1 1 _diffrn_reflns_number 3713 _reflns_number_total 3559 _reflns_number_observed 2858 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 1.71 _diffrn_reflns_av_sigmaI/netI 0.062 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06520 _diffrn_orient_matrix_UB_12 -0.00095 _diffrn_orient_matrix_UB_13 0.05853 _diffrn_orient_matrix_UB_21 -0.04250 _diffrn_orient_matrix_UB_22 0.01715 _diffrn_orient_matrix_UB_23 0.03921 _diffrn_orient_matrix_UB_31 -0.00776 _diffrn_orient_matrix_UB_32 -0.10197 _diffrn_orient_matrix_UB_33 0.00605 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 58 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 86 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 14 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 6 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 2 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru -0.01203(3) 0.5013(1) 0.22965(3) 0.02803(9) Uani d . 1.00 . Cl1 0.6904(2) 0.4123(3) 0.4584(1) 0.0824(7) Uani d . 1.00 . Cl2 -0.1601(1) 0.6534(2) 0.2005(1) 0.0433(4) Uani d . 1.00 . Cl3 -0.1033(1) 0.4183(2) 0.0685(1) 0.0479(4) Uani d . 1.00 . Cl4 -0.1019(1) 0.3284(2) 0.2868(1) 0.0571(5) Uani d . 1.00 . S1 0.1150(1) 0.3386(2) 0.2564(1) 0.0423(4) Uani d . 1.00 . S2 0.0562(1) 0.5983(2) 0.3755(1) 0.0416(4) Uani d . 1.00 . S3 0.0711(1) 0.6534(2) 0.1699(1) 0.0366(4) Uani d . 1.00 . P 0.5859(1) 0.2623(2) 0.2737(1) 0.0303(4) Uani d . 1.00 . O1 0.4008(3) 0.1937(5) 0.1290(3) 0.047(1) Uani d . 1.00 . O2 0.5837(4) 0.1164(7) 0.4501(3) 0.079(2) Uani d . 1.00 . O3 0.5557(3) 0.3537(5) 0.0722(3) 0.054(1) Uani d . 1.00 . O4 0.6939(3) 0.0119(6) 0.3019(3) 0.051(1) Uani d . 1.00 . O5 0.2086(3) 0.3707(6) 0.2387(4) 0.066(1) Uani d . 1.00 . O6 0.1621(3) 0.5600(5) 0.4409(3) 0.058(1) Uani d . 1.00 . O7 0.1642(3) 0.7261(5) 0.2367(3) 0.056(1) Uani d . 1.00 . C1 0.5387(4) 0.4379(6) 0.2453(4) 0.033(1) Uani d . 1.00 . C2 0.4412(4) 0.4750(7) 0.2460(4) 0.038(1) Uani d . 1.00 . C3 0.4140(5) 0.6152(8) 0.2355(4) 0.048(2) Uani d . 1.00 . C4 0.4790(6) 0.7082(7) 0.2217(5) 0.057(2) Uani d . 1.00 . C5 0.5726(5) 0.6711(7) 0.2176(5) 0.055(2) Uani d . 1.00 . C6 0.6042(4) 0.5333(6) 0.2308(4) 0.044(2) Uani d . 1.00 . C7 0.4888(4) 0.1525(7) 0.2890(4) 0.035(1) Uani d . 1.00 . C8 0.3998(4) 0.1272(6) 0.2064(4) 0.038(1) Uani d . 1.00 . C9 0.3225(4) 0.0380(6) 0.2083(5) 0.052(2) Uani d . 1.00 . C10 0.3340(5) -0.0255(7) 0.2925(5) 0.058(2) Uani d . 1.00 . C11 0.4184(5) -0.0005(10) 0.3741(5) 0.063(2) Uani d . 1.00 . C12 0.4978(5) 0.0872(8) 0.3735(4) 0.051(2) Uani d . 1.00 . C13 0.3059(5) 0.2203(10) 0.0535(5) 0.075(2) Uani d . 1.00 . C14 0.5921(6) 0.065(1) 0.5387(5) 0.109(4) Uani d . 1.00 . C15 0.6321(4) 0.1875(6) 0.1890(4) 0.033(1) Uani d . 1.00 . C16 0.6193(4) 0.2413(7) 0.1010(4) 0.041(1) Uani d . 1.00 . C17 0.6686(5) 0.1836(8) 0.0470(4) 0.053(2) Uani d . 1.00 . C18 0.7285(6) 0.0644(8) 0.0795(5) 0.060(2) Uani d . 1.00 . C19 0.7399(4) 0.0067(9) 0.1643(4) 0.051(2) Uani d . 1.00 . C20 0.6910(5) 0.0638(7) 0.2175(4) 0.041(1) Uani d . 1.00 . C21 0.5661(7) 0.4423(9) 0.0024(5) 0.087(3) Uani d . 1.00 . C22 0.7755(6) -0.0819(9) 0.3526(5) 0.078(2) Uani d . 1.00 . C23 0.7045(4) 0.2864(8) 0.3796(4) 0.043(2) Uani d . 1.00 . C24 0.1608(6) 0.2635(9) 0.3720(5) 0.070(2) Uani d . 1.00 . C25 0.0601(6) 0.1874(8) 0.1906(6) 0.067(2) Uani d . 1.00 . C26 -0.0279(5) 0.5743(10) 0.4391(4) 0.069(2) Uani d . 1.00 . C27 0.0555(6) 0.7840(8) 0.3739(5) 0.061(2) Uani d . 1.00 . C28 0.1120(5) 0.5862(8) 0.0807(4) 0.056(2) Uani d . 1.00 . C29 -0.0149(6) 0.7871(8) 0.1015(5) 0.065(2) Uani d . 1.00 . H4 0.3932 0.4036 0.2524 0.0450 Uiso calc . 1.00 . H5 0.3484 0.6448 0.2397 0.0570 Uiso calc . 1.00 . H6 0.4547 0.8055 0.2120 0.0659 Uiso calc . 1.00 . H7 0.6173 0.7409 0.2066 0.0661 Uiso calc . 1.00 . H8 0.6708 0.5049 0.2296 0.0546 Uiso calc . 1.00 . H9 0.2623 0.0216 0.1508 0.0609 Uiso calc . 1.00 . H10 0.2824 -0.0908 0.2930 0.0678 Uiso calc . 1.00 . H11 0.4227 -0.0412 0.4347 0.0765 Uiso calc . 1.00 . H12 0.2607 0.2792 0.0708 0.0989 Uiso calc . 1.00 . H13 0.3197 0.2700 0.0027 0.0989 Uiso calc . 1.00 . H14 0.2694 0.1386 0.0256 0.0989 Uiso calc . 1.00 . H15 0.5313 0.0935 0.5544 0.1161 Uiso calc . 1.00 . H16 0.5878 -0.0363 0.5376 0.1161 Uiso calc . 1.00 . H17 0.6523 0.0912 0.5893 0.1161 Uiso calc . 1.00 . H18 0.6640 0.2261 -0.0118 0.0637 Uiso calc . 1.00 . H19 0.7574 0.0210 0.0387 0.0745 Uiso calc . 1.00 . H20 0.7855 -0.0722 0.1872 0.0606 Uiso calc . 1.00 . H21 0.6361 0.4809 0.0237 0.1061 Uiso calc . 1.00 . H22 0.5522 0.3962 -0.0552 0.1061 Uiso calc . 1.00 . H23 0.5189 0.5206 -0.0090 0.1061 Uiso calc . 1.00 . H24 0.7707 -0.1078 0.4098 0.0867 Uiso calc . 1.00 . H25 0.7724 -0.1611 0.3147 0.0867 Uiso calc . 1.00 . H26 0.8428 -0.0377 0.3661 0.0867 Uiso calc . 1.00 . H27 0.7601 0.3142 0.3602 0.0528 Uiso calc . 1.00 . H28 0.7234 0.1999 0.4118 0.0528 Uiso calc . 1.00 . H29 0.1015 0.2397 0.3893 0.0833 Uiso calc . 1.00 . H30 0.1990 0.1811 0.3750 0.0833 Uiso calc . 1.00 . H31 0.2032 0.3268 0.4187 0.0833 Uiso calc . 1.00 . H32 -0.0038 0.1639 0.1995 0.0789 Uiso calc . 1.00 . H33 0.0419 0.2046 0.1248 0.0789 Uiso calc . 1.00 . H34 0.1066 0.1130 0.2103 0.0789 Uiso calc . 1.00 . H35 -0.0039 0.6304 0.4963 0.0804 Uiso calc . 1.00 . H36 -0.0973 0.5961 0.4032 0.0804 Uiso calc . 1.00 . H37 -0.0241 0.4789 0.4607 0.0804 Uiso calc . 1.00 . H38 0.0572 0.5339 0.0340 0.0733 Uiso calc . 1.00 . H39 0.1348 0.6560 0.0498 0.0733 Uiso calc . 1.00 . H40 0.1705 0.5213 0.1084 0.0733 Uiso calc . 1.00 . H41 -0.0336 0.8485 0.1422 0.0780 Uiso calc . 1.00 . H42 0.0194 0.8420 0.0693 0.0780 Uiso calc . 1.00 . H43 -0.0769 0.7496 0.0561 0.0780 Uiso calc . 1.00 . H44 0.0750 0.8205 0.4347 0.0738 Uiso calc . 1.00 . H45 0.1104 0.8152 0.3499 0.0738 Uiso calc . 1.00 . H46 -0.0078 0.8188 0.3321 0.0738 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0232(2) 0.0299(2) 0.0314(2) -0.0012(2) 0.0109(1) -0.0024(3) Cl(1) 0.079(1) 0.098(2) 0.058(1) 0.020(1) 0.0124(9) -0.029(1) Cl(2) 0.0299(7) 0.0469(9) 0.0513(8) 0.0075(7) 0.0135(6) -0.0043(8) Cl(3) 0.0417(8) 0.052(1) 0.0432(8) -0.0049(8) 0.0088(6) -0.0189(8) Cl(4) 0.0566(9) 0.045(1) 0.085(1) -0.0130(8) 0.0449(7) 0.0020(9) S(1) 0.0361(7) 0.0368(9) 0.0551(9) 0.0066(7) 0.0186(6) 0.0020(8) S(2) 0.0418(8) 0.0484(10) 0.0304(7) 0.0034(8) 0.0088(6) -0.0040(7) S(3) 0.0339(7) 0.0370(8) 0.0399(8) -0.0055(7) 0.0151(6) 0.0016(7) P 0.0233(6) 0.0355(9) 0.0317(7) -0.0008(7) 0.0098(5) -0.0027(7) O(1) 0.034(2) 0.048(3) 0.047(2) -0.003(2) 0.003(2) 0.000(2) O(2) 0.061(3) 0.132(5) 0.044(2) -0.020(3) 0.019(2) 0.027(3) O(3) 0.068(3) 0.056(3) 0.041(2) 0.020(2) 0.023(2) 0.002(2) O(4) 0.060(2) 0.046(3) 0.047(2) 0.011(3) 0.020(2) 0.002(2) O(5) 0.039(2) 0.062(3) 0.107(3) 0.009(2) 0.039(2) 0.013(3) O(6) 0.050(2) 0.063(3) 0.041(2) 0.013(2) -0.006(2) -0.005(2) O(7) 0.046(2) 0.058(3) 0.060(3) -0.027(2) 0.017(2) -0.013(2) C(1) 0.028(2) 0.037(2) 0.033(3) 0.002(2) 0.011(2) -0.007(3) C(2) 0.031(2) 0.053(3) 0.032(3) 0.013(3) 0.013(2) 0.001(3) C(3) 0.043(3) 0.053(3) 0.051(3) 0.019(3) 0.022(3) 0.000(3) C(4) 0.070(4) 0.032(4) 0.071(4) 0.010(3) 0.028(3) 0.007(4) C(5) 0.067(4) 0.034(3) 0.071(4) -0.008(3) 0.033(3) -0.005(4) C(6) 0.038(3) 0.038(3) 0.060(3) -0.009(2) 0.024(2) -0.005(3) C(7) 0.024(2) 0.037(3) 0.047(2) -0.002(2) 0.017(2) -0.003(3) C(8) 0.030(2) 0.028(3) 0.051(3) -0.002(2) 0.012(2) -0.010(2) C(9) 0.031(3) 0.033(4) 0.091(4) -0.011(2) 0.022(3) -0.022(3) C(10) 0.049(3) 0.036(4) 0.106(4) -0.016(3) 0.050(2) -0.007(3) C(11) 0.063(3) 0.051(4) 0.091(4) -0.009(4) 0.047(2) 0.011(5) C(12) 0.051(3) 0.054(4) 0.054(3) 0.000(3) 0.026(2) 0.016(3) C(13) 0.043(4) 0.085(6) 0.065(5) 0.009(4) -0.017(3) -0.002(5) C(14) 0.085(5) 0.20(1) 0.041(3) -0.017(7) 0.020(4) 0.045(5) C(15) 0.033(3) 0.034(3) 0.032(2) -0.008(2) 0.013(2) -0.011(2) C(16) 0.038(3) 0.046(3) 0.035(3) -0.013(2) 0.008(2) 0.002(2) C(17) 0.077(4) 0.051(4) 0.049(3) -0.013(3) 0.043(3) -0.019(3) C(18) 0.077(4) 0.058(4) 0.059(3) -0.001(3) 0.040(3) -0.020(3) C(19) 0.049(3) 0.045(4) 0.064(3) 0.007(4) 0.028(2) -0.012(3) C(20) 0.041(3) 0.031(3) 0.047(3) -0.009(2) 0.012(2) -0.008(2) C(21) 0.136(6) 0.069(5) 0.083(4) 0.017(5) 0.073(4) 0.046(4) C(22) 0.104(6) 0.068(5) 0.036(4) 0.056(4) -0.002(4) -0.001(4) C(23) 0.021(2) 0.064(4) 0.038(3) -0.004(3) 0.005(2) 0.009(2) C(24) 0.085(5) 0.061(5) 0.062(3) 0.034(4) 0.024(4) 0.024(4) C(25) 0.070(5) 0.038(4) 0.083(5) 0.005(3) 0.017(4) -0.017(3) C(26) 0.076(4) 0.102(6) 0.059(3) -0.012(4) 0.059(2) -0.006(4) C(27) 0.062(4) 0.047(2) 0.060(4) 0.008(4) 0.006(3) -0.025(4) C(28) 0.072(4) 0.068(5) 0.046(3) -0.005(4) 0.041(3) -0.013(3) C(29) 0.065(4) 0.054(4) 0.079(5) 0.022(3) 0.029(3) 0.041(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2858 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0405 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.352 _refine_ls_shift/esd_max 0.3660 _refine_ls_shift/esd_mean 0.0540 _refine_diff_density_min -0.36 _refine_diff_density_max 0.72 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl(2) 2.420(2) 1_555 1_555 yes Ru Cl(3) 2.438(2) 1_555 1_555 yes Ru Cl(4) 2.435(2) 1_555 1_555 yes Ru S(1) 2.276(2) 1_555 1_555 yes Ru S(2) 2.268(2) 1_555 1_555 yes Ru S(3) 2.263(2) 1_555 1_555 yes Cl(1) C(23) 1.775(8) 1_555 1_555 yes S(1) O(5) 1.452(6) 1_555 1_555 yes S(1) C(24) 1.789(8) 1_555 1_555 yes S(1) C(25) 1.773(9) 1_555 1_555 yes S(2) O(6) 1.472(5) 1_555 1_555 yes S(2) C(26) 1.793(7) 1_555 1_555 yes S(2) C(27) 1.796(9) 1_555 1_555 yes S(3) O(7) 1.481(5) 1_555 1_555 yes S(3) C(28) 1.785(7) 1_555 1_555 yes S(3) C(29) 1.797(8) 1_555 1_555 yes P C(1) 1.811(7) 1_555 1_555 yes P C(7) 1.795(7) 1_555 1_555 yes P C(15) 1.800(7) 1_555 1_555 yes P C(23) 1.829(6) 1_555 1_555 yes O(1) C(8) 1.352(8) 1_555 1_555 yes O(1) C(13) 1.403(8) 1_555 1_555 yes O(2) C(12) 1.343(8) 1_555 1_555 yes O(2) C(14) 1.406(10) 1_555 1_555 yes O(3) C(16) 1.362(9) 1_555 1_555 yes O(3) C(21) 1.418(10) 1_555 1_555 yes O(4) C(20) 1.371(8) 1_555 1_555 yes O(4) C(22) 1.426(9) 1_555 1_555 yes C(1) C(2) 1.398(9) 1_555 1_555 yes C(1) C(6) 1.368(10) 1_555 1_555 yes C(2) C(3) 1.40(1) 1_555 1_555 yes C(3) C(4) 1.34(1) 1_555 1_555 yes C(4) C(5) 1.37(1) 1_555 1_555 yes C(5) C(6) 1.39(1) 1_555 1_555 yes C(7) C(8) 1.410(9) 1_555 1_555 yes C(7) C(12) 1.400(10) 1_555 1_555 yes C(8) C(9) 1.382(10) 1_555 1_555 yes C(9) C(10) 1.38(1) 1_555 1_555 yes C(10) C(11) 1.37(1) 1_555 1_555 yes C(11) C(12) 1.39(1) 1_555 1_555 yes C(15) C(16) 1.390(9) 1_555 1_555 yes C(15) C(20) 1.419(10) 1_555 1_555 yes C(16) C(17) 1.37(1) 1_555 1_555 yes C(17) C(18) 1.40(1) 1_555 1_555 yes C(18) C(19) 1.36(1) 1_555 1_555 yes C(19) C(20) 1.36(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(2) Ru Cl(3) 86.41(6) 1_555 1_555 1_555 yes Cl(2) Ru Cl(4) 88.43(7) 1_555 1_555 1_555 yes Cl(2) Ru S(1) 173.66(7) 1_555 1_555 1_555 yes Cl(2) Ru S(2) 86.34(7) 1_555 1_555 1_555 yes Cl(2) Ru S(3) 93.10(7) 1_555 1_555 1_555 yes Cl(3) Ru Cl(4) 89.86(7) 1_555 1_555 1_555 yes Cl(3) Ru S(1) 91.24(7) 1_555 1_555 1_555 yes Cl(3) Ru S(2) 172.72(7) 1_555 1_555 1_555 yes Cl(3) Ru S(3) 87.31(7) 1_555 1_555 1_555 yes Cl(4) Ru S(1) 85.67(7) 1_555 1_555 1_555 yes Cl(4) Ru S(2) 90.54(7) 1_555 1_555 1_555 yes Cl(4) Ru S(3) 176.70(8) 1_555 1_555 1_555 yes S(1) Ru S(2) 96.03(7) 1_555 1_555 1_555 yes S(1) Ru S(3) 92.67(7) 1_555 1_555 1_555 yes S(2) Ru S(3) 92.48(7) 1_555 1_555 1_555 yes Ru S(1) O(5) 120.0(3) 1_555 1_555 1_555 yes Ru S(1) C(24) 114.7(3) 1_555 1_555 1_555 yes Ru S(1) C(25) 109.5(3) 1_555 1_555 1_555 yes O(5) S(1) C(24) 105.4(4) 1_555 1_555 1_555 yes O(5) S(1) C(25) 106.8(4) 1_555 1_555 1_555 yes C(24) S(1) C(25) 98.1(5) 1_555 1_555 1_555 yes Ru S(2) O(6) 119.9(2) 1_555 1_555 1_555 yes Ru S(2) C(26) 111.6(3) 1_555 1_555 1_555 yes Ru S(2) C(27) 113.7(3) 1_555 1_555 1_555 yes O(6) S(2) C(26) 106.4(4) 1_555 1_555 1_555 yes O(6) S(2) C(27) 105.0(4) 1_555 1_555 1_555 yes C(26) S(2) C(27) 97.8(5) 1_555 1_555 1_555 yes Ru S(3) O(7) 118.1(2) 1_555 1_555 1_555 yes Ru S(3) C(28) 115.4(3) 1_555 1_555 1_555 yes Ru S(3) C(29) 112.2(3) 1_555 1_555 1_555 yes O(7) S(3) C(28) 104.8(3) 1_555 1_555 1_555 yes O(7) S(3) C(29) 105.6(4) 1_555 1_555 1_555 yes C(28) S(3) C(29) 98.6(4) 1_555 1_555 1_555 yes C(1) P C(7) 111.5(3) 1_555 1_555 1_555 yes C(1) P C(15) 113.4(3) 1_555 1_555 1_555 yes C(1) P C(23) 102.3(3) 1_555 1_555 1_555 yes C(7) P C(15) 110.1(3) 1_555 1_555 1_555 yes C(7) P C(23) 115.1(3) 1_555 1_555 1_555 yes C(15) P C(23) 104.1(3) 1_555 1_555 1_555 yes C(8) O(1) C(13) 119.4(6) 1_555 1_555 1_555 yes C(12) O(2) C(14) 119.2(7) 1_555 1_555 1_555 yes C(16) O(3) C(21) 119.2(6) 1_555 1_555 1_555 yes C(20) O(4) C(22) 118.6(6) 1_555 1_555 1_555 yes P C(1) C(2) 119.9(6) 1_555 1_555 1_555 yes P C(1) C(6) 118.1(5) 1_555 1_555 1_555 yes C(2) C(1) C(6) 121.8(7) 1_555 1_555 1_555 yes C(1) C(2) C(3) 117.8(7) 1_555 1_555 1_555 yes C(1) C(2) H(4) 120.5(7) 1_555 1_555 1_555 no C(3) C(2) H(4) 121.7(6) 1_555 1_555 1_555 no C(2) C(3) C(4) 120.0(7) 1_555 1_555 1_555 yes C(2) C(3) H(5) 119.5(8) 1_555 1_555 1_555 no C(4) C(3) H(5) 120.5(8) 1_555 1_555 1_555 no C(3) C(4) C(5) 122.2(8) 1_555 1_555 1_555 yes C(3) C(4) H(6) 116.8(8) 1_555 1_555 1_555 no C(5) C(4) H(6) 120.9(8) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.6(7) 1_555 1_555 1_555 yes C(4) C(5) H(7) 120.1(8) 1_555 1_555 1_555 no C(6) C(5) H(7) 120.3(8) 1_555 1_555 1_555 no C(1) C(6) C(5) 118.6(7) 1_555 1_555 1_555 yes C(1) C(6) H(8) 120.3(7) 1_555 1_555 1_555 no C(5) C(6) H(8) 121.1(7) 1_555 1_555 1_555 no P C(7) C(8) 115.3(5) 1_555 1_555 1_555 yes P C(7) C(12) 125.3(5) 1_555 1_555 1_555 yes C(8) C(7) C(12) 119.3(7) 1_555 1_555 1_555 yes O(1) C(8) C(7) 113.9(6) 1_555 1_555 1_555 yes O(1) C(8) C(9) 125.5(6) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120.5(7) 1_555 1_555 1_555 yes C(8) C(9) C(10) 118.8(7) 1_555 1_555 1_555 yes C(8) C(9) H(9) 119.3(8) 1_555 1_555 1_555 no C(10) C(9) H(9) 121.9(7) 1_555 1_555 1_555 no C(9) C(10) C(11) 121.8(7) 1_555 1_555 1_555 yes C(9) C(10) H(10) 118.7(8) 1_555 1_555 1_555 no C(11) C(10) H(10) 119.5(9) 1_555 1_555 1_555 no C(10) C(11) C(12) 120.3(8) 1_555 1_555 1_555 yes C(10) C(11) H(11) 120.8(8) 1_555 1_555 1_555 no C(12) C(11) H(11) 118.9(7) 1_555 1_555 1_555 no O(2) C(12) C(7) 116.7(7) 1_555 1_555 1_555 yes O(2) C(12) C(11) 124.1(7) 1_555 1_555 1_555 yes C(7) C(12) C(11) 119.1(7) 1_555 1_555 1_555 yes O(1) C(13) H(12) 112.8(8) 1_555 1_555 1_555 no O(1) C(13) H(13) 109.6(8) 1_555 1_555 1_555 no O(1) C(13) H(14) 112.9(9) 1_555 1_555 1_555 no H(12) C(13) H(13) 105.6(10) 1_555 1_555 1_555 no H(12) C(13) H(14) 109.3(9) 1_555 1_555 1_555 no H(13) C(13) H(14) 106.1(9) 1_555 1_555 1_555 no O(2) C(14) H(15) 111.5(9) 1_555 1_555 1_555 no O(2) C(14) H(16) 110.7(10) 1_555 1_555 1_555 no O(2) C(14) H(17) 115.2(10) 1_555 1_555 1_555 no H(15) C(14) H(16) 103.2(10) 1_555 1_555 1_555 no H(15) C(14) H(17) 107(1) 1_555 1_555 1_555 no H(16) C(14) H(17) 108(1) 1_555 1_555 1_555 no P C(15) C(16) 126.7(6) 1_555 1_555 1_555 yes P C(15) C(20) 115.9(5) 1_555 1_555 1_555 yes C(16) C(15) C(20) 117.3(6) 1_555 1_555 1_555 yes O(3) C(16) C(15) 116.2(7) 1_555 1_555 1_555 yes O(3) C(16) C(17) 122.5(7) 1_555 1_555 1_555 yes C(15) C(16) C(17) 121.4(7) 1_555 1_555 1_555 yes C(16) C(17) C(18) 119.0(7) 1_555 1_555 1_555 yes C(16) C(17) H(18) 120.9(8) 1_555 1_555 1_555 no C(18) C(17) H(18) 120.1(7) 1_555 1_555 1_555 no C(17) C(18) C(19) 120.9(7) 1_555 1_555 1_555 yes C(17) C(18) H(19) 118.0(8) 1_555 1_555 1_555 no C(19) C(18) H(19) 120.9(9) 1_555 1_555 1_555 no C(18) C(19) C(20) 119.9(8) 1_555 1_555 1_555 yes C(18) C(19) H(20) 119.4(7) 1_555 1_555 1_555 no C(20) C(19) H(20) 120.6(7) 1_555 1_555 1_555 no O(4) C(20) C(15) 113.9(6) 1_555 1_555 1_555 yes O(4) C(20) C(19) 124.9(7) 1_555 1_555 1_555 yes C(15) C(20) C(19) 121.2(7) 1_555 1_555 1_555 yes O(3) C(21) H(21) 110.7(8) 1_555 1_555 1_555 no O(3) C(21) H(22) 112.1(9) 1_555 1_555 1_555 no O(3) C(21) H(23) 110.6(8) 1_555 1_555 1_555 no H(21) C(21) H(22) 108.6(9) 1_555 1_555 1_555 no H(21) C(21) H(23) 106.1(10) 1_555 1_555 1_555 no H(22) C(21) H(23) 108.5(9) 1_555 1_555 1_555 no O(4) C(22) H(24) 110.8(8) 1_555 1_555 1_555 no O(4) C(22) H(25) 109.7(7) 1_555 1_555 1_555 no O(4) C(22) H(26) 109.3(9) 1_555 1_555 1_555 no H(24) C(22) H(25) 110(1) 1_555 1_555 1_555 no H(24) C(22) H(26) 108.8(8) 1_555 1_555 1_555 no H(25) C(22) H(26) 107.5(9) 1_555 1_555 1_555 no Cl(1) C(23) P 113.3(4) 1_555 1_555 1_555 yes Cl(1) C(23) H(27) 108.9(6) 1_555 1_555 1_555 no Cl(1) C(23) H(28) 109.2(5) 1_555 1_555 1_555 no P C(23) H(27) 108.4(5) 1_555 1_555 1_555 no P C(23) H(28) 108.8(6) 1_555 1_555 1_555 no H(27) C(23) H(28) 108.1(7) 1_555 1_555 1_555 no S(1) C(24) H(29) 110.1(6) 1_555 1_555 1_555 no S(1) C(24) H(30) 111.7(7) 1_555 1_555 1_555 no S(1) C(24) H(31) 111.4(7) 1_555 1_555 1_555 no H(29) C(24) H(30) 107.3(9) 1_555 1_555 1_555 no H(29) C(24) H(31) 106.7(9) 1_555 1_555 1_555 no H(30) C(24) H(31) 109.4(8) 1_555 1_555 1_555 no S(1) C(25) H(32) 109.3(7) 1_555 1_555 1_555 no S(1) C(25) H(33) 109.8(7) 1_555 1_555 1_555 no S(1) C(25) H(34) 111.0(7) 1_555 1_555 1_555 no H(32) C(25) H(33) 107.4(8) 1_555 1_555 1_555 no H(32) C(25) H(34) 109.0(9) 1_555 1_555 1_555 no H(33) C(25) H(34) 110.2(9) 1_555 1_555 1_555 no S(2) C(26) H(35) 110.2(7) 1_555 1_555 1_555 no S(2) C(26) H(36) 112.7(6) 1_555 1_555 1_555 no S(2) C(26) H(37) 110.1(7) 1_555 1_555 1_555 no H(35) C(26) H(36) 109.1(9) 1_555 1_555 1_555 no H(35) C(26) H(37) 105.5(7) 1_555 1_555 1_555 no H(36) C(26) H(37) 109.0(9) 1_555 1_555 1_555 no S(2) C(27) H(44) 111.5(7) 1_555 1_555 1_555 no S(2) C(27) H(45) 107.7(6) 1_555 1_555 1_555 no S(2) C(27) H(46) 111.7(7) 1_555 1_555 1_555 no H(44) C(27) H(45) 106.2(8) 1_555 1_555 1_555 no H(44) C(27) H(46) 112.9(9) 1_555 1_555 1_555 no H(45) C(27) H(46) 106.5(9) 1_555 1_555 1_555 no S(3) C(28) H(38) 111.7(6) 1_555 1_555 1_555 no S(3) C(28) H(39) 112.7(7) 1_555 1_555 1_555 no S(3) C(28) H(40) 110.6(5) 1_555 1_555 1_555 no H(38) C(28) H(39) 108.8(7) 1_555 1_555 1_555 no H(38) C(28) H(40) 105.7(9) 1_555 1_555 1_555 no H(39) C(28) H(40) 107.1(7) 1_555 1_555 1_555 no S(3) C(29) H(41) 110.4(6) 1_555 1_555 1_555 no S(3) C(29) H(42) 110.4(6) 1_555 1_555 1_555 no S(3) C(29) H(43) 111.4(7) 1_555 1_555 1_555 no H(41) C(29) H(42) 107.3(9) 1_555 1_555 1_555 no H(41) C(29) H(43) 108.6(8) 1_555 1_555 1_555 no H(42) C(29) H(43) 108.7(8) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(11) 3.531(8) 1_555 2_656 ? Cl(4) C(23) 3.497(7) 1_555 1_455 ? O(1) C(21) 3.30(1) 1_555 2_645 ? O(2) O(6) 3.312(8) 1_555 2_646 ? O(5) C(2) 3.332(8) 1_555 1_555 ? O(6) C(22) 3.246(10) 1_555 2_656 ? O(6) C(14) 3.29(1) 1_555 2_656 ? O(6) C(23) 3.447(9) 1_555 2_656 ? O(7) C(10) 3.238(9) 1_555 1_565 ? C(3) C(14) 3.52(1) 1_555 2_656 ? C(13) C(21) 3.50(1) 1_555 2_645 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_4b #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 10 10:26:07 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source compound4b _chemical_name_common ? _chemical_formula_weight 1164.94 _chemical_formula_analytical ? _chemical_formula_sum 'C48 H59 Cl4 O10 P2 S2 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 14.253(3) _cell_length_b 16.592(3) _cell_length_c 12.623(3) _cell_angle_alpha 102.13(2) _cell_angle_beta 110.07(2) _cell_angle_gamma 102.09(2) _cell_volume 2609(1) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 13.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1202.00 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.863 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 2 1 -1 2 0 1 2 _diffrn_reflns_number 9584 _reflns_number_total 9176 _reflns_number_observed 4831 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 2.21 _diffrn_reflns_av_sigmaI/netI 0.071 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01431 _diffrn_orient_matrix_UB_12 0.00072 _diffrn_orient_matrix_UB_13 0.07235 _diffrn_orient_matrix_UB_21 -0.02876 _diffrn_orient_matrix_UB_22 -0.06463 _diffrn_orient_matrix_UB_23 -0.02910 _diffrn_orient_matrix_UB_31 0.07160 _diffrn_orient_matrix_UB_32 -0.00405 _diffrn_orient_matrix_UB_33 0.04211 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 96 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 118 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 20 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 2 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru1 0.28675(4) 0.25386(3) 1.12865(4) 0.0470(1) Uani d . 1.00 . Cl1 0.1994(1) 0.2805(1) 1.2664(1) 0.0713(5) Uani d . 1.00 . Cl2 -0.3526(2) 0.0855(1) 0.2517(2) 0.1439(10) Uani d . 1.00 . Cl3 -0.1099(2) 0.2464(2) -0.0450(3) 0.1372(10) Uani d . 1.00 . Cl4 0.0135(2) 0.4246(1) 0.0701(2) 0.1277(9) Uani d . 1.00 . S1 0.2796(2) 0.1234(1) 1.1563(2) 0.0815(6) Uani d . 1.00 . S2 0.4440(1) 0.32111(9) 1.2742(1) 0.0562(5) Uani d . 1.00 . P1 0.3314(1) 0.23458(9) 0.9722(1) 0.0469(4) Uani d . 1.00 . P2 -0.2187(1) 0.24772(10) 0.4436(1) 0.0544(5) Uani d . 1.00 . O1 0.2860(3) 0.1108(3) 0.7207(4) 0.073(1) Uani d . 1.00 . O2 0.1375(3) 0.1981(2) 0.9910(3) 0.061(1) Uani d . 1.00 . O3 0.3686(4) 0.2981(3) 0.7726(4) 0.082(1) Uani d . 1.00 . O4 0.2813(3) 0.3734(2) 1.1040(3) 0.057(1) Uani d . 1.00 . O5 0.3258(5) 0.0646(4) 1.1016(6) 0.158(3) Uani d . 1.00 . O6 0.5079(4) 0.2754(4) 1.3288(7) 0.173(3) Uani d . 1.00 . O7 -0.1568(4) 0.3575(3) 0.3240(4) 0.084(1) Uani d . 1.00 . O8 -0.2557(4) 0.3616(3) 0.6385(4) 0.085(1) Uani d . 1.00 . O9 -0.1382(4) 0.1638(3) 0.2670(4) 0.118(2) Uani d . 1.00 . O10 -0.0466(3) 0.3179(3) 0.6580(3) 0.068(1) Uani d . 1.00 . C1 0.2140(4) 0.1546(3) 0.8554(5) 0.046(2) Uani d . 1.00 . C2 0.1979(5) 0.1052(3) 0.7425(5) 0.052(2) Uani d . 1.00 . C3 0.0999(5) 0.0542(4) 0.6618(5) 0.061(2) Uani d . 1.00 . C4 0.0150(5) 0.0542(4) 0.6911(6) 0.064(2) Uani d . 1.00 . C5 0.0266(4) 0.1023(4) 0.7998(6) 0.064(2) Uani d . 1.00 . C6 0.1270(4) 0.1535(3) 0.8861(5) 0.052(2) Uani d . 1.00 . C7 0.2763(6) 0.0647(5) 0.6077(6) 0.096(3) Uani d . 1.00 . C8 0.3323(4) 0.3363(3) 0.9408(5) 0.047(2) Uani d . 1.00 . C9 0.3494(5) 0.3604(4) 0.8465(5) 0.059(2) Uani d . 1.00 . C10 0.3419(5) 0.4381(4) 0.8285(5) 0.066(2) Uani d . 1.00 . C11 0.3158(5) 0.4921(4) 0.9037(6) 0.067(2) Uani d . 1.00 . C12 0.2960(5) 0.4722(4) 0.9950(5) 0.063(2) Uani d . 1.00 . C13 0.3024(4) 0.3925(3) 1.0177(5) 0.052(2) Uani d . 1.00 . C14 0.4133(7) 0.3242(5) 0.6952(8) 0.123(3) Uani d . 1.00 . C15 0.4482(4) 0.2088(4) 0.9658(5) 0.050(2) Uani d . 1.00 . C16 0.5335(5) 0.2715(4) 0.9743(7) 0.085(2) Uani d . 1.00 . C17 0.6236(5) 0.2528(5) 0.9736(8) 0.098(3) Uani d . 1.00 . C18 0.6257(5) 0.1697(5) 0.9609(6) 0.077(2) Uani d . 1.00 . C19 0.5442(6) 0.1075(4) 0.9522(6) 0.079(2) Uani d . 1.00 . C20 0.4536(5) 0.1260(4) 0.9532(5) 0.060(2) Uani d . 1.00 . C21 0.1439(6) 0.0592(4) 1.1022(8) 0.115(3) Uani d . 1.00 . C22 0.3207(6) 0.1268(4) 1.3037(6) 0.094(2) Uani d . 1.00 . C23 0.5260(8) 0.3925(7) 1.2412(9) 0.254(4) Uani d . 1.00 . C24 0.4405(8) 0.3969(9) 1.389(1) 0.288(5) Uani d . 1.00 . C25 -0.2086(4) 0.3619(4) 0.4793(5) 0.053(2) Uani d . 1.00 . C26 -0.1754(5) 0.4063(4) 0.4099(5) 0.059(2) Uani d . 1.00 . C27 -0.1630(5) 0.4935(4) 0.4316(6) 0.076(2) Uani d . 1.00 . C28 -0.1858(6) 0.5359(4) 0.5222(6) 0.078(2) Uani d . 1.00 . C29 -0.2177(5) 0.4948(4) 0.5919(6) 0.071(2) Uani d . 1.00 . C30 -0.2275(5) 0.4071(4) 0.5721(5) 0.059(2) Uani d . 1.00 . C31 -0.1031(6) 0.3961(6) 0.2647(7) 0.106(3) Uani d . 1.00 . C32 -0.2827(7) 0.3999(5) 0.7298(7) 0.120(3) Uani d . 1.00 . C33 -0.0913(5) 0.2375(4) 0.4662(5) 0.054(2) Uani d . 1.00 . C34 -0.0635(5) 0.1960(4) 0.3780(6) 0.073(2) Uani d . 1.00 . C35 0.0376(6) 0.1923(5) 0.4065(7) 0.097(3) Uani d . 1.00 . C36 0.1093(6) 0.2283(5) 0.5205(9) 0.103(3) Uani d . 1.00 . C37 0.0868(5) 0.2701(4) 0.6091(7) 0.081(2) Uani d . 1.00 . C38 -0.0147(5) 0.2755(4) 0.5802(5) 0.060(2) Uani d . 1.00 . C39 -0.1197(7) 0.1113(5) 0.1757(6) 0.125(3) Uani d . 1.00 . C40 0.0210(7) 0.3528(5) 0.7782(7) 0.106(3) Uani d . 1.00 . C41 -0.2741(5) 0.1908(3) 0.5245(5) 0.056(2) Uani d . 1.00 . C42 -0.2193(5) 0.1502(4) 0.5976(6) 0.067(2) Uani d . 1.00 . C43 -0.2651(6) 0.1033(5) 0.6529(7) 0.092(3) Uani d . 1.00 . C44 -0.3662(7) 0.0953(5) 0.6380(7) 0.106(3) Uani d . 1.00 . C45 -0.4231(6) 0.1356(5) 0.5628(8) 0.106(3) Uani d . 1.00 . C46 -0.3765(6) 0.1822(5) 0.5078(7) 0.088(2) Uani d . 1.00 . C47 -0.3139(5) 0.1982(4) 0.2909(5) 0.074(2) Uani d . 1.00 . C48 0.0132(6) 0.3191(5) 0.0516(6) 0.093(3) Uani d . 1.00 . H1 0.0899 0.0189 0.5863 0.0730 Uiso calc . 1.00 . H2 -0.0532 0.0197 0.6343 0.0750 Uiso calc . 1.00 . H3 -0.0339 0.1008 0.8164 0.0760 Uiso calc . 1.00 . H4 0.2444 0.0047 0.5915 0.1141 Uiso calc . 1.00 . H5 0.2347 0.0850 0.5492 0.1141 Uiso calc . 1.00 . H6 0.3443 0.0736 0.6067 0.1141 Uiso calc . 1.00 . H7 0.3546 0.4542 0.7655 0.0783 Uiso calc . 1.00 . H8 0.3111 0.5461 0.8927 0.0791 Uiso calc . 1.00 . H9 0.2775 0.5120 1.0439 0.0740 Uiso calc . 1.00 . H10 0.4238 0.2761 0.6499 0.1454 Uiso calc . 1.00 . H11 0.3676 0.3466 0.6430 0.1454 Uiso calc . 1.00 . H12 0.4793 0.3683 0.7403 0.1454 Uiso calc . 1.00 . H13 0.5304 0.3282 0.9794 0.1033 Uiso calc . 1.00 . H14 0.6823 0.2965 0.9811 0.1174 Uiso calc . 1.00 . H15 0.6869 0.1560 0.9592 0.0925 Uiso calc . 1.00 . H16 0.5485 0.0504 0.9447 0.0936 Uiso calc . 1.00 . H17 0.3961 0.0813 0.9458 0.0736 Uiso calc . 1.00 . H18 0.1129 0.0433 1.0185 0.1385 Uiso calc . 1.00 . H19 0.1075 0.0918 1.1344 0.1385 Uiso calc . 1.00 . H20 0.1407 0.0083 1.1264 0.1385 Uiso calc . 1.00 . H21 0.3948 0.1494 1.3410 0.1129 Uiso calc . 1.00 . H22 0.2904 0.1628 1.3413 0.1129 Uiso calc . 1.00 . H23 0.2988 0.0699 1.3078 0.1129 Uiso calc . 1.00 . H24 0.5101 0.4222 1.4507 0.3472 Uiso calc . 1.00 . H25 0.4167 0.4404 1.3619 0.3472 Uiso calc . 1.00 . H26 0.3958 0.3691 1.4204 0.3472 Uiso calc . 1.00 . H27 0.5803 0.4316 1.3122 0.2950 Uiso calc . 1.00 . H28 0.4865 0.4242 1.1984 0.2950 Uiso calc . 1.00 . H29 0.5536 0.3621 1.1939 0.2950 Uiso calc . 1.00 . H30 -0.1406 0.5245 0.3847 0.0914 Uiso calc . 1.00 . H31 -0.1788 0.5957 0.5365 0.0921 Uiso calc . 1.00 . H32 -0.2337 0.5253 0.6529 0.0839 Uiso calc . 1.00 . H33 -0.1427 0.4280 0.2240 0.1264 Uiso calc . 1.00 . H34 -0.0365 0.4333 0.3200 0.1264 Uiso calc . 1.00 . H35 -0.0959 0.3521 0.2091 0.1264 Uiso calc . 1.00 . H36 -0.3438 0.4166 0.6965 0.1418 Uiso calc . 1.00 . H37 -0.2267 0.4497 0.7843 0.1418 Uiso calc . 1.00 . H38 -0.2969 0.3595 0.7698 0.1418 Uiso calc . 1.00 . H39 0.0563 0.1645 0.3462 0.1143 Uiso calc . 1.00 . H40 0.1777 0.2232 0.5368 0.1239 Uiso calc . 1.00 . H41 0.1398 0.2951 0.6874 0.0981 Uiso calc . 1.00 . H42 -0.0621 0.1448 0.1660 0.1479 Uiso calc . 1.00 . H43 -0.1804 0.0925 0.1042 0.1479 Uiso calc . 1.00 . H44 -0.1037 0.0630 0.1977 0.1479 Uiso calc . 1.00 . H45 -0.0142 0.3800 0.8206 0.1283 Uiso calc . 1.00 . H46 0.0380 0.3073 0.8084 0.1283 Uiso calc . 1.00 . H47 0.0821 0.3937 0.7878 0.1283 Uiso calc . 1.00 . H48 -0.1485 0.1551 0.6090 0.0802 Uiso calc . 1.00 . H49 -0.2266 0.0755 0.7020 0.1130 Uiso calc . 1.00 . H50 -0.3988 0.0629 0.6769 0.1265 Uiso calc . 1.00 . H51 -0.4938 0.1305 0.5506 0.1263 Uiso calc . 1.00 . H52 -0.4154 0.2092 0.4569 0.1040 Uiso calc . 1.00 . H53 0.3021 0.0082 1.1072 0.1904 Uiso calc . 1.00 . H54 0.3059 0.0609 1.0199 0.1904 Uiso calc . 1.00 . H55 0.4005 0.0856 1.1407 0.1904 Uiso calc . 1.00 . H56 -0.2828 0.2172 0.2367 0.0768 Uiso calc . 1.00 . H57 -0.3741 0.2196 0.2764 0.0768 Uiso calc . 1.00 . H58 0.0345 0.3083 0.1274 0.1100 Uiso calc . 1.00 . H59 0.0652 0.3090 0.0210 0.1100 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0402(3) 0.0394(2) 0.0561(3) 0.0134(2) 0.0153(2) 0.0106(2) Cl(1) 0.078(1) 0.0766(10) 0.0728(10) 0.0306(8) 0.0427(8) 0.0220(8) Cl(2) 0.186(3) 0.082(1) 0.106(2) 0.034(2) 0.014(2) 0.000(1) Cl(3) 0.092(2) 0.145(2) 0.167(2) 0.032(1) 0.056(2) 0.033(2) Cl(4) 0.192(2) 0.107(1) 0.126(2) 0.071(1) 0.090(1) 0.049(1) S(1) 0.074(1) 0.0527(9) 0.135(1) 0.0274(8) 0.050(1) 0.0417(9) S(2) 0.0492(10) 0.0524(8) 0.0560(9) 0.0161(7) 0.0101(8) 0.0141(7) P(1) 0.0348(9) 0.0401(8) 0.0569(9) 0.0102(7) 0.0140(7) 0.0071(7) P(2) 0.059(1) 0.0555(9) 0.0489(9) 0.0294(7) 0.0178(8) 0.0123(7) O(1) 0.061(3) 0.084(3) 0.063(3) 0.016(2) 0.028(2) 0.004(2) O(2) 0.036(2) 0.063(2) 0.066(2) 0.013(2) 0.017(2) -0.003(2) O(3) 0.100(3) 0.082(3) 0.092(3) 0.032(2) 0.066(2) 0.035(2) O(4) 0.074(3) 0.047(2) 0.062(2) 0.030(2) 0.034(2) 0.021(2) O(5) 0.207(6) 0.103(4) 0.237(6) 0.075(4) 0.142(4) 0.083(4) O(6) 0.075(4) 0.103(4) 0.255(7) 0.028(3) -0.032(5) 0.055(4) O(7) 0.119(4) 0.090(3) 0.071(3) 0.044(3) 0.061(2) 0.031(2) O(8) 0.118(3) 0.081(3) 0.079(3) 0.042(2) 0.066(2) 0.020(2) O(9) 0.155(4) 0.154(4) 0.073(3) 0.109(3) 0.052(3) 0.019(3) O(10) 0.058(3) 0.079(3) 0.045(2) 0.016(2) 0.005(2) 0.008(2) C(1) 0.034(3) 0.038(3) 0.056(3) 0.008(2) 0.012(3) 0.008(2) C(2) 0.052(4) 0.045(3) 0.056(3) 0.016(3) 0.020(3) 0.011(3) C(3) 0.058(4) 0.054(4) 0.048(4) 0.005(3) 0.008(3) 0.004(3) C(4) 0.043(4) 0.050(3) 0.066(4) 0.002(3) 0.002(3) 0.001(3) C(5) 0.029(3) 0.065(4) 0.079(4) 0.008(3) 0.010(3) 0.012(3) C(6) 0.034(3) 0.041(3) 0.067(4) 0.010(3) 0.011(3) 0.008(3) C(7) 0.086(5) 0.123(6) 0.083(5) 0.042(4) 0.044(4) 0.013(4) C(8) 0.032(3) 0.040(3) 0.055(3) 0.007(2) 0.011(3) 0.005(3) C(9) 0.044(4) 0.059(4) 0.065(4) 0.005(3) 0.024(3) 0.014(3) C(10) 0.064(4) 0.054(3) 0.079(4) 0.005(3) 0.030(3) 0.030(3) C(11) 0.062(5) 0.048(3) 0.078(4) 0.008(3) 0.016(4) 0.025(3) C(12) 0.065(4) 0.046(3) 0.061(4) 0.018(3) 0.013(3) 0.007(3) C(13) 0.040(4) 0.036(3) 0.061(4) 0.009(3) 0.005(3) 0.011(3) C(14) 0.162(7) 0.111(6) 0.144(6) 0.039(5) 0.118(5) 0.044(5) C(15) 0.035(3) 0.057(3) 0.053(3) 0.015(3) 0.016(3) 0.010(3) C(16) 0.044(4) 0.058(4) 0.134(6) 0.009(3) 0.028(4) 0.015(4) C(17) 0.039(4) 0.091(5) 0.147(7) 0.012(4) 0.032(4) 0.024(5) C(18) 0.046(4) 0.109(5) 0.089(5) 0.039(4) 0.034(3) 0.029(4) C(19) 0.073(5) 0.076(4) 0.101(5) 0.043(3) 0.039(4) 0.031(4) C(20) 0.048(4) 0.058(3) 0.078(4) 0.021(3) 0.027(3) 0.019(3) C(21) 0.089(6) 0.061(4) 0.164(7) -0.017(4) 0.038(5) 0.038(4) C(22) 0.117(6) 0.078(4) 0.093(5) 0.031(4) 0.029(4) 0.057(3) C(23) 0.152(9) 0.260(9) 0.153(7) -0.161(7) -0.080(6) 0.138(6) C(24) 0.085(8) 0.35(1) 0.211(10) 0.027(8) 0.003(7) -0.214(8) C(25) 0.045(3) 0.064(3) 0.049(3) 0.027(3) 0.016(3) 0.014(3) C(26) 0.063(4) 0.066(4) 0.049(3) 0.025(3) 0.021(3) 0.016(3) C(27) 0.075(5) 0.063(4) 0.088(5) 0.021(3) 0.024(4) 0.034(3) C(28) 0.076(5) 0.051(4) 0.086(5) 0.022(3) 0.017(4) 0.007(3) C(29) 0.075(5) 0.059(4) 0.071(4) 0.028(3) 0.028(3) 0.000(3) C(30) 0.059(4) 0.064(4) 0.054(3) 0.021(3) 0.023(3) 0.015(3) C(31) 0.103(6) 0.146(6) 0.102(5) 0.053(5) 0.062(4) 0.055(4) C(32) 0.161(7) 0.114(6) 0.114(5) 0.041(5) 0.103(4) 0.015(5) C(33) 0.060(4) 0.063(3) 0.050(3) 0.030(3) 0.027(3) 0.018(3) C(34) 0.090(5) 0.082(4) 0.087(4) 0.053(3) 0.058(3) 0.037(3) C(35) 0.122(5) 0.096(5) 0.143(5) 0.069(4) 0.100(4) 0.063(4) C(36) 0.072(5) 0.092(5) 0.182(7) 0.045(4) 0.074(4) 0.058(5) C(37) 0.046(4) 0.075(4) 0.114(5) 0.015(3) 0.023(4) 0.036(4) C(38) 0.062(4) 0.051(3) 0.074(4) 0.020(3) 0.032(3) 0.026(3) C(39) 0.217(7) 0.137(5) 0.086(5) 0.124(5) 0.091(4) 0.044(4) C(40) 0.106(7) 0.102(6) 0.083(5) 0.012(5) 0.022(5) 0.021(4) C(41) 0.053(4) 0.049(3) 0.062(4) 0.024(3) 0.017(3) 0.011(3) C(42) 0.055(4) 0.053(3) 0.074(4) 0.008(3) 0.011(3) 0.019(3) C(43) 0.078(6) 0.084(5) 0.096(5) 0.009(4) 0.013(4) 0.045(4) C(44) 0.108(7) 0.096(5) 0.113(6) 0.010(5) 0.049(5) 0.044(4) C(45) 0.061(5) 0.109(6) 0.162(7) 0.028(4) 0.056(5) 0.053(5) C(46) 0.064(5) 0.102(5) 0.112(5) 0.033(4) 0.037(4) 0.051(4) C(47) 0.086(5) 0.065(4) 0.058(4) 0.041(3) 0.010(3) 0.009(3) C(48) 0.089(5) 0.129(6) 0.088(5) 0.063(4) 0.043(4) 0.042(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4831 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0509 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0645 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.879 _refine_ls_shift/esd_max 0.2550 _refine_ls_shift/esd_mean 0.0340 _refine_diff_density_min -0.35 _refine_diff_density_max 0.51 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.482(2) 1_555 1_555 yes Ru(1) S(1) 2.250(2) 1_555 1_555 yes Ru(1) S(2) 2.216(2) 1_555 1_555 yes Ru(1) P(1) 2.257(2) 1_555 1_555 yes Ru(1) O(2) 2.089(4) 1_555 1_555 yes Ru(1) O(4) 2.084(4) 1_555 1_555 yes Cl(2) C(47) 1.744(6) 1_555 1_555 yes Cl(3) C(48) 1.745(7) 1_555 1_555 yes Cl(4) C(48) 1.716(8) 1_555 1_555 yes S(1) O(5) 1.470(7) 1_555 1_555 yes S(1) C(21) 1.808(8) 1_555 1_555 yes S(1) C(22) 1.733(7) 1_555 1_555 yes S(2) O(6) 1.398(6) 1_555 1_555 yes S(2) C(23) 1.704(10) 1_555 1_555 yes S(2) C(24) 1.73(1) 1_555 1_555 yes P(1) C(1) 1.813(5) 1_555 1_555 yes P(1) C(8) 1.812(6) 1_555 1_555 yes P(1) C(15) 1.826(6) 1_555 1_555 yes P(2) C(25) 1.816(6) 1_555 1_555 yes P(2) C(33) 1.790(6) 1_555 1_555 yes P(2) C(41) 1.791(7) 1_555 1_555 yes P(2) C(47) 1.818(6) 1_555 1_555 yes O(1) C(2) 1.364(7) 1_555 1_555 yes O(1) C(7) 1.414(8) 1_555 1_555 yes O(2) C(6) 1.315(7) 1_555 1_555 yes O(3) C(9) 1.379(8) 1_555 1_555 yes O(3) C(14) 1.428(9) 1_555 1_555 yes O(4) C(13) 1.308(7) 1_555 1_555 yes O(7) C(26) 1.349(7) 1_555 1_555 yes O(7) C(31) 1.395(9) 1_555 1_555 yes O(8) C(30) 1.343(7) 1_555 1_555 yes O(8) C(32) 1.407(9) 1_555 1_555 yes O(9) C(34) 1.343(7) 1_555 1_555 yes O(9) C(39) 1.429(9) 1_555 1_555 yes O(10) C(38) 1.347(8) 1_555 1_555 yes O(10) C(40) 1.400(8) 1_555 1_555 yes C(1) C(2) 1.401(8) 1_555 1_555 yes C(1) C(6) 1.419(8) 1_555 1_555 yes C(2) C(3) 1.367(7) 1_555 1_555 yes C(3) C(4) 1.380(9) 1_555 1_555 yes C(4) C(5) 1.370(9) 1_555 1_555 yes C(5) C(6) 1.410(7) 1_555 1_555 yes C(8) C(9) 1.411(8) 1_555 1_555 yes C(8) C(13) 1.435(8) 1_555 1_555 yes C(9) C(10) 1.375(8) 1_555 1_555 yes C(10) C(11) 1.365(9) 1_555 1_555 yes C(11) C(12) 1.365(9) 1_555 1_555 yes C(12) C(13) 1.426(8) 1_555 1_555 yes C(15) C(16) 1.380(8) 1_555 1_555 yes C(15) C(20) 1.370(8) 1_555 1_555 yes C(16) C(17) 1.385(10) 1_555 1_555 yes C(17) C(18) 1.363(10) 1_555 1_555 yes C(18) C(19) 1.338(9) 1_555 1_555 yes C(19) C(20) 1.393(9) 1_555 1_555 yes C(25) C(26) 1.393(9) 1_555 1_555 yes C(25) C(30) 1.393(8) 1_555 1_555 yes C(26) C(27) 1.377(8) 1_555 1_555 yes C(27) C(28) 1.39(1) 1_555 1_555 yes C(28) C(29) 1.357(10) 1_555 1_555 yes C(29) C(30) 1.391(8) 1_555 1_555 yes C(33) C(34) 1.402(9) 1_555 1_555 yes C(33) C(38) 1.383(7) 1_555 1_555 yes C(34) C(35) 1.378(10) 1_555 1_555 yes C(35) C(36) 1.36(1) 1_555 1_555 yes C(36) C(37) 1.36(1) 1_555 1_555 yes C(37) C(38) 1.392(9) 1_555 1_555 yes C(41) C(42) 1.378(8) 1_555 1_555 yes C(41) C(46) 1.373(9) 1_555 1_555 yes C(42) C(43) 1.36(1) 1_555 1_555 yes C(43) C(44) 1.36(1) 1_555 1_555 yes C(44) C(45) 1.40(1) 1_555 1_555 yes C(45) C(46) 1.36(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru(1) S(1) 88.06(7) 1_555 1_555 1_555 yes Cl(1) Ru(1) S(2) 91.55(6) 1_555 1_555 1_555 yes Cl(1) Ru(1) P(1) 165.96(6) 1_555 1_555 1_555 yes Cl(1) Ru(1) O(2) 87.8(1) 1_555 1_555 1_555 yes Cl(1) Ru(1) O(4) 88.0(1) 1_555 1_555 1_555 yes S(1) Ru(1) S(2) 94.75(6) 1_555 1_555 1_555 yes S(1) Ru(1) P(1) 99.06(7) 1_555 1_555 1_555 yes S(1) Ru(1) O(2) 88.8(1) 1_555 1_555 1_555 yes S(1) Ru(1) O(4) 175.2(1) 1_555 1_555 1_555 yes S(2) Ru(1) P(1) 99.84(6) 1_555 1_555 1_555 yes S(2) Ru(1) O(2) 176.4(1) 1_555 1_555 1_555 yes S(2) Ru(1) O(4) 88.2(1) 1_555 1_555 1_555 yes P(1) Ru(1) O(2) 80.3(1) 1_555 1_555 1_555 yes P(1) Ru(1) O(4) 84.2(1) 1_555 1_555 1_555 yes O(2) Ru(1) O(4) 88.3(1) 1_555 1_555 1_555 yes Ru(1) S(1) O(5) 121.7(3) 1_555 1_555 1_555 yes Ru(1) S(1) C(21) 109.3(3) 1_555 1_555 1_555 yes Ru(1) S(1) C(22) 113.8(2) 1_555 1_555 1_555 yes O(5) S(1) C(21) 103.2(4) 1_555 1_555 1_555 yes O(5) S(1) C(22) 106.7(4) 1_555 1_555 1_555 yes C(21) S(1) C(22) 99.5(4) 1_555 1_555 1_555 yes Ru(1) S(2) O(6) 121.8(2) 1_555 1_555 1_555 yes Ru(1) S(2) C(23) 114.6(3) 1_555 1_555 1_555 yes Ru(1) S(2) C(24) 112.5(4) 1_555 1_555 1_555 yes O(6) S(2) C(23) 103.2(5) 1_555 1_555 1_555 yes O(6) S(2) C(24) 105.4(6) 1_555 1_555 1_555 yes C(23) S(2) C(24) 96.0(7) 1_555 1_555 1_555 yes Ru(1) P(1) C(1) 102.3(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(8) 101.2(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(15) 127.1(2) 1_555 1_555 1_555 yes C(1) P(1) C(8) 105.7(2) 1_555 1_555 1_555 yes C(1) P(1) C(15) 110.3(3) 1_555 1_555 1_555 yes C(8) P(1) C(15) 108.3(3) 1_555 1_555 1_555 yes C(25) P(2) C(33) 108.7(3) 1_555 1_555 1_555 yes C(25) P(2) C(41) 114.5(3) 1_555 1_555 1_555 yes C(25) P(2) C(47) 105.9(3) 1_555 1_555 1_555 yes C(33) P(2) C(41) 110.4(3) 1_555 1_555 1_555 yes C(33) P(2) C(47) 113.5(3) 1_555 1_555 1_555 yes C(41) P(2) C(47) 103.9(3) 1_555 1_555 1_555 yes C(2) O(1) C(7) 119.0(5) 1_555 1_555 1_555 yes Ru(1) O(2) C(6) 119.7(4) 1_555 1_555 1_555 yes C(9) O(3) C(14) 117.8(5) 1_555 1_555 1_555 yes Ru(1) O(4) C(13) 118.5(3) 1_555 1_555 1_555 yes S(1) O(5) H(53) 110.3(6) 1_555 1_555 1_555 no S(1) O(5) H(54) 110.0(5) 1_555 1_555 1_555 no S(1) O(5) H(55) 110.1(5) 1_555 1_555 1_555 no H(53) O(5) H(54) 108.9(6) 1_555 1_555 1_555 no H(53) O(5) H(55) 108.9(6) 1_555 1_555 1_555 no H(54) O(5) H(55) 108.7(7) 1_555 1_555 1_555 no C(26) O(7) C(31) 120.7(6) 1_555 1_555 1_555 yes C(30) O(8) C(32) 121.0(6) 1_555 1_555 1_555 yes C(34) O(9) C(39) 119.8(6) 1_555 1_555 1_555 yes C(38) O(10) C(40) 120.0(6) 1_555 1_555 1_555 yes P(1) C(1) C(2) 130.1(5) 1_555 1_555 1_555 yes P(1) C(1) C(6) 109.9(4) 1_555 1_555 1_555 yes C(2) C(1) C(6) 119.6(5) 1_555 1_555 1_555 yes O(1) C(2) C(1) 115.4(5) 1_555 1_555 1_555 yes O(1) C(2) C(3) 123.4(6) 1_555 1_555 1_555 yes C(1) C(2) C(3) 121.2(6) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.1(6) 1_555 1_555 1_555 yes C(2) C(3) H(1) 120.8(7) 1_555 1_555 1_555 no C(4) C(3) H(1) 120.0(6) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.8(5) 1_555 1_555 1_555 yes C(3) C(4) H(2) 119.0(6) 1_555 1_555 1_555 no C(5) C(4) H(2) 119.2(7) 1_555 1_555 1_555 no C(4) C(5) C(6) 120.4(6) 1_555 1_555 1_555 yes C(4) C(5) H(3) 119.3(6) 1_555 1_555 1_555 no C(6) C(5) H(3) 120.3(6) 1_555 1_555 1_555 no O(2) C(6) C(1) 122.2(5) 1_555 1_555 1_555 yes O(2) C(6) C(5) 120.0(6) 1_555 1_555 1_555 yes C(1) C(6) C(5) 117.8(5) 1_555 1_555 1_555 yes O(1) C(7) H(4) 109.6(7) 1_555 1_555 1_555 no O(1) C(7) H(5) 109.6(7) 1_555 1_555 1_555 no O(1) C(7) H(6) 109.3(6) 1_555 1_555 1_555 no H(4) C(7) H(5) 109.7(7) 1_555 1_555 1_555 no H(4) C(7) H(6) 109.2(8) 1_555 1_555 1_555 no H(5) C(7) H(6) 109.4(8) 1_555 1_555 1_555 no P(1) C(8) C(9) 127.4(5) 1_555 1_555 1_555 yes P(1) C(8) C(13) 112.6(5) 1_555 1_555 1_555 yes C(9) C(8) C(13) 119.7(5) 1_555 1_555 1_555 yes O(3) C(9) C(8) 114.4(5) 1_555 1_555 1_555 yes O(3) C(9) C(10) 123.9(6) 1_555 1_555 1_555 yes C(8) C(9) C(10) 121.7(6) 1_555 1_555 1_555 yes C(9) C(10) C(11) 118.3(6) 1_555 1_555 1_555 yes C(9) C(10) H(7) 121.1(7) 1_555 1_555 1_555 no C(11) C(10) H(7) 120.5(6) 1_555 1_555 1_555 no C(10) C(11) C(12) 123.1(6) 1_555 1_555 1_555 yes C(10) C(11) H(8) 119.1(7) 1_555 1_555 1_555 no C(12) C(11) H(8) 117.8(7) 1_555 1_555 1_555 no C(11) C(12) C(13) 121.0(6) 1_555 1_555 1_555 yes C(11) C(12) H(9) 119.4(6) 1_555 1_555 1_555 no C(13) C(12) H(9) 119.6(7) 1_555 1_555 1_555 no O(4) C(13) C(8) 123.4(5) 1_555 1_555 1_555 yes O(4) C(13) C(12) 120.4(6) 1_555 1_555 1_555 yes C(8) C(13) C(12) 116.2(6) 1_555 1_555 1_555 yes O(3) C(14) H(10) 110.0(7) 1_555 1_555 1_555 no O(3) C(14) H(11) 109.9(8) 1_555 1_555 1_555 no O(3) C(14) H(12) 110.0(7) 1_555 1_555 1_555 no H(10) C(14) H(11) 109.2(8) 1_555 1_555 1_555 no H(10) C(14) H(12) 108.9(9) 1_555 1_555 1_555 no H(11) C(14) H(12) 108.8(8) 1_555 1_555 1_555 no P(1) C(15) C(16) 121.5(5) 1_555 1_555 1_555 yes P(1) C(15) C(20) 120.5(5) 1_555 1_555 1_555 yes C(16) C(15) C(20) 118.0(6) 1_555 1_555 1_555 yes C(15) C(16) C(17) 121.6(7) 1_555 1_555 1_555 yes C(15) C(16) H(13) 119.6(7) 1_555 1_555 1_555 no C(17) C(16) H(13) 118.7(7) 1_555 1_555 1_555 no C(16) C(17) C(18) 118.4(7) 1_555 1_555 1_555 yes C(16) C(17) H(14) 121.1(8) 1_555 1_555 1_555 no C(18) C(17) H(14) 120.4(8) 1_555 1_555 1_555 no C(17) C(18) C(19) 121.3(7) 1_555 1_555 1_555 yes C(17) C(18) H(15) 119.1(7) 1_555 1_555 1_555 no C(19) C(18) H(15) 119.6(8) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.4(6) 1_555 1_555 1_555 yes C(18) C(19) H(16) 119.4(8) 1_555 1_555 1_555 no C(20) C(19) H(16) 120.2(7) 1_555 1_555 1_555 no C(15) C(20) C(19) 120.2(6) 1_555 1_555 1_555 yes C(15) C(20) H(17) 120.3(6) 1_555 1_555 1_555 no C(19) C(20) H(17) 119.6(6) 1_555 1_555 1_555 no S(1) C(21) H(18) 109.5(7) 1_555 1_555 1_555 no S(1) C(21) H(19) 109.4(5) 1_555 1_555 1_555 no S(1) C(21) H(20) 109.2(7) 1_555 1_555 1_555 no H(18) C(21) H(19) 110.0(9) 1_555 1_555 1_555 no H(18) C(21) H(20) 109.5(7) 1_555 1_555 1_555 no H(19) C(21) H(20) 109.3(9) 1_555 1_555 1_555 no S(1) C(22) H(21) 109.2(7) 1_555 1_555 1_555 no S(1) C(22) H(22) 109.1(5) 1_555 1_555 1_555 no S(1) C(22) H(23) 109.1(5) 1_555 1_555 1_555 no H(21) C(22) H(22) 110.0(7) 1_555 1_555 1_555 no H(21) C(22) H(23) 109.8(7) 1_555 1_555 1_555 no H(22) C(22) H(23) 109.7(8) 1_555 1_555 1_555 no S(2) C(23) H(27) 109.4(8) 1_555 1_555 1_555 no S(2) C(23) H(28) 108.5(9) 1_555 1_555 1_555 no S(2) C(23) H(29) 109.7(8) 1_555 1_555 1_555 no H(27) C(23) H(28) 109(1) 1_555 1_555 1_555 no H(27) C(23) H(29) 110(1) 1_555 1_555 1_555 no H(28) C(23) H(29) 109(1) 1_555 1_555 1_555 no S(2) C(24) H(24) 108.8(9) 1_555 1_555 1_555 no S(2) C(24) H(25) 110(1) 1_555 1_555 1_555 no S(2) C(24) H(26) 109.4(10) 1_555 1_555 1_555 no H(24) C(24) H(25) 109(1) 1_555 1_555 1_555 no H(24) C(24) H(26) 108(1) 1_555 1_555 1_555 no H(25) C(24) H(26) 110(1) 1_555 1_555 1_555 no P(2) C(25) C(26) 115.9(5) 1_555 1_555 1_555 yes P(2) C(25) C(30) 124.8(5) 1_555 1_555 1_555 yes C(26) C(25) C(30) 119.2(6) 1_555 1_555 1_555 yes O(7) C(26) C(25) 114.9(5) 1_555 1_555 1_555 yes O(7) C(26) C(27) 124.6(6) 1_555 1_555 1_555 yes C(25) C(26) C(27) 120.4(6) 1_555 1_555 1_555 yes C(26) C(27) C(28) 118.8(7) 1_555 1_555 1_555 yes C(26) C(27) H(30) 121.2(7) 1_555 1_555 1_555 no C(28) C(27) H(30) 119.9(7) 1_555 1_555 1_555 no C(27) C(28) C(29) 122.3(6) 1_555 1_555 1_555 yes C(27) C(28) H(31) 119.3(8) 1_555 1_555 1_555 no C(29) C(28) H(31) 118.4(8) 1_555 1_555 1_555 no C(28) C(29) C(30) 118.9(6) 1_555 1_555 1_555 yes C(28) C(29) H(32) 120.6(7) 1_555 1_555 1_555 no C(30) C(29) H(32) 120.5(7) 1_555 1_555 1_555 no O(8) C(30) C(25) 116.6(5) 1_555 1_555 1_555 yes O(8) C(30) C(29) 123.2(6) 1_555 1_555 1_555 yes C(25) C(30) C(29) 120.3(6) 1_555 1_555 1_555 yes O(7) C(31) H(33) 108.6(8) 1_555 1_555 1_555 no O(7) C(31) H(34) 109.5(7) 1_555 1_555 1_555 no O(7) C(31) H(35) 109.0(8) 1_555 1_555 1_555 no H(33) C(31) H(34) 110.1(9) 1_555 1_555 1_555 no H(33) C(31) H(35) 109.4(8) 1_555 1_555 1_555 no H(34) C(31) H(35) 110.3(9) 1_555 1_555 1_555 no O(8) C(32) H(36) 109.3(7) 1_555 1_555 1_555 no O(8) C(32) H(37) 109.9(8) 1_555 1_555 1_555 no O(8) C(32) H(38) 109.6(8) 1_555 1_555 1_555 no H(36) C(32) H(37) 109.2(9) 1_555 1_555 1_555 no H(36) C(32) H(38) 109.3(9) 1_555 1_555 1_555 no H(37) C(32) H(38) 109.5(8) 1_555 1_555 1_555 no P(2) C(33) C(34) 125.3(4) 1_555 1_555 1_555 yes P(2) C(33) C(38) 116.3(5) 1_555 1_555 1_555 yes C(34) C(33) C(38) 118.4(6) 1_555 1_555 1_555 yes O(9) C(34) C(33) 117.0(6) 1_555 1_555 1_555 yes O(9) C(34) C(35) 123.1(7) 1_555 1_555 1_555 yes C(33) C(34) C(35) 119.9(6) 1_555 1_555 1_555 yes C(34) C(35) C(36) 119.5(8) 1_555 1_555 1_555 yes C(34) C(35) H(39) 119.7(8) 1_555 1_555 1_555 no C(36) C(35) H(39) 120.8(9) 1_555 1_555 1_555 no C(35) C(36) C(37) 122.9(8) 1_555 1_555 1_555 yes C(35) C(36) H(40) 116.9(9) 1_555 1_555 1_555 no C(37) C(36) H(40) 120.2(9) 1_555 1_555 1_555 no C(36) C(37) C(38) 117.8(7) 1_555 1_555 1_555 yes C(36) C(37) H(41) 120.0(8) 1_555 1_555 1_555 no C(38) C(37) H(41) 122.3(8) 1_555 1_555 1_555 no O(10) C(38) C(33) 114.5(6) 1_555 1_555 1_555 yes O(10) C(38) C(37) 124.0(6) 1_555 1_555 1_555 yes C(33) C(38) C(37) 121.4(7) 1_555 1_555 1_555 yes O(9) C(39) H(42) 108.9(7) 1_555 1_555 1_555 no O(9) C(39) H(43) 109.0(8) 1_555 1_555 1_555 no O(9) C(39) H(44) 109.2(7) 1_555 1_555 1_555 no H(42) C(39) H(43) 109.8(8) 1_555 1_555 1_555 no H(42) C(39) H(44) 109.7(9) 1_555 1_555 1_555 no H(43) C(39) H(44) 110.2(8) 1_555 1_555 1_555 no O(10) C(40) H(45) 108.9(7) 1_555 1_555 1_555 no O(10) C(40) H(46) 109.2(6) 1_555 1_555 1_555 no O(10) C(40) H(47) 110.0(7) 1_555 1_555 1_555 no H(45) C(40) H(46) 108.6(9) 1_555 1_555 1_555 no H(45) C(40) H(47) 109.8(8) 1_555 1_555 1_555 no H(46) C(40) H(47) 110.3(9) 1_555 1_555 1_555 no P(2) C(41) C(42) 122.0(5) 1_555 1_555 1_555 yes P(2) C(41) C(46) 119.2(5) 1_555 1_555 1_555 yes C(42) C(41) C(46) 118.6(7) 1_555 1_555 1_555 yes C(41) C(42) C(43) 120.8(7) 1_555 1_555 1_555 yes C(41) C(42) H(48) 119.3(7) 1_555 1_555 1_555 no C(43) C(42) H(48) 119.8(7) 1_555 1_555 1_555 no C(42) C(43) C(44) 121.0(7) 1_555 1_555 1_555 yes C(42) C(43) H(49) 119.6(9) 1_555 1_555 1_555 no C(44) C(43) H(49) 119.4(9) 1_555 1_555 1_555 no C(43) C(44) C(45) 118.6(8) 1_555 1_555 1_555 yes C(43) C(44) H(50) 121.6(9) 1_555 1_555 1_555 no C(45) C(44) H(50) 119.8(10) 1_555 1_555 1_555 no C(44) C(45) C(46) 119.9(8) 1_555 1_555 1_555 yes C(44) C(45) H(51) 120.0(10) 1_555 1_555 1_555 no C(46) C(45) H(51) 120.1(9) 1_555 1_555 1_555 no C(41) C(46) C(45) 121.0(7) 1_555 1_555 1_555 yes C(41) C(46) H(52) 119.5(8) 1_555 1_555 1_555 no C(45) C(46) H(52) 119.5(8) 1_555 1_555 1_555 no Cl(2) C(47) P(2) 111.7(3) 1_555 1_555 1_555 yes Cl(2) C(47) H(56) 109.3(5) 1_555 1_555 1_555 no Cl(2) C(47) H(57) 111.1(5) 1_555 1_555 1_555 no P(2) C(47) H(56) 109.5(5) 1_555 1_555 1_555 no P(2) C(47) H(57) 111.2(5) 1_555 1_555 1_555 no H(56) C(47) H(57) 103.7(6) 1_555 1_555 1_555 no Cl(3) C(48) Cl(4) 111.8(4) 1_555 1_555 1_555 yes Cl(3) C(48) H(58) 109.8(6) 1_555 1_555 1_555 no Cl(3) C(48) H(59) 109.4(6) 1_555 1_555 1_555 no Cl(4) C(48) H(58) 110.0(6) 1_555 1_555 1_555 no Cl(4) C(48) H(59) 109.6(6) 1_555 1_555 1_555 no H(58) C(48) H(59) 106.1(7) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(48) 3.362(7) 1_555 1_556 ? Cl(2) C(7) 3.494(9) 1_555 2_556 ? Cl(2) C(19) 3.518(7) 1_555 2_556 ? Cl(2) C(20) 3.549(6) 1_555 2_556 ? Cl(4) Cl(4) 3.368(5) 1_555 2_565 ? Cl(4) C(31) 3.461(9) 1_555 1_555 ? O(2) C(48) 3.086(9) 1_555 1_556 ? O(4) C(48) 3.524(9) 1_555 1_556 ? O(6) C(46) 3.193(10) 1_555 1_656 ? O(6) C(47) 3.20(1) 1_555 1_656 ? C(10) C(23) 3.49(1) 1_555 2_667 ? C(24) C(24) 3.57(2) 1_555 2_668 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_5a #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 10 10:31:55 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source 'compound 5a' _chemical_name_common ? _chemical_formula_weight 887.85 _chemical_formula_analytical ? _chemical_formula_sum 'C47 H46 Cl2 N3 O2 P Ru ' _chemical_formula_moiety 'C47 H46 Cl2 N3 O2 P Ru ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.441(5) _cell_length_b 19.851(3) _cell_length_c 19.068(3) _cell_angle_alpha 90 _cell_angle_beta 93.17(2) _cell_angle_gamma 90 _cell_volume 4323(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.9 _cell_measurement_theta_max 13.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pale' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.940 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0.98 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 4 1 2 2 -2 1 2 2 _diffrn_reflns_number 6221 _reflns_number_total 5878 _reflns_number_observed 3169 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 6.35 _diffrn_reflns_av_sigmaI/netI 0.137 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 22.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08615 _diffrn_orient_matrix_UB_12 0.00330 _diffrn_orient_matrix_UB_13 0.01153 _diffrn_orient_matrix_UB_21 0.01544 _diffrn_orient_matrix_UB_22 -0.01220 _diffrn_orient_matrix_UB_23 -0.04952 _diffrn_orient_matrix_UB_31 -0.00196 _diffrn_orient_matrix_UB_32 0.04877 _diffrn_orient_matrix_UB_33 -0.01316 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 188 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 184 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru1 0.13535(6) 0.09484(3) 0.24477(3) 0.0334(2) Uani d . 1.00 . Cl1 0.2620(2) 0.1641(1) 0.3221(1) 0.0522(7) Uani d . 1.00 . Cl2 -0.0073(2) 0.0313(1) 0.1734(1) 0.0553(7) Uani d . 1.00 . P1 0.2962(2) 0.0373(1) 0.1956(1) 0.0354(6) Uani d . 1.00 . O1 0.2545(6) -0.1034(3) 0.2393(3) 0.069(2) Uani d . 1.00 . O2 0.2061(6) 0.0421(3) 0.0488(3) 0.059(2) Uani d . 1.00 . N1 0.1060(6) -0.0139(3) 0.3625(4) 0.041(2) Uani d . 1.00 . N2 -0.0794(6) 0.1726(4) 0.3003(4) 0.048(2) Uani d . 1.00 . N3 0.1097(6) 0.2039(3) 0.1256(3) 0.040(2) Uani d . 1.00 . C1 0.2486(7) -0.0343(4) 0.1402(4) 0.041(3) Uani d . 1.00 . C2 0.2334(8) -0.0987(5) 0.1682(5) 0.050(3) Uani d . 1.00 . C3 0.1947(9) -0.1521(4) 0.1258(6) 0.068(4) Uani d . 1.00 . C4 0.1646(10) -0.1405(5) 0.0566(5) 0.069(4) Uani d . 1.00 . C5 0.1665(9) -0.0763(5) 0.0277(5) 0.061(3) Uani d . 1.00 . C6 0.2068(7) -0.0232(4) 0.0713(4) 0.043(3) Uani d . 1.00 . C7 0.255(1) -0.1663(5) 0.2727(6) 0.090(4) Uani d . 1.00 . C8 0.159(1) 0.0598(7) -0.0179(6) 0.108(5) Uani d . 1.00 . C9 0.3955(7) 0.0864(4) 0.1423(4) 0.040(2) Uani d . 1.00 . C10 0.4538(9) 0.0612(5) 0.0867(5) 0.066(3) Uani d . 1.00 . C11 0.5337(9) 0.0989(7) 0.0523(6) 0.086(4) Uani d . 1.00 . C12 0.5595(9) 0.1641(6) 0.0741(6) 0.076(4) Uani d . 1.00 . C13 0.5021(8) 0.1895(5) 0.1297(6) 0.063(3) Uani d . 1.00 . C14 0.4197(8) 0.1520(5) 0.1629(5) 0.051(3) Uani d . 1.00 . C15 0.4109(7) 0.0015(4) 0.2567(4) 0.043(3) Uani d . 1.00 . C16 0.4122(8) 0.0117(5) 0.3286(5) 0.051(3) Uani d . 1.00 . C17 0.4989(9) -0.0168(6) 0.3726(5) 0.067(3) Uani d . 1.00 . C18 0.5845(10) -0.0554(6) 0.3467(6) 0.083(4) Uani d . 1.00 . C19 0.5866(9) -0.0661(6) 0.2754(6) 0.084(4) Uani d . 1.00 . C20 0.4995(9) -0.0373(5) 0.2317(5) 0.070(3) Uani d . 1.00 . C21 0.1221(7) 0.0247(4) 0.3181(4) 0.038(3) Uani d . 1.00 . C22 0.0658(8) -0.0579(4) 0.4140(4) 0.043(3) Uani d . 1.00 . C23 0.1212(8) -0.0548(5) 0.4806(5) 0.055(3) Uani d . 1.00 . C24 0.072(1) -0.0946(6) 0.5311(5) 0.080(4) Uani d . 1.00 . C25 -0.022(1) -0.1355(6) 0.5158(6) 0.086(4) Uani d . 1.00 . C26 -0.0708(9) -0.1380(5) 0.4493(7) 0.076(4) Uani d . 1.00 . C27 -0.0281(8) -0.0993(5) 0.3954(5) 0.058(3) Uani d . 1.00 . C28 0.2277(10) -0.0129(6) 0.4965(5) 0.080(4) Uani d . 1.00 . C29 -0.0806(9) -0.1008(6) 0.3217(6) 0.085(4) Uani d . 1.00 . C30 0.0006(8) 0.1423(4) 0.2812(4) 0.043(3) Uani d . 1.00 . C31 -0.1758(8) 0.2118(5) 0.3131(4) 0.052(3) Uani d . 1.00 . C32 -0.2866(9) 0.1857(6) 0.2976(5) 0.070(4) Uani d . 1.00 . C33 -0.3794(10) 0.2275(8) 0.3102(6) 0.100(5) Uani d . 1.00 . C34 -0.360(1) 0.2920(8) 0.3355(6) 0.109(5) Uani d . 1.00 . C35 -0.250(1) 0.3144(6) 0.3512(6) 0.093(5) Uani d . 1.00 . C36 -0.1529(10) 0.2752(5) 0.3413(5) 0.066(3) Uani d . 1.00 . C37 -0.302(1) 0.1163(7) 0.2716(7) 0.106(5) Uani d . 1.00 . C38 -0.035(1) 0.3001(6) 0.3604(7) 0.100(5) Uani d . 1.00 . C39 0.1278(7) 0.1641(4) 0.1683(4) 0.036(2) Uani d . 1.00 . C40 0.0669(8) 0.2508(4) 0.0747(4) 0.038(3) Uani d . 1.00 . C41 -0.0516(8) 0.2668(4) 0.0736(4) 0.046(3) Uani d . 1.00 . C42 -0.0913(9) 0.3118(5) 0.0215(5) 0.062(3) Uani d . 1.00 . C43 -0.016(1) 0.3370(5) -0.0257(5) 0.074(4) Uani d . 1.00 . C44 0.0975(10) 0.3213(5) -0.0212(5) 0.063(3) Uani d . 1.00 . C45 0.1435(8) 0.2766(4) 0.0287(4) 0.046(3) Uani d . 1.00 . C46 -0.1298(9) 0.2384(6) 0.1261(5) 0.080(4) Uani d . 1.00 . C47 0.2695(9) 0.2573(6) 0.0323(5) 0.070(4) Uani d . 1.00 . H1 0.1894 -0.1983 0.1454 0.0832 Uiso calc . 1.00 . H2 0.1402 -0.1796 0.0251 0.0815 Uiso calc . 1.00 . H3 0.1402 -0.0685 -0.0220 0.0749 Uiso calc . 1.00 . H4 0.1800 -0.1890 0.2646 0.1022 Uiso calc . 1.00 . H5 0.3127 -0.1966 0.2539 0.1022 Uiso calc . 1.00 . H6 0.2711 -0.1635 0.3218 0.1022 Uiso calc . 1.00 . H7 0.1661 0.1086 -0.0263 0.1171 Uiso calc . 1.00 . H8 0.2001 0.0386 -0.0550 0.1171 Uiso calc . 1.00 . H9 0.0784 0.0491 -0.0247 0.1171 Uiso calc . 1.00 . H10 0.4383 0.0158 0.0703 0.0775 Uiso calc . 1.00 . H11 0.5745 0.0810 0.0130 0.0994 Uiso calc . 1.00 . H12 0.6153 0.1928 0.0501 0.0887 Uiso calc . 1.00 . H13 0.5210 0.2356 0.1462 0.0713 Uiso calc . 1.00 . H14 0.3795 0.1727 0.2010 0.0624 Uiso calc . 1.00 . H15 0.3514 0.0398 0.3486 0.0614 Uiso calc . 1.00 . H16 0.4970 -0.0106 0.4241 0.0799 Uiso calc . 1.00 . H17 0.6446 -0.0752 0.3792 0.0952 Uiso calc . 1.00 . H18 0.6467 -0.0955 0.2575 0.0991 Uiso calc . 1.00 . H19 0.5031 -0.0442 0.1803 0.0828 Uiso calc . 1.00 . H20 0.1060 -0.0959 0.5789 0.0946 Uiso calc . 1.00 . H21 -0.0560 -0.1638 0.5522 0.1033 Uiso calc . 1.00 . H22 -0.1383 -0.1694 0.4382 0.0902 Uiso calc . 1.00 . H23 0.2959 -0.0407 0.5124 0.0941 Uiso calc . 1.00 . H24 0.2508 0.0119 0.4571 0.0941 Uiso calc . 1.00 . H25 0.2181 0.0188 0.5346 0.0941 Uiso calc . 1.00 . H26 -0.1103 -0.0584 0.3078 0.0943 Uiso calc . 1.00 . H27 -0.0236 -0.1150 0.2894 0.0943 Uiso calc . 1.00 . H28 -0.1450 -0.1334 0.3165 0.0943 Uiso calc . 1.00 . H29 -0.4598 0.2120 0.3021 0.1119 Uiso calc . 1.00 . H30 -0.4258 0.3206 0.3432 0.1217 Uiso calc . 1.00 . H31 -0.2393 0.3605 0.3706 0.1073 Uiso calc . 1.00 . H32 -0.3828 0.1040 0.2632 0.1108 Uiso calc . 1.00 . H33 -0.2645 0.1101 0.2277 0.1108 Uiso calc . 1.00 . H34 -0.2672 0.0838 0.3042 0.1108 Uiso calc . 1.00 . H35 0.0259 0.2667 0.3513 0.1080 Uiso calc . 1.00 . H36 -0.0131 0.3404 0.3362 0.1080 Uiso calc . 1.00 . H37 -0.0218 0.3104 0.4108 0.1080 Uiso calc . 1.00 . H38 -0.1751 0.3240 0.0182 0.0708 Uiso calc . 1.00 . H39 -0.0468 0.3658 -0.0623 0.0824 Uiso calc . 1.00 . H40 0.1509 0.3423 -0.0545 0.0756 Uiso calc . 1.00 . H41 -0.1040 0.2492 0.1727 0.0855 Uiso calc . 1.00 . H42 -0.2094 0.2533 0.1180 0.0855 Uiso calc . 1.00 . H43 -0.1320 0.1891 0.1226 0.0855 Uiso calc . 1.00 . H44 0.2885 0.2254 0.0692 0.0773 Uiso calc . 1.00 . H45 0.2925 0.2361 -0.0113 0.0773 Uiso calc . 1.00 . H46 0.3210 0.2954 0.0398 0.0773 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0390(4) 0.0294(3) 0.0312(3) 0.0006(4) -0.0033(3) 0.0028(4) Cl(1) 0.066(2) 0.039(1) 0.050(1) -0.007(1) -0.011(1) -0.008(1) Cl(2) 0.048(1) 0.065(2) 0.052(1) -0.009(1) -0.010(1) -0.007(1) P(1) 0.040(1) 0.028(1) 0.037(1) 0.001(1) -0.006(1) -0.003(1) O(1) 0.111(5) 0.038(4) 0.056(4) -0.011(4) -0.021(4) 0.008(3) O(2) 0.078(5) 0.057(4) 0.039(4) -0.005(4) -0.014(3) 0.005(3) N(1) 0.045(4) 0.039(4) 0.040(4) 0.004(4) -0.001(4) 0.007(4) N(2) 0.042(5) 0.057(5) 0.047(5) 0.013(4) 0.012(4) 0.009(4) N(3) 0.043(4) 0.040(4) 0.037(4) -0.002(4) 0.004(4) 0.001(4) C(1) 0.046(5) 0.042(5) 0.036(5) 0.000(4) -0.001(4) -0.004(4) C(2) 0.061(6) 0.039(5) 0.050(5) 0.002(5) -0.006(5) 0.001(5) C(3) 0.080(8) 0.029(5) 0.094(8) -0.016(5) 0.004(6) -0.017(6) C(4) 0.096(8) 0.055(7) 0.055(6) -0.009(6) -0.009(6) -0.020(6) C(5) 0.068(7) 0.069(7) 0.042(5) -0.011(5) -0.013(5) -0.023(5) C(6) 0.043(5) 0.049(6) 0.036(5) -0.002(5) 0.000(4) -0.006(5) C(7) 0.14(1) 0.032(6) 0.096(9) -0.002(7) 0.001(8) 0.025(6) C(8) 0.14(1) 0.115(10) 0.065(8) -0.030(9) -0.042(8) 0.027(7) C(9) 0.040(5) 0.043(6) 0.036(5) 0.000(5) -0.005(4) 0.002(4) C(10) 0.061(7) 0.070(7) 0.069(7) -0.005(6) 0.007(6) -0.025(6) C(11) 0.069(7) 0.12(1) 0.069(7) -0.021(8) 0.025(6) -0.010(8) C(12) 0.058(7) 0.090(9) 0.080(8) -0.014(7) 0.016(6) 0.007(7) C(13) 0.043(6) 0.063(7) 0.084(8) -0.014(5) 0.001(6) 0.000(6) C(14) 0.040(6) 0.057(6) 0.055(6) -0.008(5) -0.004(5) -0.001(5) C(15) 0.043(5) 0.034(5) 0.050(6) 0.009(4) -0.012(5) -0.006(4) C(16) 0.049(6) 0.053(6) 0.050(6) 0.002(5) -0.005(5) 0.002(5) C(17) 0.070(7) 0.080(8) 0.050(6) 0.008(6) -0.025(5) 0.011(6) C(18) 0.082(8) 0.079(8) 0.085(8) 0.029(7) -0.038(7) -0.008(7) C(19) 0.063(7) 0.081(8) 0.104(9) 0.033(6) -0.025(7) -0.030(7) C(20) 0.062(7) 0.087(8) 0.057(6) 0.030(6) -0.017(5) -0.024(6) C(21) 0.033(5) 0.044(5) 0.037(5) -0.001(4) -0.007(4) -0.003(4) C(22) 0.058(6) 0.038(5) 0.034(5) 0.017(5) 0.017(5) 0.017(4) C(23) 0.067(7) 0.053(6) 0.044(6) 0.016(5) 0.012(5) 0.007(5) C(24) 0.105(9) 0.089(8) 0.047(6) 0.026(8) 0.013(6) 0.027(7) C(25) 0.103(9) 0.084(9) 0.073(8) 0.009(8) 0.038(7) 0.029(7) C(26) 0.059(7) 0.047(6) 0.125(9) -0.002(5) 0.039(7) 0.026(7) C(27) 0.060(6) 0.044(6) 0.070(7) -0.001(6) 0.003(5) -0.005(6) C(28) 0.093(8) 0.079(8) 0.064(7) -0.006(7) -0.025(6) 0.000(6) C(29) 0.067(7) 0.089(9) 0.096(8) -0.018(7) -0.012(6) 0.000(8) C(30) 0.050(6) 0.048(6) 0.032(5) 0.002(5) 0.002(4) 0.010(4) C(31) 0.049(6) 0.071(7) 0.040(5) 0.011(6) 0.019(5) 0.021(5) C(32) 0.060(7) 0.098(9) 0.054(6) 0.015(7) 0.008(6) 0.019(6) C(33) 0.052(7) 0.17(1) 0.073(8) 0.022(9) -0.006(6) 0.027(9) C(34) 0.12(1) 0.15(1) 0.065(8) 0.083(9) 0.024(8) 0.016(8) C(35) 0.14(1) 0.073(8) 0.066(8) 0.035(8) 0.026(8) 0.005(6) C(36) 0.089(8) 0.060(7) 0.051(6) 0.026(6) 0.019(6) -0.002(5) C(37) 0.081(9) 0.13(1) 0.107(10) -0.031(8) -0.028(8) 0.035(9) C(38) 0.14(1) 0.058(8) 0.102(10) -0.012(8) 0.009(9) 0.002(7) C(39) 0.037(5) 0.037(5) 0.033(5) 0.001(4) -0.006(4) -0.001(4) C(40) 0.066(6) 0.027(5) 0.021(4) 0.000(4) -0.005(4) 0.000(4) C(41) 0.052(6) 0.045(5) 0.041(5) 0.007(5) -0.001(5) -0.001(5) C(42) 0.063(7) 0.070(7) 0.051(6) 0.023(6) -0.006(5) 0.011(5) C(43) 0.118(9) 0.056(7) 0.043(6) 0.016(7) -0.027(6) 0.007(5) C(44) 0.088(8) 0.062(7) 0.040(6) -0.010(6) 0.002(6) 0.019(5) C(45) 0.064(6) 0.039(5) 0.036(5) 0.003(5) 0.006(5) 0.004(4) C(46) 0.069(7) 0.102(9) 0.070(7) 0.004(7) 0.005(6) 0.023(7) C(47) 0.068(7) 0.093(8) 0.051(6) 0.001(6) 0.021(5) 0.010(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00087|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3169 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0654 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.297 _refine_ls_shift/esd_max 0.1860 _refine_ls_shift/esd_mean 0.0280 _refine_diff_density_min -0.41 _refine_diff_density_max 0.41 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.434(2) 1_555 1_555 yes Ru(1) Cl(2) 2.421(2) 1_555 1_555 yes Ru(1) P(1) 2.401(2) 1_555 1_555 yes Ru(1) C(21) 1.985(9) 1_555 1_555 yes Ru(1) C(30) 1.966(9) 1_555 1_555 yes Ru(1) C(39) 2.002(8) 1_555 1_555 yes P(1) C(1) 1.836(8) 1_555 1_555 yes P(1) C(9) 1.844(8) 1_555 1_555 yes P(1) C(15) 1.849(8) 1_555 1_555 yes O(1) C(2) 1.37(1) 1_555 1_555 yes O(1) C(7) 1.40(1) 1_555 1_555 yes O(2) C(6) 1.364(10) 1_555 1_555 yes O(2) C(8) 1.40(1) 1_555 1_555 yes N(1) C(21) 1.162(10) 1_555 1_555 yes N(1) C(22) 1.41(1) 1_555 1_555 yes N(2) C(30) 1.17(1) 1_555 1_555 yes N(2) C(31) 1.38(1) 1_555 1_555 yes N(3) C(39) 1.146(9) 1_555 1_555 yes N(3) C(40) 1.413(10) 1_555 1_555 yes C(1) C(2) 1.40(1) 1_555 1_555 yes C(1) C(6) 1.39(1) 1_555 1_555 yes C(2) C(3) 1.39(1) 1_555 1_555 yes C(3) C(4) 1.37(1) 1_555 1_555 yes C(4) C(5) 1.39(1) 1_555 1_555 yes C(5) C(6) 1.40(1) 1_555 1_555 yes C(9) C(10) 1.38(1) 1_555 1_555 yes C(9) C(14) 1.38(1) 1_555 1_555 yes C(10) C(11) 1.38(1) 1_555 1_555 yes C(11) C(12) 1.39(2) 1_555 1_555 yes C(12) C(13) 1.37(1) 1_555 1_555 yes C(13) C(14) 1.38(1) 1_555 1_555 yes C(15) C(16) 1.39(1) 1_555 1_555 yes C(15) C(20) 1.38(1) 1_555 1_555 yes C(16) C(17) 1.38(1) 1_555 1_555 yes C(17) C(18) 1.36(1) 1_555 1_555 yes C(18) C(19) 1.38(2) 1_555 1_555 yes C(19) C(20) 1.39(1) 1_555 1_555 yes C(22) C(23) 1.39(1) 1_555 1_555 yes C(22) C(27) 1.38(1) 1_555 1_555 yes C(23) C(24) 1.39(1) 1_555 1_555 yes C(23) C(28) 1.49(1) 1_555 1_555 yes C(24) C(25) 1.37(2) 1_555 1_555 yes C(25) C(26) 1.36(2) 1_555 1_555 yes C(26) C(27) 1.39(1) 1_555 1_555 yes C(27) C(29) 1.50(1) 1_555 1_555 yes C(31) C(32) 1.39(1) 1_555 1_555 yes C(31) C(36) 1.39(1) 1_555 1_555 yes C(32) C(33) 1.38(2) 1_555 1_555 yes C(32) C(37) 1.47(2) 1_555 1_555 yes C(33) C(34) 1.38(2) 1_555 1_555 yes C(34) C(35) 1.35(2) 1_555 1_555 yes C(35) C(36) 1.38(1) 1_555 1_555 yes C(36) C(38) 1.46(2) 1_555 1_555 yes C(40) C(41) 1.39(1) 1_555 1_555 yes C(40) C(45) 1.37(1) 1_555 1_555 yes C(41) C(42) 1.39(1) 1_555 1_555 yes C(41) C(46) 1.49(1) 1_555 1_555 yes C(42) C(43) 1.37(1) 1_555 1_555 yes C(43) C(44) 1.34(1) 1_555 1_555 yes C(44) C(45) 1.38(1) 1_555 1_555 yes C(45) C(47) 1.49(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(2) C(24) 3.57(1) 1_555 3_556 ? N(3) C(7) 3.53(1) 1_555 2_555 ? C(22) C(24) 3.59(1) 1_555 3_556 ? C(33) C(44) 3.38(2) 1_555 4_455 ? C(34) C(44) 3.59(2) 1_555 4_455 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_5b #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 10 10:32:26 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source 'compound 5b' _chemical_name_common ? _chemical_formula_weight 929.93 _chemical_formula_analytical ? _chemical_formula_sum 'C50 H52 Cl2 N3 O2 P Ru ' _chemical_formula_moiety 'C50 H52 Cl2 N3 O2 P Ru ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.667(3) _cell_length_b 20.205(4) _cell_length_c 19.932(4) _cell_angle_alpha 90 _cell_angle_beta 93.17(2) _cell_angle_gamma 90 _cell_volume 4691(1) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.4 _cell_measurement_theta_max 14.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pale' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1928.00 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.960 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% -0.07 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 -1 0 1 -4 0 2 -3 _diffrn_reflns_number 6729 _reflns_number_total 6364 _reflns_number_observed 4334 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 5.32 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00845 _diffrn_orient_matrix_UB_12 0.04520 _diffrn_orient_matrix_UB_13 -0.02010 _diffrn_orient_matrix_UB_21 0.01883 _diffrn_orient_matrix_UB_22 -0.01818 _diffrn_orient_matrix_UB_23 -0.04474 _diffrn_orient_matrix_UB_31 -0.08332 _diffrn_orient_matrix_UB_32 -0.00869 _diffrn_orient_matrix_UB_33 -0.01093 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 200 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 208 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru1 0.15720(5) 0.08339(3) 0.23486(3) 0.0352(2) Uani d . 1.00 . Cl1 0.0158(2) 0.0242(1) 0.1644(1) 0.0569(7) Uani d . 1.00 . Cl2 0.2844(2) 0.1481(1) 0.3108(1) 0.0499(7) Uani d . 1.00 . P1 0.3148(2) 0.0281(1) 0.1856(1) 0.0350(6) Uani d . 1.00 . O1 0.2169(5) 0.0397(3) 0.0477(3) 0.058(2) Uani d . 1.00 . O2 0.2873(6) -0.1155(3) 0.2202(4) 0.067(2) Uani d . 1.00 . N1 0.1421(6) 0.1950(4) 0.1242(4) 0.047(2) Uani d . 1.00 . N2 -0.0495(6) 0.1607(4) 0.2904(4) 0.052(2) Uani d . 1.00 . N3 0.1106(6) -0.0224(4) 0.3454(4) 0.049(2) Uani d . 1.00 . C1 0.2675(6) -0.0404(4) 0.1306(4) 0.042(2) Uani d . 1.00 . C2 0.2206(7) -0.0264(5) 0.0655(5) 0.049(3) Uani d . 1.00 . C3 0.1804(8) -0.0825(7) 0.0241(5) 0.078(4) Uani d . 1.00 . C4 0.1841(9) -0.1457(5) 0.0498(6) 0.076(4) Uani d . 1.00 . C5 0.2208(8) -0.1583(5) 0.1134(5) 0.059(3) Uani d . 1.00 . C6 0.2583(7) -0.1065(4) 0.1538(5) 0.045(3) Uani d . 1.00 . C7 0.160(1) 0.0624(7) -0.0120(7) 0.106(5) Uani d . 1.00 . C8 0.2634(10) -0.1753(5) 0.2519(6) 0.075(4) Uani d . 1.00 . C9 0.4279(7) -0.0095(4) 0.2418(5) 0.042(2) Uani d . 1.00 . C10 0.5238(8) -0.0386(5) 0.2149(5) 0.055(3) Uani d . 1.00 . C11 0.6072(9) -0.0693(5) 0.2561(7) 0.072(4) Uani d . 1.00 . C12 0.5966(9) -0.0721(5) 0.3232(6) 0.074(4) Uani d . 1.00 . C13 0.5044(10) -0.0439(5) 0.3508(5) 0.065(3) Uani d . 1.00 . C14 0.4205(7) -0.0113(4) 0.3101(5) 0.048(3) Uani d . 1.00 . C15 0.4120(6) 0.0815(4) 0.1377(4) 0.038(2) Uani d . 1.00 . C16 0.4467(7) 0.1411(4) 0.1674(4) 0.044(3) Uani d . 1.00 . C17 0.5309(8) 0.1792(5) 0.1392(5) 0.057(3) Uani d . 1.00 . C18 0.5771(8) 0.1607(5) 0.0814(6) 0.065(3) Uani d . 1.00 . C19 0.5413(9) 0.1032(6) 0.0493(6) 0.076(4) Uani d . 1.00 . C20 0.4598(8) 0.0624(5) 0.0785(5) 0.056(3) Uani d . 1.00 . C21 0.1554(7) 0.1543(4) 0.1643(4) 0.042(3) Uani d . 1.00 . C22 0.1057(8) 0.2432(4) 0.0799(4) 0.044(3) Uani d . 1.00 . C23 -0.0094(8) 0.2638(5) 0.0805(5) 0.052(3) Uani d . 1.00 . C24 -0.0436(8) 0.3138(5) 0.0365(5) 0.060(3) Uani d . 1.00 . C25 0.0321(10) 0.3428(5) -0.0047(5) 0.065(3) Uani d . 1.00 . C26 0.1442(9) 0.3210(5) -0.0042(5) 0.060(3) Uani d . 1.00 . C27 0.1830(8) 0.2709(5) 0.0380(5) 0.050(3) Uani d . 1.00 . C28 -0.0908(9) 0.2333(6) 0.1278(6) 0.080(4) Uani d . 1.00 . C29 -0.006(1) 0.3983(6) -0.0521(6) 0.091(4) Uani d . 1.00 . C30 0.3051(10) 0.2475(6) 0.0395(6) 0.077(4) Uani d . 1.00 . C31 0.0288(7) 0.1325(4) 0.2711(4) 0.044(3) Uani d . 1.00 . C32 -0.1485(7) 0.1943(4) 0.3090(4) 0.042(3) Uani d . 1.00 . C33 -0.2541(8) 0.1626(5) 0.2998(5) 0.056(3) Uani d . 1.00 . C34 -0.3497(7) 0.1966(6) 0.3164(5) 0.063(3) Uani d . 1.00 . C35 -0.3437(8) 0.2572(6) 0.3427(5) 0.060(3) Uani d . 1.00 . C36 -0.2389(9) 0.2861(5) 0.3509(5) 0.058(3) Uani d . 1.00 . C37 -0.1381(7) 0.2566(4) 0.3343(5) 0.047(3) Uani d . 1.00 . C38 -0.262(1) 0.0954(7) 0.2705(8) 0.106(5) Uani d . 1.00 . C39 -0.4526(9) 0.2894(7) 0.3631(6) 0.091(4) Uani d . 1.00 . C40 -0.026(1) 0.2894(6) 0.3416(8) 0.091(4) Uani d . 1.00 . C41 0.1355(7) 0.0143(4) 0.3041(5) 0.044(3) Uani d . 1.00 . C42 0.0587(7) -0.0635(4) 0.3919(4) 0.045(3) Uani d . 1.00 . C43 -0.0316(7) -0.1054(5) 0.3695(5) 0.047(3) Uani d . 1.00 . C44 -0.0843(7) -0.1414(5) 0.4177(5) 0.052(3) Uani d . 1.00 . C45 -0.0510(8) -0.1391(5) 0.4852(5) 0.056(3) Uani d . 1.00 . C46 0.0410(10) -0.1000(5) 0.5050(5) 0.064(3) Uani d . 1.00 . C47 0.0995(8) -0.0611(5) 0.4593(5) 0.054(3) Uani d . 1.00 . C48 -0.0686(10) -0.1093(6) 0.2962(6) 0.075(4) Uani d . 1.00 . C49 -0.113(1) -0.1794(7) 0.5351(6) 0.093(4) Uani d . 1.00 . C50 0.2007(9) -0.0172(6) 0.4801(6) 0.074(4) Uani d . 1.00 . H1 0.1499 -0.0761 -0.0210 0.0987 Uiso calc . 1.00 . H2 0.1618 -0.1839 0.0220 0.0891 Uiso calc . 1.00 . H3 0.2212 -0.2036 0.1317 0.0732 Uiso calc . 1.00 . H4 0.5338 -0.0369 0.1673 0.0643 Uiso calc . 1.00 . H5 0.6717 -0.0883 0.2364 0.0830 Uiso calc . 1.00 . H6 0.6522 -0.0962 0.3509 0.0847 Uiso calc . 1.00 . H7 0.4995 -0.0450 0.3988 0.0772 Uiso calc . 1.00 . H8 0.3566 0.0096 0.3305 0.0572 Uiso calc . 1.00 . H9 0.4123 0.1553 0.2090 0.0533 Uiso calc . 1.00 . H10 0.5573 0.2199 0.1613 0.0714 Uiso calc . 1.00 . H11 0.6314 0.1898 0.0596 0.0770 Uiso calc . 1.00 . H12 0.5752 0.0901 0.0094 0.0929 Uiso calc . 1.00 . H13 0.4364 0.0223 0.0567 0.0691 Uiso calc . 1.00 . H14 -0.1227 0.3286 0.0334 0.0708 Uiso calc . 1.00 . H15 0.1938 0.3402 -0.0360 0.0732 Uiso calc . 1.00 . H16 -0.4234 0.1756 0.3093 0.0735 Uiso calc . 1.00 . H17 -0.2341 0.3298 0.3700 0.0722 Uiso calc . 1.00 . H18 -0.1461 -0.1708 0.4029 0.0608 Uiso calc . 1.00 . H19 0.0678 -0.0995 0.5512 0.0784 Uiso calc . 1.00 . H20 0.1683 0.1103 -0.0155 0.1279 Uiso calc . 1.00 . H21 0.1913 0.0433 -0.0504 0.1279 Uiso calc . 1.00 . H22 0.0803 0.0529 -0.0121 0.1279 Uiso calc . 1.00 . H23 0.1812 -0.1850 0.2496 0.0888 Uiso calc . 1.00 . H24 0.3001 -0.2125 0.2322 0.0888 Uiso calc . 1.00 . H25 0.2870 -0.1747 0.2991 0.0888 Uiso calc . 1.00 . H26 -0.1640 0.2514 0.1224 0.0951 Uiso calc . 1.00 . H27 -0.0949 0.1858 0.1206 0.0951 Uiso calc . 1.00 . H28 -0.0613 0.2394 0.1738 0.0951 Uiso calc . 1.00 . H29 0.0394 0.4362 -0.0424 0.1087 Uiso calc . 1.00 . H30 0.0045 0.3848 -0.0977 0.1087 Uiso calc . 1.00 . H31 -0.0843 0.4079 -0.0475 0.1087 Uiso calc . 1.00 . H32 0.3198 0.2138 0.0716 0.0865 Uiso calc . 1.00 . H33 0.3236 0.2312 -0.0040 0.0865 Uiso calc . 1.00 . H34 0.3571 0.2840 0.0501 0.0865 Uiso calc . 1.00 . H35 -0.2962 0.0639 0.3015 0.1177 Uiso calc . 1.00 . H36 -0.3070 0.0938 0.2297 0.1177 Uiso calc . 1.00 . H37 -0.1868 0.0775 0.2628 0.1177 Uiso calc . 1.00 . H38 -0.4355 0.3334 0.3798 0.0998 Uiso calc . 1.00 . H39 -0.5069 0.2940 0.3254 0.0998 Uiso calc . 1.00 . H40 -0.4868 0.2651 0.3972 0.0998 Uiso calc . 1.00 . H41 0.0268 0.2650 0.3709 0.1051 Uiso calc . 1.00 . H42 0.0069 0.2943 0.2992 0.1051 Uiso calc . 1.00 . H43 -0.0335 0.3330 0.3608 0.1051 Uiso calc . 1.00 . H44 -0.1468 -0.0976 0.2880 0.0904 Uiso calc . 1.00 . H45 -0.0221 -0.0810 0.2704 0.0904 Uiso calc . 1.00 . H46 -0.0588 -0.1541 0.2794 0.0904 Uiso calc . 1.00 . H47 -0.1403 -0.1511 0.5705 0.1070 Uiso calc . 1.00 . H48 -0.1745 -0.2030 0.5156 0.1070 Uiso calc . 1.00 . H49 -0.0594 -0.2103 0.5578 0.1070 Uiso calc . 1.00 . H50 0.2193 -0.0215 0.5280 0.0916 Uiso calc . 1.00 . H51 0.2686 -0.0299 0.4578 0.0916 Uiso calc . 1.00 . H52 0.1852 0.0279 0.4708 0.0916 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0283(3) 0.0363(4) 0.0415(4) 0.0068(3) 0.0059(3) 0.0055(3) Cl(1) 0.032(1) 0.077(2) 0.062(2) -0.003(1) 0.000(1) -0.003(1) Cl(2) 0.054(1) 0.046(1) 0.050(1) 0.000(1) 0.003(1) -0.007(1) P(1) 0.026(1) 0.034(1) 0.045(1) 0.0008(9) 0.0018(9) -0.002(1) O(1) 0.055(4) 0.068(5) 0.051(4) -0.010(3) -0.006(3) 0.005(3) O(2) 0.076(5) 0.044(4) 0.078(5) -0.014(4) -0.020(4) 0.007(4) N(1) 0.052(4) 0.042(4) 0.046(5) 0.005(4) 0.000(4) 0.017(4) N(2) 0.040(4) 0.057(5) 0.061(5) 0.015(4) 0.017(4) 0.014(4) N(3) 0.040(4) 0.054(5) 0.055(5) 0.004(4) 0.011(4) 0.012(4) C(1) 0.020(4) 0.051(5) 0.054(5) 0.000(4) 0.001(4) -0.010(4) C(2) 0.030(4) 0.063(6) 0.055(6) -0.010(4) 0.015(4) -0.014(5) C(3) 0.033(5) 0.15(1) 0.046(6) -0.028(6) 0.013(4) -0.043(7) C(4) 0.064(6) 0.053(6) 0.114(10) -0.034(5) 0.040(6) -0.025(7) C(5) 0.044(5) 0.060(6) 0.072(7) -0.010(5) 0.011(5) -0.018(6) C(6) 0.024(4) 0.044(5) 0.068(6) -0.006(4) 0.002(4) -0.007(5) C(7) 0.12(1) 0.12(1) 0.078(9) -0.030(9) -0.035(8) 0.029(8) C(8) 0.073(7) 0.057(7) 0.095(9) -0.005(6) 0.007(6) 0.015(6) C(9) 0.029(4) 0.024(4) 0.070(6) -0.002(4) -0.010(4) -0.006(4) C(10) 0.041(5) 0.049(6) 0.073(7) 0.008(5) -0.002(5) -0.010(5) C(11) 0.045(6) 0.068(7) 0.100(9) 0.023(5) -0.016(6) -0.014(6) C(12) 0.056(6) 0.064(7) 0.098(9) 0.029(5) -0.027(6) -0.003(6) C(13) 0.077(7) 0.061(7) 0.055(6) 0.008(6) -0.023(6) -0.004(5) C(14) 0.044(5) 0.047(5) 0.053(6) 0.012(4) -0.009(4) -0.002(5) C(15) 0.022(4) 0.045(5) 0.047(5) -0.003(4) 0.003(4) 0.006(4) C(16) 0.038(5) 0.044(5) 0.050(5) -0.001(4) 0.001(4) -0.004(4) C(17) 0.054(6) 0.049(6) 0.067(7) -0.015(5) 0.005(5) -0.001(5) C(18) 0.046(5) 0.073(7) 0.076(7) -0.013(5) 0.016(5) 0.007(6) C(19) 0.048(6) 0.111(9) 0.071(7) -0.005(6) 0.037(5) -0.011(7) C(20) 0.049(5) 0.060(6) 0.061(6) -0.012(5) 0.014(5) -0.018(5) C(21) 0.036(5) 0.041(5) 0.051(5) 0.005(4) 0.009(4) -0.008(4) C(22) 0.056(5) 0.029(5) 0.044(5) 0.006(4) -0.011(4) 0.001(4) C(23) 0.056(6) 0.047(6) 0.052(6) 0.007(5) -0.008(5) 0.000(5) C(24) 0.058(6) 0.056(6) 0.064(6) 0.012(5) -0.020(5) -0.008(5) C(25) 0.090(8) 0.041(6) 0.059(6) 0.002(6) -0.030(6) 0.001(5) C(26) 0.074(7) 0.059(6) 0.045(6) -0.012(5) -0.014(5) 0.013(5) C(27) 0.053(5) 0.050(6) 0.047(5) -0.007(5) -0.011(5) 0.009(5) C(28) 0.057(7) 0.090(9) 0.093(9) 0.009(6) 0.006(6) 0.017(7) C(29) 0.12(1) 0.079(8) 0.067(7) 0.008(8) -0.037(7) 0.023(6) C(30) 0.074(7) 0.084(8) 0.075(7) 0.006(6) 0.009(6) 0.027(6) C(31) 0.034(5) 0.051(5) 0.047(5) 0.008(4) 0.004(4) 0.009(4) C(32) 0.033(4) 0.049(5) 0.045(5) 0.016(4) 0.011(4) 0.010(4) C(33) 0.045(5) 0.065(6) 0.059(6) -0.002(5) 0.004(5) -0.010(5) C(34) 0.023(4) 0.097(8) 0.069(7) 0.001(5) 0.002(4) 0.006(6) C(35) 0.051(6) 0.081(7) 0.049(6) 0.033(5) 0.009(5) 0.009(5) C(36) 0.059(6) 0.051(6) 0.065(6) 0.017(5) 0.007(5) -0.002(5) C(37) 0.036(5) 0.046(5) 0.060(6) 0.009(4) 0.004(4) 0.004(5) C(38) 0.071(8) 0.11(1) 0.13(1) -0.014(8) 0.000(8) -0.026(9) C(39) 0.061(6) 0.13(1) 0.080(8) 0.050(7) 0.029(6) 0.021(7) C(40) 0.067(7) 0.052(7) 0.15(1) 0.000(6) 0.002(8) 0.011(7) C(41) 0.031(4) 0.046(5) 0.054(6) 0.005(4) 0.002(4) 0.004(5) C(42) 0.046(5) 0.044(5) 0.045(5) 0.007(4) 0.011(4) 0.014(4) C(43) 0.037(5) 0.052(6) 0.053(6) 0.009(4) 0.005(4) 0.007(5) C(44) 0.042(5) 0.052(6) 0.062(6) -0.002(4) 0.013(5) 0.004(5) C(45) 0.060(6) 0.051(6) 0.059(6) 0.001(5) 0.013(5) 0.011(5) C(46) 0.083(7) 0.070(7) 0.041(5) 0.001(6) 0.014(5) 0.015(5) C(47) 0.055(6) 0.045(6) 0.061(6) 0.011(5) 0.000(5) 0.003(5) C(48) 0.063(7) 0.099(9) 0.062(7) -0.012(6) -0.003(6) 0.009(6) C(49) 0.111(10) 0.099(9) 0.073(8) -0.016(8) 0.032(7) 0.029(7) C(50) 0.069(7) 0.072(8) 0.079(8) -0.005(6) -0.005(6) -0.005(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00245|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4334 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0534 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1113 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.898 _refine_ls_shift/esd_max 0.7450 _refine_ls_shift/esd_mean 0.0340 _refine_diff_density_min -0.67 _refine_diff_density_max 1.04 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.423(2) 1_555 1_555 yes Ru(1) Cl(2) 2.439(2) 1_555 1_555 yes Ru(1) P(1) 2.408(2) 1_555 1_555 yes Ru(1) C(21) 2.008(9) 1_555 1_555 yes Ru(1) C(31) 1.967(9) 1_555 1_555 yes Ru(1) C(41) 1.989(9) 1_555 1_555 yes P(1) C(1) 1.831(9) 1_555 1_555 yes P(1) C(9) 1.846(8) 1_555 1_555 yes P(1) C(15) 1.866(8) 1_555 1_555 yes O(1) C(2) 1.38(1) 1_555 1_555 yes O(1) C(7) 1.41(1) 1_555 1_555 yes O(2) C(6) 1.36(1) 1_555 1_555 yes O(2) C(8) 1.40(1) 1_555 1_555 yes N(1) C(21) 1.15(1) 1_555 1_555 yes N(1) C(22) 1.37(1) 1_555 1_555 yes N(2) C(31) 1.16(1) 1_555 1_555 yes N(2) C(32) 1.41(1) 1_555 1_555 yes N(3) C(41) 1.16(1) 1_555 1_555 yes N(3) C(42) 1.41(1) 1_555 1_555 yes C(1) C(2) 1.41(1) 1_555 1_555 yes C(1) C(6) 1.42(1) 1_555 1_555 yes C(2) C(3) 1.46(1) 1_555 1_555 yes C(3) C(4) 1.38(2) 1_555 1_555 yes C(4) C(5) 1.34(2) 1_555 1_555 yes C(5) C(6) 1.38(1) 1_555 1_555 yes C(9) C(10) 1.40(1) 1_555 1_555 yes C(9) C(14) 1.37(1) 1_555 1_555 yes C(10) C(11) 1.39(1) 1_555 1_555 yes C(11) C(12) 1.35(2) 1_555 1_555 yes C(12) C(13) 1.36(2) 1_555 1_555 yes C(13) C(14) 1.40(1) 1_555 1_555 yes C(15) C(16) 1.39(1) 1_555 1_555 yes C(15) C(20) 1.39(1) 1_555 1_555 yes C(16) C(17) 1.39(1) 1_555 1_555 yes C(17) C(18) 1.35(1) 1_555 1_555 yes C(18) C(19) 1.38(2) 1_555 1_555 yes C(19) C(20) 1.41(1) 1_555 1_555 yes C(22) C(23) 1.41(1) 1_555 1_555 yes C(22) C(27) 1.38(1) 1_555 1_555 yes C(23) C(24) 1.38(1) 1_555 1_555 yes C(23) C(28) 1.51(1) 1_555 1_555 yes C(24) C(25) 1.37(1) 1_555 1_555 yes C(25) C(26) 1.38(1) 1_555 1_555 yes C(25) C(29) 1.52(1) 1_555 1_555 yes C(26) C(27) 1.38(1) 1_555 1_555 yes C(27) C(30) 1.50(1) 1_555 1_555 yes C(32) C(33) 1.39(1) 1_555 1_555 yes C(32) C(37) 1.36(1) 1_555 1_555 yes C(33) C(34) 1.37(1) 1_555 1_555 yes C(33) C(38) 1.48(2) 1_555 1_555 yes C(34) C(35) 1.33(1) 1_555 1_555 yes C(35) C(36) 1.36(1) 1_555 1_555 yes C(35) C(39) 1.50(1) 1_555 1_555 yes C(36) C(37) 1.38(1) 1_555 1_555 yes C(37) C(40) 1.47(1) 1_555 1_555 yes C(42) C(43) 1.41(1) 1_555 1_555 yes C(42) C(47) 1.40(1) 1_555 1_555 yes C(43) C(44) 1.38(1) 1_555 1_555 yes C(43) C(48) 1.50(1) 1_555 1_555 yes C(44) C(45) 1.38(1) 1_555 1_555 yes C(45) C(46) 1.37(1) 1_555 1_555 yes C(45) C(49) 1.50(1) 1_555 1_555 yes C(46) C(47) 1.41(1) 1_555 1_555 yes C(47) C(50) 1.52(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C(4) C(39) 3.54(1) 1_555 2_445 ? C(5) C(39) 3.36(1) 1_555 2_445 ? C(11) C(40) 3.56(2) 1_555 2_545 ? C(13) C(29) 3.53(2) 1_555 4_555 ? C(26) C(35) 3.45(1) 1_555 4_554 ? C(26) C(39) 3.59(2) 1_555 4_554 ? C(26) C(34) 3.60(1) 1_555 4_554 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_6 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 10 10:27:20 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source compound6 _chemical_name_common ? _chemical_formula_weight 929.60 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H40 Cl4 O5 P2 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.70(1) _cell_length_b 14.555(9) _cell_length_c 12.346(7) _cell_angle_alpha 101.25(5) _cell_angle_beta 114.69(5) _cell_angle_gamma 68.35(5) _cell_volume 2075(2) _cell_formula_units_Z 2 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 948.00 _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.595 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.31 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 0 3 0 1 2 1 1 _diffrn_reflns_number 7623 _reflns_number_total 7307 _reflns_number_observed 5251 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 1.60 _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05739 _diffrn_orient_matrix_UB_12 0.01161 _diffrn_orient_matrix_UB_13 -0.02106 _diffrn_orient_matrix_UB_21 0.02627 _diffrn_orient_matrix_UB_22 0.03554 _diffrn_orient_matrix_UB_23 0.07925 _diffrn_orient_matrix_UB_31 0.05677 _diffrn_orient_matrix_UB_32 -0.06387 _diffrn_orient_matrix_UB_33 0.03525 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 84 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 10 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 2 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ru 0.17270(5) 0.19492(4) 0.00937(5) 0.0255(2) Uani d . 1.00 . Cl1 0.0997(2) 0.0596(2) -0.0682(2) 0.0396(6) Uani d . 1.00 . Cl2 0.2080(2) 0.3485(2) 0.0802(2) 0.0420(6) Uani d . 1.00 . Cl3 0.5387(5) 0.3654(4) 0.2280(6) 0.169(2) Uani d . 1.00 . Cl4 0.4025(6) 0.5619(5) 0.2441(9) 0.270(4) Uani d . 1.00 . P1 0.1800(2) 0.1650(1) 0.1922(2) 0.0277(5) Uani d . 1.00 . P2 0.1620(2) 0.2170(1) -0.1853(2) 0.0293(5) Uani d . 1.00 . O2 -0.0056(4) 0.2824(4) -0.0009(5) 0.038(2) Uani d . 1.00 . O3 0.0652(5) 0.1182(5) 0.3317(5) 0.043(2) Uani d . 1.00 . O4 0.0425(6) 0.4337(4) -0.2149(5) 0.050(2) Uani d . 1.00 . O5 0.4016(5) 0.1978(5) -0.1065(6) 0.052(2) Uani d . 1.00 . O6 0.4157(5) 0.0798(5) 0.0791(6) 0.059(2) Uani d . 1.00 . C1 0.0313(6) 0.1990(6) 0.1671(6) 0.032(2) Uani d . 1.00 . C2 -0.0478(6) 0.2547(5) 0.0683(7) 0.032(2) Uani d . 1.00 . C3 -0.1643(7) 0.2824(7) 0.0380(8) 0.047(3) Uani d . 1.00 . C4 -0.2005(8) 0.2492(7) 0.1070(8) 0.050(3) Uani d . 1.00 . C5 -0.1281(7) 0.1950(7) 0.2033(8) 0.045(3) Uani d . 1.00 . C6 -0.0115(7) 0.1699(6) 0.2358(7) 0.039(2) Uani d . 1.00 . C7 -0.0716(8) 0.3736(7) -0.0599(8) 0.053(3) Uani d . 1.00 . C8 0.0309(8) 0.0612(7) 0.3825(8) 0.051(3) Uani d . 1.00 . C9 0.2487(7) 0.0368(6) 0.2348(6) 0.032(2) Uani d . 1.00 . C10 0.1917(7) -0.0328(6) 0.1938(7) 0.037(2) Uani d . 1.00 . C11 0.2454(9) -0.1278(7) 0.2238(8) 0.050(3) Uani d . 1.00 . C12 0.3591(9) -0.1594(7) 0.2977(9) 0.053(3) Uani d . 1.00 . C13 0.4186(8) -0.0941(7) 0.3382(8) 0.050(3) Uani d . 1.00 . C14 0.3642(6) 0.0039(6) 0.3079(7) 0.038(2) Uani d . 1.00 . C15 0.2460(6) 0.2338(6) 0.3266(6) 0.031(2) Uani d . 1.00 . C16 0.2002(7) 0.2744(6) 0.4132(6) 0.036(2) Uani d . 1.00 . C17 0.2533(9) 0.3291(7) 0.5109(7) 0.053(3) Uani d . 1.00 . C18 0.3498(8) 0.3449(8) 0.5232(8) 0.054(3) Uani d . 1.00 . C19 0.3962(8) 0.3044(8) 0.4378(8) 0.052(3) Uani d . 1.00 . C20 0.3448(7) 0.2508(7) 0.3400(7) 0.044(2) Uani d . 1.00 . C21 0.2197(7) 0.3123(6) -0.1815(6) 0.036(2) Uani d . 1.00 . C22 0.1528(8) 0.4116(6) -0.2013(7) 0.044(3) Uani d . 1.00 . C23 0.197(1) 0.4833(8) -0.2025(9) 0.063(4) Uani d . 1.00 . C24 0.314(1) 0.4547(9) -0.172(1) 0.067(4) Uani d . 1.00 . C25 0.3835(9) 0.3631(9) -0.1439(9) 0.058(3) Uani d . 1.00 . C26 0.3391(7) 0.2902(7) -0.1431(7) 0.040(2) Uani d . 1.00 . C27 -0.040(1) 0.5214(8) -0.272(1) 0.075(4) Uani d . 1.00 . C28 0.5226(9) 0.1683(9) -0.057(1) 0.072(4) Uani d . 1.00 . C29 0.0233(6) 0.2475(6) -0.3124(6) 0.033(2) Uani d . 1.00 . C30 -0.0614(8) 0.2173(7) -0.3106(8) 0.051(3) Uani d . 1.00 . C31 -0.1646(9) 0.2361(9) -0.4069(9) 0.067(3) Uani d . 1.00 . C32 -0.1837(9) 0.2847(10) -0.5014(9) 0.075(4) Uani d . 1.00 . C33 -0.1019(10) 0.3154(8) -0.5050(8) 0.062(3) Uani d . 1.00 . C34 0.0027(8) 0.2953(7) -0.4110(7) 0.049(3) Uani d . 1.00 . C35 0.2393(6) 0.1075(6) -0.2562(6) 0.033(2) Uani d . 1.00 . C36 0.2679(8) 0.0144(7) -0.2230(8) 0.045(3) Uani d . 1.00 . C37 0.3206(8) -0.0688(6) -0.2821(9) 0.052(3) Uani d . 1.00 . C38 0.3442(8) -0.0564(7) -0.3749(9) 0.055(3) Uani d . 1.00 . C39 0.3149(8) 0.0365(9) -0.4097(8) 0.057(3) Uani d . 1.00 . C40 0.2629(8) 0.1188(7) -0.3511(8) 0.047(3) Uani d . 1.00 . C41 0.3208(7) 0.1239(6) 0.0478(6) 0.034(2) Uani d . 1.00 . C42 0.410(1) 0.454(1) 0.183(2) 0.155(8) Uani d . 1.00 . H1 -0.2183 0.3243 -0.0307 0.0571 Uiso calc . 1.00 . H2 -0.2815 0.2640 0.0853 0.0605 Uiso calc . 1.00 . H3 -0.1558 0.1737 0.2516 0.0551 Uiso calc . 1.00 . H4 -0.0782 0.4284 -0.0010 0.0636 Uiso calc . 1.00 . H5 -0.0349 0.3862 -0.1041 0.0636 Uiso calc . 1.00 . H6 -0.1454 0.3740 -0.1117 0.0636 Uiso calc . 1.00 . H7 -0.0286 0.1033 0.4088 0.0666 Uiso calc . 1.00 . H8 0.0052 0.0125 0.3267 0.0666 Uiso calc . 1.00 . H9 0.0937 0.0287 0.4515 0.0666 Uiso calc . 1.00 . H10 0.1124 -0.0118 0.1429 0.0447 Uiso calc . 1.00 . H11 0.2035 -0.1736 0.1912 0.0594 Uiso calc . 1.00 . H12 0.3960 -0.2281 0.3210 0.0638 Uiso calc . 1.00 . H13 0.4987 -0.1143 0.3884 0.0624 Uiso calc . 1.00 . H14 0.4059 0.0502 0.3382 0.0453 Uiso calc . 1.00 . H15 0.1316 0.2639 0.4053 0.0453 Uiso calc . 1.00 . H16 0.2215 0.3566 0.5708 0.0622 Uiso calc . 1.00 . H17 0.3858 0.3837 0.5901 0.0639 Uiso calc . 1.00 . H18 0.4656 0.3136 0.4473 0.0612 Uiso calc . 1.00 . H19 0.3753 0.2261 0.2782 0.0554 Uiso calc . 1.00 . H20 0.1471 0.5508 -0.2237 0.0753 Uiso calc . 1.00 . H21 0.3474 0.5031 -0.1716 0.0788 Uiso calc . 1.00 . H22 0.4637 0.3468 -0.1232 0.0699 Uiso calc . 1.00 . H23 -0.0215 0.5788 -0.2289 0.0889 Uiso calc . 1.00 . H24 -0.0451 0.5204 -0.3514 0.0889 Uiso calc . 1.00 . H25 -0.1136 0.5274 -0.2752 0.0889 Uiso calc . 1.00 . H26 0.5536 0.1004 -0.0360 0.0863 Uiso calc . 1.00 . H27 0.5504 0.1740 -0.1140 0.0863 Uiso calc . 1.00 . H28 0.5487 0.2080 0.0126 0.0863 Uiso calc . 1.00 . H29 -0.0485 0.1851 -0.2417 0.0616 Uiso calc . 1.00 . H30 -0.2220 0.2124 -0.4078 0.0795 Uiso calc . 1.00 . H31 -0.2557 0.2953 -0.5688 0.0878 Uiso calc . 1.00 . H32 -0.1162 0.3514 -0.5715 0.0745 Uiso calc . 1.00 . H33 0.0630 0.3134 -0.4128 0.0593 Uiso calc . 1.00 . H34 0.2511 0.0059 -0.1584 0.0545 Uiso calc . 1.00 . H35 0.3415 -0.1343 -0.2566 0.0647 Uiso calc . 1.00 . H36 0.3799 -0.1127 -0.4172 0.0638 Uiso calc . 1.00 . H37 0.3300 0.0448 -0.4760 0.0676 Uiso calc . 1.00 . H38 0.2445 0.1853 -0.3753 0.0572 Uiso calc . 1.00 . H39 0.3812 0.4609 0.0975 0.1623 Uiso calc . 1.00 . H40 0.3557 0.4341 0.1964 0.1623 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0193(3) 0.0343(3) 0.0266(3) -0.0116(2) 0.0110(2) -0.0040(2) Cl(1) 0.044(1) 0.049(1) 0.0367(10) -0.0293(10) 0.0162(9) -0.0086(8) Cl(2) 0.051(1) 0.043(1) 0.040(1) -0.0254(10) 0.0197(9) -0.0089(8) Cl(3) 0.100(4) 0.162(5) 0.188(5) 0.008(4) 0.029(4) 0.031(4) Cl(4) 0.116(5) 0.118(5) 0.40(1) -0.024(4) -0.062(6) -0.021(6) P(1) 0.0215(10) 0.040(1) 0.0259(9) -0.0145(8) 0.0109(8) -0.0043(8) P(2) 0.028(1) 0.039(1) 0.0271(10) -0.0145(9) 0.0133(8) -0.0033(8) O(2) 0.019(3) 0.046(3) 0.046(3) 0.001(2) 0.014(2) 0.008(2) O(3) 0.036(3) 0.070(4) 0.039(3) -0.025(3) 0.019(3) 0.003(3) O(4) 0.051(4) 0.042(3) 0.061(4) -0.008(3) 0.030(3) -0.001(3) O(5) 0.027(3) 0.065(4) 0.066(4) -0.020(3) 0.012(3) 0.004(3) O(6) 0.024(4) 0.079(5) 0.066(4) 0.001(3) 0.019(3) 0.011(4) C(1) 0.028(4) 0.038(4) 0.035(4) -0.018(3) 0.014(3) -0.011(3) C(2) 0.022(4) 0.036(4) 0.040(4) -0.010(3) 0.017(3) -0.011(3) C(3) 0.024(4) 0.063(6) 0.050(5) -0.016(4) 0.012(4) -0.008(4) C(4) 0.033(5) 0.070(6) 0.061(6) -0.028(5) 0.025(4) -0.014(5) C(5) 0.030(5) 0.063(6) 0.054(5) -0.025(4) 0.025(4) -0.013(4) C(6) 0.033(4) 0.058(5) 0.034(4) -0.024(4) 0.018(4) -0.014(4) C(7) 0.036(5) 0.057(6) 0.061(6) 0.006(4) 0.023(4) 0.021(5) C(8) 0.058(6) 0.061(6) 0.057(5) -0.033(5) 0.029(5) -0.001(4) C(9) 0.032(4) 0.047(5) 0.028(4) -0.018(4) 0.019(3) -0.008(3) C(10) 0.038(5) 0.042(5) 0.037(4) -0.020(4) 0.016(4) -0.002(3) C(11) 0.063(6) 0.054(6) 0.049(5) -0.029(5) 0.030(5) -0.006(4) C(12) 0.053(6) 0.045(5) 0.061(6) -0.008(5) 0.025(5) 0.009(4) C(13) 0.034(5) 0.048(5) 0.063(6) -0.001(4) 0.016(4) 0.015(4) C(14) 0.021(4) 0.051(5) 0.042(4) -0.010(4) 0.011(3) 0.005(4) C(15) 0.031(4) 0.042(4) 0.028(4) -0.019(3) 0.012(3) -0.004(3) C(16) 0.041(5) 0.049(5) 0.032(4) -0.025(4) 0.020(4) -0.008(3) C(17) 0.066(7) 0.073(7) 0.033(4) -0.037(5) 0.026(4) -0.017(4) C(18) 0.051(6) 0.079(7) 0.041(5) -0.043(5) 0.011(4) -0.015(4) C(19) 0.036(5) 0.082(7) 0.046(5) -0.040(5) 0.009(4) -0.007(5) C(20) 0.030(4) 0.074(6) 0.039(4) -0.030(4) 0.016(4) -0.012(4) C(21) 0.046(5) 0.044(5) 0.030(4) -0.023(4) 0.022(4) -0.010(3) C(22) 0.064(6) 0.041(5) 0.037(4) -0.022(4) 0.029(4) -0.008(4) C(23) 0.098(9) 0.059(6) 0.059(6) -0.045(6) 0.044(6) -0.018(5) C(24) 0.094(9) 0.066(7) 0.085(8) -0.059(7) 0.051(7) -0.017(6) C(25) 0.061(7) 0.082(8) 0.059(6) -0.049(6) 0.028(5) -0.009(5) C(26) 0.042(5) 0.059(6) 0.036(4) -0.032(4) 0.021(4) -0.008(4) C(27) 0.077(8) 0.054(6) 0.076(7) 0.005(6) 0.029(6) 0.014(5) C(28) 0.039(6) 0.088(8) 0.094(8) -0.024(6) 0.029(6) -0.009(6) C(29) 0.029(4) 0.042(4) 0.030(4) -0.012(3) 0.013(3) -0.006(3) C(30) 0.039(5) 0.071(6) 0.046(5) -0.024(5) 0.011(4) 0.004(4) C(31) 0.040(6) 0.099(9) 0.061(6) -0.030(6) 0.003(5) 0.019(6) C(32) 0.046(7) 0.12(1) 0.043(6) -0.027(7) -0.005(5) 0.009(6) C(33) 0.064(7) 0.078(7) 0.035(5) -0.018(6) 0.008(5) 0.013(5) C(34) 0.048(6) 0.068(6) 0.032(4) -0.017(5) 0.013(4) 0.008(4) C(35) 0.028(4) 0.045(5) 0.032(4) -0.018(4) 0.015(3) -0.008(3) C(36) 0.045(5) 0.048(5) 0.055(5) -0.020(4) 0.035(4) -0.016(4) C(37) 0.053(6) 0.037(5) 0.068(6) -0.006(4) 0.033(5) -0.008(4) C(38) 0.036(5) 0.059(6) 0.064(6) -0.008(5) 0.028(5) -0.025(5) C(39) 0.044(6) 0.089(8) 0.043(5) -0.018(5) 0.030(4) -0.016(5) C(40) 0.046(5) 0.052(5) 0.047(5) -0.009(4) 0.026(4) 0.000(4) C(41) 0.024(4) 0.051(5) 0.033(4) -0.014(4) 0.014(3) -0.004(3) C(42) 0.051(9) 0.11(1) 0.26(2) -0.042(9) 0.00(1) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00181|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5251 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0725 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0984 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.911 _refine_ls_shift/esd_max 0.0330 _refine_ls_shift/esd_mean 0.0030 _refine_diff_density_min -2.48 _refine_diff_density_max 1.98 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl(1) 2.393(2) 1_555 1_555 yes Ru Cl(2) 2.381(2) 1_555 1_555 yes Ru P(1) 2.422(2) 1_555 1_555 yes Ru P(2) 2.339(2) 1_555 1_555 yes Ru O(4) 2.270(5) 1_555 1_555 yes Ru C(41) 1.810(7) 1_555 1_555 yes Cl(3) C(42) 1.56(2) 1_555 1_555 yes Cl(4) C(42) 1.71(1) 1_555 1_555 yes P(1) C(21) 1.847(7) 1_555 1_555 yes P(1) C(27) 1.860(7) 1_555 1_555 yes P(1) C(33) 1.823(8) 1_555 1_555 yes P(2) C(1) 1.806(7) 1_555 1_555 yes P(2) C(9) 1.827(7) 1_555 1_555 yes P(2) C(15) 1.809(8) 1_555 1_555 yes O(1) C(41) 1.143(9) 1_555 1_555 yes O(2) C(34) 1.363(9) 1_555 1_555 yes O(2) C(39) 1.43(1) 1_555 1_555 yes O(3) C(38) 1.38(1) 1_555 1_555 yes O(3) C(40) 1.41(1) 1_555 1_555 yes O(4) C(2) 1.403(9) 1_555 1_555 yes O(4) C(7) 1.427(10) 1_555 1_555 yes O(5) C(6) 1.339(9) 1_555 1_555 yes O(5) C(8) 1.44(1) 1_555 1_555 yes C(1) C(2) 1.387(10) 1_555 1_555 yes C(1) C(6) 1.41(1) 1_555 1_555 yes C(2) C(3) 1.40(1) 1_555 1_555 yes C(3) C(4) 1.40(1) 1_555 1_555 yes C(4) C(5) 1.34(1) 1_555 1_555 yes C(5) C(6) 1.39(1) 1_555 1_555 yes C(9) C(10) 1.39(1) 1_555 1_555 yes C(9) C(14) 1.41(1) 1_555 1_555 yes C(10) C(11) 1.38(1) 1_555 1_555 yes C(11) C(12) 1.37(1) 1_555 1_555 yes C(12) C(13) 1.38(1) 1_555 1_555 yes C(13) C(14) 1.37(1) 1_555 1_555 yes C(15) C(16) 1.38(1) 1_555 1_555 yes C(15) C(20) 1.408(10) 1_555 1_555 yes C(16) C(17) 1.34(1) 1_555 1_555 yes C(17) C(18) 1.39(1) 1_555 1_555 yes C(18) C(19) 1.38(1) 1_555 1_555 yes C(19) C(20) 1.34(1) 1_555 1_555 yes C(21) C(22) 1.34(1) 1_555 1_555 yes C(21) C(26) 1.39(1) 1_555 1_555 yes C(22) C(23) 1.40(1) 1_555 1_555 yes C(23) C(24) 1.37(1) 1_555 1_555 yes C(24) C(25) 1.37(1) 1_555 1_555 yes C(25) C(26) 1.38(1) 1_555 1_555 yes C(27) C(28) 1.40(1) 1_555 1_555 yes C(27) C(32) 1.37(1) 1_555 1_555 yes C(28) C(29) 1.37(1) 1_555 1_555 yes C(29) C(30) 1.36(1) 1_555 1_555 yes C(30) C(31) 1.37(2) 1_555 1_555 yes C(31) C(32) 1.40(1) 1_555 1_555 yes C(33) C(34) 1.40(1) 1_555 1_555 yes C(33) C(38) 1.39(1) 1_555 1_555 yes C(34) C(35) 1.39(1) 1_555 1_555 yes C(35) C(36) 1.32(1) 1_555 1_555 yes C(36) C(37) 1.40(1) 1_555 1_555 yes C(37) C(38) 1.39(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru Cl(2) 168.84(7) 1_555 1_555 1_555 yes Cl(1) Ru P(1) 91.18(7) 1_555 1_555 1_555 yes Cl(1) Ru P(2) 85.28(7) 1_555 1_555 1_555 yes Cl(1) Ru O(4) 84.5(2) 1_555 1_555 1_555 yes Cl(1) Ru C(41) 97.3(3) 1_555 1_555 1_555 yes Cl(2) Ru P(1) 89.97(7) 1_555 1_555 1_555 yes Cl(2) Ru P(2) 93.59(7) 1_555 1_555 1_555 yes Cl(2) Ru O(4) 84.4(2) 1_555 1_555 1_555 yes Cl(2) Ru C(41) 93.8(3) 1_555 1_555 1_555 yes P(1) Ru P(2) 176.44(8) 1_555 1_555 1_555 yes P(1) Ru O(4) 101.8(1) 1_555 1_555 1_555 yes P(1) Ru C(41) 89.0(2) 1_555 1_555 1_555 yes P(2) Ru O(4) 78.3(1) 1_555 1_555 1_555 yes P(2) Ru C(41) 91.0(2) 1_555 1_555 1_555 yes O(4) Ru C(41) 169.0(3) 1_555 1_555 1_555 yes Ru P(1) C(21) 116.1(3) 1_555 1_555 1_555 yes Ru P(1) C(27) 120.2(3) 1_555 1_555 1_555 yes Ru P(1) C(33) 112.4(2) 1_555 1_555 1_555 yes C(21) P(1) C(27) 98.0(3) 1_555 1_555 1_555 yes C(21) P(1) C(33) 104.0(4) 1_555 1_555 1_555 yes C(27) P(1) C(33) 103.9(4) 1_555 1_555 1_555 yes Ru P(2) C(1) 102.4(2) 1_555 1_555 1_555 yes Ru P(2) C(9) 119.0(3) 1_555 1_555 1_555 yes Ru P(2) C(15) 115.5(2) 1_555 1_555 1_555 yes C(1) P(2) C(9) 107.9(3) 1_555 1_555 1_555 yes C(1) P(2) C(15) 108.2(3) 1_555 1_555 1_555 yes C(9) P(2) C(15) 103.4(3) 1_555 1_555 1_555 yes C(34) O(2) C(39) 121.2(8) 1_555 1_555 1_555 yes C(38) O(3) C(40) 119.7(8) 1_555 1_555 1_555 yes Ru O(4) C(2) 117.3(4) 1_555 1_555 1_555 yes Ru O(4) C(7) 123.5(5) 1_555 1_555 1_555 yes C(2) O(4) C(7) 118.4(6) 1_555 1_555 1_555 yes C(6) O(5) C(8) 118.0(6) 1_555 1_555 1_555 yes P(2) C(1) C(2) 117.8(6) 1_555 1_555 1_555 yes P(2) C(1) C(6) 125.3(5) 1_555 1_555 1_555 yes C(2) C(1) C(6) 116.8(7) 1_555 1_555 1_555 yes O(4) C(2) C(1) 118.0(6) 1_555 1_555 1_555 yes O(4) C(2) C(3) 118.5(7) 1_555 1_555 1_555 yes C(1) C(2) C(3) 123.4(8) 1_555 1_555 1_555 yes C(2) C(3) C(4) 115.8(7) 1_555 1_555 1_555 yes C(2) C(3) H(1) 121.3(9) 1_555 1_555 1_555 no C(4) C(3) H(1) 122.9(8) 1_555 1_555 1_555 no C(3) C(4) C(5) 123.4(8) 1_555 1_555 1_555 yes C(3) C(4) H(2) 118.0(9) 1_555 1_555 1_555 no C(5) C(4) H(2) 118.6(9) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.5(8) 1_555 1_555 1_555 yes C(4) C(5) H(3) 121.4(8) 1_555 1_555 1_555 no C(6) C(5) H(3) 119.0(8) 1_555 1_555 1_555 no O(5) C(6) C(1) 116.3(6) 1_555 1_555 1_555 yes O(5) C(6) C(5) 122.9(8) 1_555 1_555 1_555 yes C(1) C(6) C(5) 120.8(7) 1_555 1_555 1_555 yes O(4) C(7) H(4) 110.0(7) 1_555 1_555 1_555 no O(4) C(7) H(5) 109.9(7) 1_555 1_555 1_555 no O(4) C(7) H(6) 111.6(9) 1_555 1_555 1_555 no H(4) C(7) H(5) 107(1) 1_555 1_555 1_555 no H(4) C(7) H(6) 108.7(8) 1_555 1_555 1_555 no H(5) C(7) H(6) 109.2(8) 1_555 1_555 1_555 no O(5) C(8) H(7) 111.0(8) 1_555 1_555 1_555 no O(5) C(8) H(8) 110.6(8) 1_555 1_555 1_555 no O(5) C(8) H(9) 109.6(8) 1_555 1_555 1_555 no H(7) C(8) H(8) 109.8(9) 1_555 1_555 1_555 no H(7) C(8) H(9) 108.1(8) 1_555 1_555 1_555 no H(8) C(8) H(9) 107.5(9) 1_555 1_555 1_555 no P(2) C(9) C(10) 123.5(6) 1_555 1_555 1_555 yes P(2) C(9) C(14) 117.9(6) 1_555 1_555 1_555 yes C(10) C(9) C(14) 118.4(7) 1_555 1_555 1_555 yes C(9) C(10) C(11) 120.1(8) 1_555 1_555 1_555 yes C(9) C(10) H(10) 119.2(7) 1_555 1_555 1_555 no C(11) C(10) H(10) 120.7(7) 1_555 1_555 1_555 no C(10) C(11) C(12) 121.4(8) 1_555 1_555 1_555 yes C(10) C(11) H(11) 119.8(9) 1_555 1_555 1_555 no C(12) C(11) H(11) 118.8(8) 1_555 1_555 1_555 no C(11) C(12) C(13) 119.2(8) 1_555 1_555 1_555 yes C(11) C(12) H(12) 121.8(9) 1_555 1_555 1_555 no C(13) C(12) H(12) 119.0(9) 1_555 1_555 1_555 no C(12) C(13) C(14) 120.7(8) 1_555 1_555 1_555 yes C(12) C(13) H(13) 119.3(8) 1_555 1_555 1_555 no C(14) C(13) H(13) 120.0(8) 1_555 1_555 1_555 no C(9) C(14) C(13) 120.1(7) 1_555 1_555 1_555 yes C(9) C(14) H(14) 119.8(7) 1_555 1_555 1_555 no C(13) C(14) H(14) 120.1(8) 1_555 1_555 1_555 no P(2) C(15) C(16) 123.0(5) 1_555 1_555 1_555 yes P(2) C(15) C(20) 121.2(6) 1_555 1_555 1_555 yes C(16) C(15) C(20) 115.7(7) 1_555 1_555 1_555 yes C(15) C(16) C(17) 122.3(7) 1_555 1_555 1_555 yes C(15) C(16) H(15) 118.5(7) 1_555 1_555 1_555 no C(17) C(16) H(15) 119.2(8) 1_555 1_555 1_555 no C(16) C(17) C(18) 121.0(8) 1_555 1_555 1_555 yes C(16) C(17) H(16) 120.5(8) 1_555 1_555 1_555 no C(18) C(17) H(16) 118.5(9) 1_555 1_555 1_555 no C(17) C(18) C(19) 118.0(8) 1_555 1_555 1_555 yes C(17) C(18) H(17) 121.4(10) 1_555 1_555 1_555 no C(19) C(18) H(17) 120.5(9) 1_555 1_555 1_555 no C(18) C(19) C(20) 120.5(8) 1_555 1_555 1_555 yes C(18) C(19) H(18) 120.6(9) 1_555 1_555 1_555 no C(20) C(19) H(18) 119.0(9) 1_555 1_555 1_555 no C(15) C(20) C(19) 122.4(8) 1_555 1_555 1_555 yes C(15) C(20) H(19) 118.4(8) 1_555 1_555 1_555 no C(19) C(20) H(19) 119.1(7) 1_555 1_555 1_555 no P(1) C(21) C(22) 122.0(6) 1_555 1_555 1_555 yes P(1) C(21) C(26) 119.9(6) 1_555 1_555 1_555 yes C(22) C(21) C(26) 118.0(7) 1_555 1_555 1_555 yes C(21) C(22) C(23) 122.1(8) 1_555 1_555 1_555 yes C(21) C(22) H(20) 119.0(8) 1_555 1_555 1_555 no C(23) C(22) H(20) 118.9(9) 1_555 1_555 1_555 no C(22) C(23) C(24) 119.8(9) 1_555 1_555 1_555 yes C(22) C(23) H(21) 121.2(10) 1_555 1_555 1_555 no C(24) C(23) H(21) 119.0(9) 1_555 1_555 1_555 no C(23) C(24) C(25) 118.7(8) 1_555 1_555 1_555 yes C(23) C(24) H(22) 120.0(10) 1_555 1_555 1_555 no C(25) C(24) H(22) 121.2(10) 1_555 1_555 1_555 no C(24) C(25) C(26) 121.4(9) 1_555 1_555 1_555 yes C(24) C(25) H(23) 117.9(9) 1_555 1_555 1_555 no C(26) C(25) H(23) 120(1) 1_555 1_555 1_555 no C(21) C(26) C(25) 120.0(8) 1_555 1_555 1_555 yes C(21) C(26) H(24) 119.3(8) 1_555 1_555 1_555 no C(25) C(26) H(24) 120.7(9) 1_555 1_555 1_555 no P(1) C(27) C(28) 117.7(6) 1_555 1_555 1_555 yes P(1) C(27) C(32) 122.6(6) 1_555 1_555 1_555 yes C(28) C(27) C(32) 119.6(7) 1_555 1_555 1_555 yes C(27) C(28) C(29) 118.6(9) 1_555 1_555 1_555 yes C(27) C(28) H(25) 119.6(8) 1_555 1_555 1_555 no C(29) C(28) H(25) 121.8(10) 1_555 1_555 1_555 no C(28) C(29) C(30) 121(1) 1_555 1_555 1_555 yes C(28) C(29) H(26) 119(1) 1_555 1_555 1_555 no C(30) C(29) H(26) 119.1(9) 1_555 1_555 1_555 no C(29) C(30) C(31) 121.1(9) 1_555 1_555 1_555 yes C(29) C(30) H(27) 119(1) 1_555 1_555 1_555 no C(31) C(30) H(27) 119(1) 1_555 1_555 1_555 no C(30) C(31) C(32) 118.1(9) 1_555 1_555 1_555 yes C(30) C(31) H(28) 121.0(10) 1_555 1_555 1_555 no C(32) C(31) H(28) 120(1) 1_555 1_555 1_555 no C(27) C(32) C(31) 120.8(9) 1_555 1_555 1_555 yes C(27) C(32) H(29) 119.1(7) 1_555 1_555 1_555 no C(31) C(32) H(29) 120.1(9) 1_555 1_555 1_555 no P(1) C(33) C(34) 120.7(6) 1_555 1_555 1_555 yes P(1) C(33) C(38) 122.6(6) 1_555 1_555 1_555 yes C(34) C(33) C(38) 116.3(8) 1_555 1_555 1_555 yes O(2) C(34) C(33) 114.8(7) 1_555 1_555 1_555 yes O(2) C(34) C(35) 124.4(7) 1_555 1_555 1_555 yes C(33) C(34) C(35) 120.7(8) 1_555 1_555 1_555 yes C(34) C(35) C(36) 120.1(9) 1_555 1_555 1_555 yes C(34) C(35) H(30) 119.3(9) 1_555 1_555 1_555 no C(36) C(35) H(30) 120.6(10) 1_555 1_555 1_555 no C(35) C(36) C(37) 122.9(9) 1_555 1_555 1_555 yes C(35) C(36) H(31) 117(1) 1_555 1_555 1_555 no C(37) C(36) H(31) 119.8(10) 1_555 1_555 1_555 no C(36) C(37) C(38) 116.5(9) 1_555 1_555 1_555 yes C(36) C(37) H(32) 121.6(10) 1_555 1_555 1_555 no C(38) C(37) H(32) 121.9(10) 1_555 1_555 1_555 no O(3) C(38) C(33) 115.7(8) 1_555 1_555 1_555 yes O(3) C(38) C(37) 121.4(8) 1_555 1_555 1_555 yes C(33) C(38) C(37) 122.8(9) 1_555 1_555 1_555 yes O(2) C(39) H(33) 112.9(10) 1_555 1_555 1_555 no O(2) C(39) H(34) 109.3(9) 1_555 1_555 1_555 no O(2) C(39) H(35) 110.0(9) 1_555 1_555 1_555 no H(33) C(39) H(34) 109(1) 1_555 1_555 1_555 no H(33) C(39) H(35) 109(1) 1_555 1_555 1_555 no H(34) C(39) H(35) 105(1) 1_555 1_555 1_555 no O(3) C(40) H(36) 112.3(9) 1_555 1_555 1_555 no O(3) C(40) H(37) 112.0(9) 1_555 1_555 1_555 no O(3) C(40) H(38) 109(1) 1_555 1_555 1_555 no H(36) C(40) H(37) 109(1) 1_555 1_555 1_555 no H(36) C(40) H(38) 106.2(10) 1_555 1_555 1_555 no H(37) C(40) H(38) 106(1) 1_555 1_555 1_555 no Ru C(41) O(1) 175.9(7) 1_555 1_555 1_555 yes Cl(3) C(42) Cl(4) 116.5(9) 1_555 1_555 1_555 yes Cl(3) C(42) H(39) 108(1) 1_555 1_555 1_555 no Cl(3) C(42) H(40) 109(1) 1_555 1_555 1_555 no Cl(4) C(42) H(39) 109(1) 1_555 1_555 1_555 no Cl(4) C(42) H(40) 106(1) 1_555 1_555 1_555 no H(39) C(42) H(40) 105(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(42) 3.34(2) 1_555 1_555 ? O(1) C(39) 3.37(1) 1_555 2_655 ? O(1) C(23) 3.39(1) 1_555 2_655 ? O(1) O(1) 3.55(1) 1_555 2_655 ? O(5) C(25) 3.565(10) 1_555 1_556 ? C(3) C(17) 3.57(1) 1_555 2_555 ? C(3) C(37) 3.59(1) 1_555 2_565 ? C(10) C(40) 3.29(1) 1_555 2_565 ? C(11) C(40) 3.56(1) 1_555 2_565 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;