# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1369 data_br442 _audit_creation_date 98-11-10 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common 'compound 5' #ActaC _chemical_formula_analytical C17_H2_O15_Ru5 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural Ru5(CO)15(CCH2) #ActaC _chemical_formula_sum C17_H2_O15_Ru5 #ActaC _chemical_formula_weight 951.54 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius Software' #ActaC _computing_cell_refinement 'Enraf-Nonius Software' #ActaC _computing_data_reduction xtal_ADDREF_ABSORB #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 21.312(2) #ActaC _cell_length_b 15.290(6) #ActaC _cell_length_c 14.8226(9) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 90.00000 #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 4830(2) #ActaC _cell_formula_units_Z 8 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 6 #ActaC _cell_measurement_theta_min 21.8 #ActaC _cell_measurement_theta_max 25.6 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M p_b_c_a #ActaC _symmetry_space_group_name_Hall -p_2ac_2ab #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _exptl_crystal_description needle #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour dark #ActaC _exptl_crystal_size_max 0.34 #ActaC _exptl_crystal_size_mid 0.12 #ActaC _exptl_crystal_size_min 0.12 #ActaC _exptl_crystal_density_diffrn 2.614 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 3543.63 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 3.13 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.67 #ActaC _exptl_absorpt_correction_T_max 0.73 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number 6 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 26 0 0 -26 0 0 0 16 0 0 -16 0 0 0 16 0 0 -16 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 4236 #ActaC _diffrn_reflns_av_R_equivalents ? #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 25 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 18 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 17 #ActaC _diffrn_reflns_theta_min 1.91 #ActaC _diffrn_reflns_theta_max 24.96 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 136 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 8 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 120 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 40 -1.42 .836 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru1 .61914(3) .41240(4) .78260(4) .0299(3) Uani ? ? Ru2 .50017(3) .48872(5) .75557(5) .0423(4) Uani ? ? Ru3 .60602(3) .54507(4) .65592(4) .0323(3) Uani ? ? Ru4 .71717(3) .44359(4) .65863(4) .0338(3) Uani ? ? Ru5 .69531(3) .56245(4) .79458(4) .0317(3) Uani ? ? C11 .6915(4) .3517(5) .8269(5) .041(5) Uani ? ? O11 .7278(3) .3110(4) .8643(4) .055(4) Uani ? ? C12 .5785(4) .3805(6) .8940(6) .049(5) Uani ? ? O12 .5603(3) .3609(5) .9620(4) .084(5) Uani ? ? C13 .5911(3) .3156(5) .7106(6) .044(5) Uani ? ? O13 .5745(3) .2594(4) .6666(4) .068(4) Uani ? ? C21 .4521(4) .4447(7) .8519(6) .065(6) Uani ? ? O21 .4239(3) .4208(5) .9113(5) .087(5) Uani ? ? C22 .4356(4) .5683(6) .7236(6) .059(6) Uani ? ? O22 .3973(3) .6159(5) .7046(5) .088(5) Uani ? ? C23 .4695(4) .4025(6) .6676(6) .054(6) Uani ? ? O23 .4474(3) .3543(5) .6203(5) .085(5) Uani ? ? C31 .5511(4) .6435(6) .6438(6) .059(6) Uani ? ? O31 .5240(3) .7068(4) .6370(5) .095(6) Uani ? ? C32 .6647(4) .6070(6) .5832(6) .048(5) Uani ? ? O32 .6928(3) .6533(4) .5383(4) .068(4) Uani ? ? C33 .5759(4) .4778(5) .5557(6) .045(5) Uani ? ? O33 .5586(3) .4384(4) .4966(4) .069(4) Uani ? ? C41 .7745(4) .5059(6) .5873(6) .047(5) Uani ? ? O41 .8106(3) .5419(4) .5454(5) .076(5) Uani ? ? C42 .7860(4) .3773(6) .6976(6) .054(6) Uani ? ? O42 .8280(3) .3373(5) .7201(5) .081(5) Uani ? ? C43 .6923(4) .3609(5) .5658(6) .048(5) Uani ? ? O43 .6806(3) .3124(5) .5115(5) .080(5) Uani ? ? C51 .7487(4) .6415(5) .7331(5) .040(4) Uani ? ? O51 .7808(3) .6897(4) .6978(4) .063(4) Uani ? ? C52 .7657(4) .5117(5) .8519(5) .044(5) Uani ? ? O52 .8088(3) .4842(4) .8877(4) .069(4) Uani ? ? C53 .6752(4) .6405(6) .8937(6) .050(5) Uani ? ? O53 .6642(3) .6840(5) .9530(5) .091(5) Uani ? ? C1 .5968(3) .5436(5) .7965(5) .035(4) Uani ? ? C2 .5459(4) .5811(6) .8471(7) .046(6) Uani ? ? H2a .537(3) .643(4) .832(4) .016(16) Uiso ? ? H2b .545(4) .567(5) .901(5) .06(3) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru1 .0291(3) .0321(3) .0287(3) -.0050(3) .0002(3) .0008(3) Ru2 .0250(3) .0594(4) .0425(3) -.0009(3) -.0001(3) -.0142(3) Ru3 .0325(3) .0347(3) .0297(3) .0062(3) -.0039(3) .0004(3) Ru4 .0290(3) .0381(3) .0344(3) .0027(3) .0048(3) -.0011(3) Ru5 .0300(3) .0328(3) .0324(3) -.0059(3) -.0028(3) -.0018(3) C11 .037(5) .046(5) .039(5) .001(4) .004(4) .001(4) O11 .054(4) .057(4) .055(4) .012(3) -.006(3) .020(3) C12 .043(5) .052(5) .051(6) -.001(4) .000(4) .006(4) O12 .072(5) .127(6) .053(4) -.019(4) .020(4) .024(4) C13 .041(5) .040(5) .051(5) .003(4) -.007(4) .004(4) O13 .072(4) .051(4) .081(5) -.011(3) -.026(4) -.015(4) C21 .032(5) .107(8) .055(6) -.019(5) .006(4) -.019(6) O21 .048(4) .144(7) .069(5) -.018(4) .013(4) .010(5) C22 .034(5) .081(7) .063(6) .006(5) -.004(4) -.035(5) O22 .045(4) .103(6) .115(6) .034(4) -.026(4) -.033(5) C23 .037(5) .067(6) .058(6) .000(4) -.005(4) -.020(5) O23 .070(5) .092(5) .094(5) -.016(4) -.013(4) -.047(5) C31 .065(6) .045(5) .066(6) .016(5) -.008(5) .005(5) O31 .090(5) .067(5) .130(7) .042(4) -.002(5) .022(5) C32 .053(6) .050(5) .043(5) .004(4) .001(4) .010(4) O32 .072(5) .067(4) .065(4) .003(4) .012(4) .028(4) C33 .037(4) .055(5) .041(5) .008(4) -.001(4) .000(4) O33 .075(4) .085(5) .046(4) .010(4) -.020(3) -.023(4) C41 .043(5) .050(5) .048(5) .006(4) .007(4) .005(4) O41 .069(5) .080(5) .079(5) -.002(4) .026(4) .023(4) C42 .042(5) .062(6) .058(6) -.003(5) .013(5) .018(5) O42 .045(4) .090(5) .108(6) .020(4) .004(4) .037(5) C43 .035(5) .046(5) .061(6) .008(4) .002(4) -.003(4) O43 .080(5) .087(5) .072(5) -.007(4) .001(4) -.037(4) C51 .049(5) .033(4) .039(5) -.007(4) -.009(4) -.001(4) O51 .075(4) .044(4) .070(4) -.019(3) .003(4) .013(3) C52 .048(5) .041(5) .043(5) -.016(4) -.007(4) .003(4) O52 .047(4) .086(5) .074(5) -.004(4) -.026(3) .018(4) C53 .044(5) .054(6) .053(6) -.018(4) -.001(4) -.016(5) O53 .093(6) .092(5) .086(5) -.034(4) .030(4) -.058(5) C1 .027(4) .045(4) .033(4) -.007(3) -.001(3) -.009(4) C2 .037(5) .054(6) .047(6) -.003(4) .002(4) -.011(5) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 4260(217) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 2983 #ActaC _refine_ls_number_parameters 343 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .052 #ActaC _refine_ls_R_factor_obs .031 #ActaC _refine_ls_wR_factor_all .035 #ActaC _refine_ls_wR_factor_obs .031 #ActaC _refine_ls_goodness_of_fit_all 1.151 #ActaC _refine_ls_goodness_of_fit_obs 1.21 #ActaC _refine_ls_shift/esd_max .05 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -.541 #ActaC _refine_diff_density_max .517 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru1 Ru2 2.8198(10) . . ? Ru1 Ru3 2.7783(10) . . ? Ru1 Ru4 2.8229(9) . . ? Ru1 Ru5 2.8161(11) . . ? Ru1 C11 1.915(8) . . ? Ru1 C12 1.927(9) . . ? Ru1 C13 1.920(8) . . ? Ru1 C1 2.072(7) . . ? Ru2 Ru3 2.8307(9) . . ? Ru2 C21 1.881(9) . . ? Ru2 C22 1.897(9) . . ? Ru2 C23 1.966(9) . . ? Ru2 C1 2.305(7) . . ? Ru2 C2 2.187(9) . . ? Ru3 Ru4 2.8321(10) . . ? Ru3 Ru5 2.8136(9) . . ? Ru3 C31 1.916(9) . . ? Ru3 C32 1.903(8) . . ? Ru3 C33 1.917(8) . . ? Ru3 C1 2.093(7) . . ? Ru4 Ru5 2.7533(10) . . ? Ru4 C41 1.875(8) . . ? Ru4 C42 1.873(9) . . ? Ru4 C43 1.942(9) . . ? Ru5 C51 1.893(8) . . ? Ru5 C52 1.891(8) . . ? Ru5 C53 1.941(9) . . ? Ru5 C1 2.119(6) . . ? C11 O11 1.138(9) . . ? C12 O12 1.121(11) . . ? C13 O13 1.136(10) . . ? C21 O21 1.128(11) . . ? C22 O22 1.129(11) . . ? C23 O23 1.120(11) . . ? C31 O31 1.131(11) . . ? C32 O32 1.142(10) . . ? C33 O33 1.126(10) . . ? C41 O41 1.132(10) . . ? C42 O42 1.136(11) . . ? C43 O43 1.123(11) . . ? C51 O51 1.134(10) . . ? C52 O52 1.141(10) . . ? C53 O53 1.126(11) . . ? C1 C2 1.438(11) . . ? C2 H2a .99(6) . . ? C2 H2b .83(8) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru2 Ru1 Ru3 60.74(2) . . . ? Ru2 Ru1 Ru4 120.20(3) . . . ? Ru2 Ru1 Ru5 100.96(3) . . . ? Ru2 Ru1 C11 166.6(2) . . . ? Ru2 Ru1 C12 79.8(2) . . . ? Ru2 Ru1 C13 87.7(2) . . . ? Ru2 Ru1 C1 53.63(18) . . . ? Ru3 Ru1 Ru4 60.74(2) . . . ? Ru3 Ru1 Ru5 60.38(3) . . . ? Ru3 Ru1 C11 131.8(2) . . . ? Ru3 Ru1 C12 135.9(2) . . . ? Ru3 Ru1 C13 99.0(2) . . . ? Ru3 Ru1 C1 48.5(2) . . . ? Ru4 Ru1 Ru5 58.45(2) . . . ? Ru4 Ru1 C11 73.1(2) . . . ? Ru4 Ru1 C12 158.9(2) . . . ? Ru4 Ru1 C13 89.9(2) . . . ? Ru4 Ru1 C1 94.08(19) . . . ? Ru5 Ru1 C11 84.8(2) . . . ? Ru5 Ru1 C12 114.3(3) . . . ? Ru5 Ru1 C13 147.4(2) . . . ? Ru5 Ru1 C1 48.50(18) . . . ? C11 Ru1 C12 86.9(3) . . . ? C11 Ru1 C13 93.9(3) . . . ? C11 Ru1 C1 128.3(3) . . . ? C12 Ru1 C13 98.1(4) . . . ? C12 Ru1 C1 93.2(3) . . . ? C13 Ru1 C1 136.9(3) . . . ? Ru1 Ru2 Ru3 58.90(2) . . . ? Ru1 Ru2 C21 103.5(3) . . . ? Ru1 Ru2 C22 162.4(3) . . . ? Ru1 Ru2 C23 96.6(2) . . . ? Ru1 Ru2 C1 46.36(18) . . . ? Ru1 Ru2 C2 77.2(2) . . . ? Ru3 Ru2 C21 159.8(3) . . . ? Ru3 Ru2 C22 104.6(3) . . . ? Ru3 Ru2 C23 97.0(2) . . . ? Ru3 Ru2 C1 46.73(17) . . . ? Ru3 Ru2 C2 76.8(2) . . . ? C21 Ru2 C22 91.4(4) . . . ? C21 Ru2 C23 94.8(4) . . . ? C21 Ru2 C1 114.6(3) . . . ? C21 Ru2 C2 90.2(4) . . . ? C22 Ru2 C23 91.3(4) . . . ? C22 Ru2 C1 118.7(3) . . . ? C22 Ru2 C2 93.7(4) . . . ? C23 Ru2 C1 135.7(3) . . . ? C23 Ru2 C2 172.9(3) . . . ? C1 Ru2 C2 37.2(3) . . . ? Ru1 Ru3 Ru2 60.35(2) . . . ? Ru1 Ru3 Ru4 60.41(2) . . . ? Ru1 Ru3 Ru5 60.47(2) . . . ? Ru1 Ru3 C31 134.3(3) . . . ? Ru1 Ru3 C32 132.8(3) . . . ? Ru1 Ru3 C33 99.5(2) . . . ? Ru1 Ru3 C1 47.8(2) . . . ? Ru2 Ru3 Ru4 119.50(3) . . . ? Ru2 Ru3 Ru5 100.76(3) . . . ? Ru2 Ru3 C31 78.5(3) . . . ? Ru2 Ru3 C32 166.1(3) . . . ? Ru2 Ru3 C33 88.5(2) . . . ? Ru2 Ru3 C1 53.32(18) . . . ? Ru4 Ru3 Ru5 58.37(2) . . . ? Ru4 Ru3 C31 160.6(3) . . . ? Ru4 Ru3 C32 74.4(3) . . . ? Ru4 Ru3 C33 89.8(2) . . . ? Ru4 Ru3 C1 93.35(18) . . . ? Ru5 Ru3 C31 114.1(3) . . . ? Ru5 Ru3 C32 85.6(3) . . . ? Ru5 Ru3 C33 147.5(2) . . . ? Ru5 Ru3 C1 48.48(18) . . . ? C31 Ru3 C32 87.5(4) . . . ? C31 Ru3 C33 98.3(4) . . . ? C31 Ru3 C1 92.6(3) . . . ? C32 Ru3 C33 92.7(3) . . . ? C32 Ru3 C1 129.1(3) . . . ? C33 Ru3 C1 137.2(3) . . . ? Ru1 Ru4 Ru3 58.85(2) . . . ? Ru1 Ru4 Ru5 60.65(3) . . . ? Ru1 Ru4 C41 159.2(3) . . . ? Ru1 Ru4 C42 106.7(3) . . . ? Ru1 Ru4 C43 98.6(2) . . . ? Ru3 Ru4 Ru5 60.48(2) . . . ? Ru3 Ru4 C41 105.0(3) . . . ? Ru3 Ru4 C42 162.8(3) . . . ? Ru3 Ru4 C43 96.8(2) . . . ? Ru5 Ru4 C41 100.8(3) . . . ? Ru5 Ru4 C42 105.3(3) . . . ? Ru5 Ru4 C43 154.4(2) . . . ? C41 Ru4 C42 86.5(4) . . . ? C41 Ru4 C43 96.3(4) . . . ? C42 Ru4 C43 94.6(4) . . . ? Ru1 Ru5 Ru3 59.14(2) . . . ? Ru1 Ru5 Ru4 60.90(3) . . . ? Ru1 Ru5 C51 146.7(2) . . . ? Ru1 Ru5 C52 98.7(2) . . . ? Ru1 Ru5 C53 114.9(2) . . . ? Ru1 Ru5 C1 47.1(2) . . . ? Ru3 Ru5 Ru4 61.15(2) . . . ? Ru3 Ru5 C51 96.6(2) . . . ? Ru3 Ru5 C52 145.7(2) . . . ? Ru3 Ru5 C53 117.5(2) . . . ? Ru3 Ru5 C1 47.70(19) . . . ? Ru4 Ru5 C51 88.1(2) . . . ? Ru4 Ru5 C52 85.6(2) . . . ? Ru4 Ru5 C53 175.8(3) . . . ? Ru4 Ru5 C1 95.0(2) . . . ? C51 Ru5 C52 90.1(3) . . . ? C51 Ru5 C53 96.0(3) . . . ? C51 Ru5 C1 133.5(3) . . . ? C52 Ru5 C53 95.0(3) . . . ? C52 Ru5 C1 136.4(3) . . . ? C53 Ru5 C1 81.7(3) . . . ? Ru1 C11 O11 168.4(7) . . . ? Ru1 C12 O12 173.6(7) . . . ? Ru1 C13 O13 178.7(7) . . . ? Ru2 C21 O21 177.6(9) . . . ? Ru2 C22 O22 179.8(9) . . . ? Ru2 C23 O23 174.4(7) . . . ? Ru3 C31 O31 173.0(8) . . . ? Ru3 C32 O32 169.6(7) . . . ? Ru3 C33 O33 179.5(7) . . . ? Ru4 C41 O41 177.7(7) . . . ? Ru4 C42 O42 179.2(8) . . . ? Ru4 C43 O43 177.0(7) . . . ? Ru5 C51 O51 178.7(7) . . . ? Ru5 C52 O52 177.4(7) . . . ? Ru5 C53 O53 178.0(8) . . . ? Ru1 C1 Ru2 80.0(2) . . . ? Ru1 C1 Ru3 83.7(3) . . . ? Ru1 C1 Ru5 84.4(2) . . . ? Ru1 C1 C2 127.7(6) . . . ? Ru2 C1 Ru3 80.0(2) . . . ? Ru2 C1 Ru5 158.6(4) . . . ? Ru2 C1 C2 66.9(4) . . . ? Ru3 C1 Ru5 83.8(2) . . . ? Ru3 C1 C2 125.8(6) . . . ? Ru5 C1 C2 134.5(6) . . . ? Ru2 C2 C1 75.9(5) . . . ? Ru2 C2 H2a 113(3) . . . ? Ru2 C2 H2b 114(6) . . . ? C1 C2 H2a 114(3) . . . ? C1 C2 H2b 115(6) . . . ? H2a C2 H2b 118(7) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _reflns_number_total 4236 #ActaC _reflns_number_observed 2992 #ActaC _reflns_observed_criterion refl_observed_if_Inet_>3.000_sigma(Inet) _reflns_d_resolution_high .842 _reflns_d_resolution_low 10.656 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_br431 _audit_creation_date 98-11-10 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common 'compound 1' #ActaC _chemical_formula_analytical C12_H2_O10_Ru3 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural Ru3(CO)10(C2H2) #ActaC _chemical_formula_sum C12_H2_O10_Ru3 #ActaC _chemical_formula_weight 609.35 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius Software' #ActaC _computing_cell_refinement 'Enraf-Nonius Software' #ActaC _computing_data_reduction xtal #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 9.6050(10) #ActaC _cell_length_b 9.516(3) #ActaC _cell_length_c 9.189(3) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 100.93(2) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 824.7(4) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 6 #ActaC _cell_measurement_theta_min 21.9 #ActaC _cell_measurement_theta_max 23.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21_1 #ActaC _symmetry_space_group_name_Hall P_2y1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,1/2+y,-z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour dark #ActaC _exptl_crystal_size_max 0.27 #ActaC _exptl_crystal_size_mid 0.17 #ActaC _exptl_crystal_size_min 0.05 #ActaC _exptl_crystal_density_diffrn 2.454 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 572 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 2.76 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.67 #ActaC _exptl_absorpt_correction_T_max 0.88 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/omega #ActaC _diffrn_standards_number 6 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 10 0 0 -10 0 0 0 10 0 0 -10 0 0 0 10 0 0 -10 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 4793 #ActaC _diffrn_reflns_av_R_equivalents .032 #ActaC _diffrn_reflns_av_sigmaI/netI .028 #ActaC _diffrn_reflns_limit_h_min -13 #ActaC _diffrn_reflns_limit_h_max 13 #ActaC _diffrn_reflns_limit_k_min -13 #ActaC _diffrn_reflns_limit_k_max 13 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 12 #ActaC _diffrn_reflns_theta_min 2.16 #ActaC _diffrn_reflns_theta_max 29.99 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 24 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 4 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 6 -1.42 .836 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 20 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru1 .69656(6) .00000 .87011(6) .0317(3) Uani ? ? Ru2 .75588(7) .28146(9) .79781(7) .0331(3) Uani ? ? Ru3 .90359(6) .06335(9) .71004(6) .0324(3) Uani ? ? C11 .7377(10) -.1638(11) .7666(10) .044(5) Uani ? ? O11 .7481(8) -.2745(7) .7186(8) .064(4) Uani ? ? C12 .6742(9) -.1037(9) 1.0429(10) .044(5) Uani ? ? O12 .6653(8) -.1660(8) 1.1459(7) .074(5) Uani ? ? C13 .5018(9) -.0088(10) .7571(9) .045(4) Uani ? ? O13 .3904(7) -.0111(10) .6900(8) .076(5) Uani ? ? C14 .6462(9) .1713(8) .9795(9) .041(4) Uani ? ? O14 .5973(7) .2185(7) 1.0732(7) .060(4) Uani ? ? C21 .7228(10) .4369(9) .9208(11) .046(5) Uani ? ? O21 .7067(8) .5284(7) .9942(8) .069(5) Uani ? ? C22 .8580(11) .3965(9) .6870(11) .052(5) Uani ? ? O22 .9213(9) .4703(8) .6295(9) .080(5) Uani ? ? C23 .5833(10) .3007(11) .6476(10) .051(5) Uani ? ? O23 .4873(8) .3045(11) .5573(8) .092(6) Uani ? ? C31 1.0492(10) .1644(9) .6451(10) .043(4) Uani ? ? O31 1.1354(7) .2249(8) .6012(8) .065(4) Uani ? ? C32 1.0129(10) -.1055(10) .7095(10) .049(5) Uani ? ? O32 1.0816(7) -.2003(8) .7088(8) .069(4) Uani ? ? C33 .7900(9) .0595(11) .5135(9) .047(4) Uani ? ? O33 .7193(8) .0588(9) .4016(7) .074(4) Uani ? ? C1 .9129(7) .0484(8) .9521(7) .034(3) Uani ? ? C2 .9337(8) .1905(8) .9196(8) .033(4) Uani ? ? H1 .98533 -.01570 1.00191 .04300 Uiso ? ? H2 1.02213 .23995 .95214 .04100 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru1 .0334(3) .0301(3) .0324(3) -.0005(3) .0080(2) .0029(3) Ru2 .0391(3) .0272(3) .0343(3) .0037(3) .0103(3) .0026(3) Ru3 .0335(3) .0353(3) .0302(3) .0011(3) .0108(2) -.0046(3) C11 .049(5) .044(5) .038(5) -.007(4) .010(4) -.002(4) O11 .085(5) .040(4) .071(5) -.008(4) .027(4) -.012(4) C12 .046(5) .044(5) .045(5) -.010(4) .016(4) -.004(4) O12 .091(6) .086(6) .044(4) -.012(4) .013(4) .024(4) C13 .049(5) .046(5) .041(5) .001(5) .009(4) .004(4) O13 .048(4) .104(6) .068(5) -.004(4) -.007(4) -.007(5) C14 .044(5) .032(4) .046(5) .002(4) .006(4) -.000(4) O14 .082(5) .049(4) .061(4) .009(3) .045(4) .001(3) C21 .053(5) .038(5) .053(5) .006(4) .026(5) .007(4) O21 .097(5) .042(5) .079(5) .005(4) .047(4) -.011(3) C22 .077(7) .037(5) .050(5) .005(5) .033(5) .004(4) O22 .118(7) .051(5) .091(5) .007(4) .072(5) .020(4) C23 .054(5) .053(6) .047(5) .011(5) .009(4) .011(5) O23 .067(5) .132(8) .066(5) .019(5) -.014(4) .031(5) C31 .052(5) .036(4) .045(5) .003(4) .018(4) -.008(4) O31 .060(4) .073(5) .067(5) -.017(4) .026(4) -.013(4) C32 .052(5) .049(5) .053(5) .005(4) .026(5) -.010(4) O32 .070(5) .054(4) .088(5) .020(4) .025(4) -.007(4) C33 .052(5) .051(5) .041(5) -.008(5) .016(4) .002(5) O33 .083(5) .090(5) .043(4) -.020(5) -.007(3) -.006(4) C1 .037(4) .042(4) .023(3) .004(3) .004(3) .006(3) C2 .033(4) .035(4) .032(4) -.003(3) .011(3) -.005(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment noref #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 943(172) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 2097 #ActaC _refine_ls_number_parameters 226 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .04 #ActaC _refine_ls_R_factor_obs .03 #ActaC _refine_ls_wR_factor_all .03 #ActaC _refine_ls_wR_factor_obs .029 #ActaC _refine_ls_goodness_of_fit_all 1.466 #ActaC _refine_ls_goodness_of_fit_obs 1.534 #ActaC _refine_ls_shift/esd_max .059 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -1.176 #ActaC _refine_diff_density_max .581 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru1 Ru2 2.8431(12) . . ? Ru1 Ru3 2.7550(10) . . ? Ru1 C11 1.906(10) . . ? Ru1 C12 1.916(9) . . ? Ru1 C13 1.962(8) . . ? Ru1 C14 2.021(8) . . ? Ru1 C1 2.122(7) . . ? Ru1 C2 2.879(7) . . ? Ru2 Ru3 2.7212(12) . . ? Ru2 C14 2.380(9) . . ? Ru2 C21 1.924(10) . . ? Ru2 C22 1.891(11) . . ? Ru2 C23 1.955(8) . . ? Ru2 C1 2.897(7) . . ? Ru2 C2 2.048(7) . . ? Ru3 C11 2.792(10) . . ? Ru3 C31 1.885(9) . . ? Ru3 C32 1.920(9) . . ? Ru3 C33 1.925(8) . . ? Ru3 C1 2.213(7) . . ? Ru3 C2 2.246(7) . . ? C11 O11 1.153(12) . . ? C12 O12 1.134(12) . . ? C13 O13 1.129(10) . . ? C14 O14 1.148(12) . . ? C21 O21 1.130(12) . . ? C22 O22 1.124(13) . . ? C23 O23 1.118(11) . . ? C31 O31 1.144(12) . . ? C32 O32 1.119(12) . . ? C33 O33 1.120(10) . . ? C1 C2 1.407(11) . . ? C1 H1 .972(7) . . ? C2 H2 .967(7) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru1 O11 3.044(7) . . ? Ru1 O12 3.049(7) . . ? Ru1 O13 3.090(6) . . ? Ru1 O14 3.064(7) . . ? Ru1 C23 3.565(10) . . ? Ru1 C32 3.757(10) . . ? Ru1 C33 3.603(9) . . ? Ru1 H1 2.8121(6) . . ? Ru2 C13 3.658(10) . . ? Ru2 O14 3.247(7) . . ? Ru2 O21 3.053(7) . . ? Ru2 O22 3.013(9) . . ? Ru2 O23 3.070(7) . . ? Ru2 C31 3.556(10) . . ? Ru2 C33 3.424(9) . . ? Ru2 H1 3.3995(8) . 2_757 ? Ru2 H2 2.7077(7) . . ? Ru3 O11 3.552(7) . . ? Ru3 C22 3.202(9) . . ? Ru3 C23 3.772(10) . . ? Ru3 O31 3.028(7) . . ? Ru3 O32 3.037(7) . . ? Ru3 O33 3.044(6) . . ? Ru3 H1 2.7526(10) . . ? Ru3 H2 2.8477(9) . . ? C11 C12 2.781(14) . . ? C11 C13 2.691(14) . . ? C11 C32 2.845(14) . . ? C11 C1 2.954(12) . . ? C12 C13 2.967(12) . . ? C12 C14 2.683(12) . . ? C12 C1 2.963(12) . . ? O12 O31 2.908(9) . 2_747 ? C13 C14 2.822(12) . . ? C14 C21 2.715(12) . . ? C14 C1 2.871(11) . . ? C14 C2 2.922(12) . . ? O14 C21 2.894(12) . . ? C21 C22 2.740(15) . . ? C21 C23 2.916(13) . . ? C22 C23 2.750(14) . . ? C22 C31 2.945(13) . . ? C22 C2 2.890(12) . . ? C31 C32 2.673(13) . . ? C31 C33 2.741(12) . . ? C31 C2 2.952(12) . . ? C32 C33 2.972(12) . . ? C32 C1 2.975(12) . . ? C1 H2 2.103(8) . . ? C2 H1 2.128(7) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru2 Ru1 Ru3 58.14(2) . . . ? Ru2 Ru1 C11 125.7(3) . . . ? Ru2 Ru1 C12 137.6(3) . . . ? Ru2 Ru1 C13 97.5(3) . . . ? Ru2 Ru1 C14 55.5(3) . . . ? Ru2 Ru1 C1 69.7(2) . . . ? Ru2 Ru1 C2 41.93(14) . . . ? Ru3 Ru1 C11 70.9(3) . . . ? Ru3 Ru1 C12 139.6(3) . . . ? Ru3 Ru1 C13 116.0(3) . . . ? Ru3 Ru1 C14 110.7(3) . . . ? Ru3 Ru1 C1 52.02(18) . . . ? Ru3 Ru1 C2 46.93(16) . . . ? C11 Ru1 C12 93.4(4) . . . ? C11 Ru1 C13 88.1(4) . . . ? C11 Ru1 C14 178.1(4) . . . ? C11 Ru1 C1 94.2(3) . . . ? C11 Ru1 C2 111.2(3) . . . ? C12 Ru1 C13 99.8(4) . . . ? C12 Ru1 C14 85.9(4) . . . ? C12 Ru1 C1 94.2(3) . . . ? C12 Ru1 C2 113.8(3) . . . ? C13 Ru1 C14 90.2(4) . . . ? C13 Ru1 C1 165.6(3) . . . ? C13 Ru1 C2 139.2(3) . . . ? C14 Ru1 C1 87.7(3) . . . ? C14 Ru1 C2 70.8(3) . . . ? C1 Ru1 C2 27.8(3) . . . ? Ru1 Ru2 Ru3 59.31(3) . . . ? Ru1 Ru2 C14 44.4(2) . . . ? Ru1 Ru2 C21 121.6(3) . . . ? Ru1 Ru2 C22 145.0(3) . . . ? Ru1 Ru2 C23 94.2(3) . . . ? Ru1 Ru2 C1 43.39(15) . . . ? Ru1 Ru2 C2 70.0(2) . . . ? Ru3 Ru2 C14 101.4(2) . . . ? Ru3 Ru2 C21 156.0(3) . . . ? Ru3 Ru2 C22 86.0(3) . . . ? Ru3 Ru2 C23 106.4(3) . . . ? Ru3 Ru2 C1 46.27(14) . . . ? Ru3 Ru2 C2 54.0(2) . . . ? C14 Ru2 C21 77.4(4) . . . ? C14 Ru2 C22 167.6(3) . . . ? C14 Ru2 C23 96.2(4) . . . ? C14 Ru2 C1 65.1(2) . . . ? C14 Ru2 C2 82.2(3) . . . ? C21 Ru2 C22 91.8(4) . . . ? C21 Ru2 C23 97.5(4) . . . ? C21 Ru2 C1 115.4(3) . . . ? C21 Ru2 C2 102.5(3) . . . ? C22 Ru2 C23 91.3(4) . . . ? C22 Ru2 C1 115.6(3) . . . ? C22 Ru2 C2 94.3(4) . . . ? C23 Ru2 C1 135.3(3) . . . ? C23 Ru2 C2 159.0(4) . . . ? C1 Ru2 C2 26.6(3) . . . ? Ru1 Ru3 Ru2 62.55(3) . . . ? Ru1 Ru3 C11 40.2(2) . . . ? Ru1 Ru3 C31 159.2(3) . . . ? Ru1 Ru3 C32 105.6(3) . . . ? Ru1 Ru3 C33 99.1(3) . . . ? Ru1 Ru3 C1 49.11(18) . . . ? Ru1 Ru3 C2 69.4(2) . . . ? Ru2 Ru3 C11 100.8(2) . . . ? Ru2 Ru3 C31 99.5(3) . . . ? Ru2 Ru3 C32 162.8(3) . . . ? Ru2 Ru3 C33 93.3(3) . . . ? Ru2 Ru3 C1 71.0(2) . . . ? Ru2 Ru3 C2 47.51(18) . . . ? C11 Ru3 C31 159.7(3) . . . ? C11 Ru3 C32 71.6(4) . . . ? C11 Ru3 C33 85.3(3) . . . ? C11 Ru3 C1 71.3(3) . . . ? C11 Ru3 C2 104.1(3) . . . ? C31 Ru3 C32 89.3(4) . . . ? C31 Ru3 C33 92.0(4) . . . ? C31 Ru3 C1 117.4(3) . . . ? C31 Ru3 C2 90.8(3) . . . ? C32 Ru3 C33 101.2(4) . . . ? C32 Ru3 C1 91.8(4) . . . ? C32 Ru3 C2 118.1(3) . . . ? C33 Ru3 C1 148.1(3) . . . ? C33 Ru3 C2 140.6(3) . . . ? C1 Ru3 C2 36.8(3) . . . ? Ru1 C11 Ru3 68.9(3) . . . ? Ru1 C11 O11 168.1(9) . . . ? Ru3 C11 O11 122.8(7) . . . ? Ru1 C12 O12 177.9(8) . . . ? Ru1 C13 O13 178.3(9) . . . ? Ru1 C14 Ru2 80.0(3) . . . ? Ru1 C14 O14 149.2(7) . . . ? Ru2 C14 O14 130.7(6) . . . ? Ru2 C21 O21 178.4(8) . . . ? Ru2 C22 O22 175.3(8) . . . ? Ru2 C23 O23 175.6(9) . . . ? Ru3 C31 O31 177.9(7) . . . ? Ru3 C32 O32 176.9(9) . . . ? Ru3 C33 O33 177.1(9) . . . ? Ru1 C1 Ru2 66.96(18) . . . ? Ru1 C1 Ru3 78.9(2) . . . ? Ru1 C1 C2 107.6(5) . . . ? Ru1 C1 H1 126.6(6) . . . ? Ru2 C1 Ru3 62.68(17) . . . ? Ru2 C1 C2 40.7(3) . . . ? Ru2 C1 H1 166.1(6) . . . ? Ru3 C1 C2 72.9(4) . . . ? Ru3 C1 H1 113.8(5) . . . ? C2 C1 H1 125.8(7) . . . ? Ru1 C2 Ru2 68.1(2) . . . ? Ru1 C2 Ru3 63.63(17) . . . ? Ru1 C2 C1 44.6(3) . . . ? Ru1 C2 H2 167.7(6) . . . ? Ru2 C2 Ru3 78.5(2) . . . ? Ru2 C2 C1 112.6(5) . . . ? Ru2 C2 H2 123.8(6) . . . ? Ru3 C2 C1 70.3(4) . . . ? Ru3 C2 H2 119.3(6) . . . ? C1 C2 H2 123.6(7) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_total 2533 #ActaC _reflns_number_observed 2097 #ActaC _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 9.431 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 2.0984 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_br430 _audit_creation_date 98-11-10 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common 'compound 2' #ActaC _chemical_formula_analytical C11_H2_O9_Ru3 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural Ru3(mu-H)(CO)9(C2H) #ActaC _chemical_formula_sum C11_H2_O9_Ru3 #ActaC _chemical_formula_weight 581.3 #Acta5 _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius Software' #ActaC _computing_cell_refinement 'Enraf-Nonius Software' #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 13.099(4) #ActaC _cell_length_b 15.619(4) #ActaC _cell_length_c 16.345(4) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 105.86(2) #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 3216.8(15) #ActaC _cell_formula_units_Z 8 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 6 #ActaC _cell_measurement_theta_min 15.8 #ActaC _cell_measurement_theta_max 21.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M p_1_21/c_1 #ActaC _symmetry_space_group_name_Hall -P_-2ybc #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z +x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z _exptl_crystal_description plate #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour dark #ActaC _exptl_crystal_size_max 0.24 #ActaC _exptl_crystal_size_mid 0.18 #ActaC _exptl_crystal_size_min 0.10 #ActaC _exptl_crystal_density_diffrn 2.401 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 2176 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 2.82 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.63 #ActaC _exptl_absorpt_correction_T_max 0.73 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/omega #ActaC _diffrn_standards_number 6 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 12 0 0 -12 0 0 0 12 0 0 -12 0 0 0 16 0 0 -16 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 7376 #ActaC _diffrn_reflns_av_R_equivalents ? #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 17 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 20 #ActaC _diffrn_reflns_limit_l_min -21 #ActaC _diffrn_reflns_limit_l_max 20 #ActaC _diffrn_reflns_theta_min 1.62 #ActaC _diffrn_reflns_theta_max 27.5 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 88 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 16 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 24 -1.42 .836 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 72 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru11 .33937(5) .15021(4) .81150(4) .0377(3) Uani ? ? Ru12 .36303(5) .31485(4) .75274(4) .0361(3) Uani ? ? Ru13 .17478(5) .26954(4) .79292(4) .0355(3) Uani ? ? C111 .2493(7) .0526(5) .7990(5) .057(5) Uani ? ? O111 .1955(6) -.0052(4) .7908(5) .095(5) Uani ? ? C112 .4597(7) .0837(5) .8047(6) .061(5) Uani ? ? O112 .5281(5) .0419(4) .7988(5) .099(5) Uani ? ? C113 .3527(7) .1542(5) .9309(5) .054(5) Uani ? ? O113 .3639(6) .1592(5) 1.0018(4) .090(5) Uani ? ? C121 .4971(6) .3230(5) .7251(5) .056(5) Uani ? ? O121 .5744(5) .3287(5) .7087(5) .098(5) Uani ? ? C122 .2945(7) .4008(5) .6740(5) .054(5) Uani ? ? O122 .2538(5) .4530(4) .6296(4) .079(4) Uani ? ? C123 .3931(6) .3962(5) .8445(5) .050(4) Uani ? ? O123 .4160(5) .4421(4) .8989(4) .075(4) Uani ? ? C131 .0810(6) .3567(6) .7382(5) .051(5) Uani ? ? O131 .0241(5) .4081(4) .7015(4) .074(4) Uani ? ? C132 .0643(6) .1936(5) .8041(5) .056(5) Uani ? ? O132 -.0033(5) .1491(4) .8068(4) .083(4) Uani ? ? C133 .2007(6) .3201(5) .9022(5) .049(4) Uani ? ? O133 .2203(5) .3537(4) .9671(3) .076(4) Uani ? ? C11 .3094(6) .1957(5) .6776(4) .043(4) Uani ? ? C12 .2318(5) .2211(4) .7052(4) .036(4) Uani ? ? Ru21 -.27122(5) .16029(4) .54921(4) .0394(3) Uani ? ? Ru22 -.23624(5) .32654(4) .50065(4) .0360(3) Uani ? ? Ru23 -.07721(5) .20260(4) .51650(4) .0364(3) Uani ? ? C211 -.2114(7) .0749(5) .6299(6) .065(5) Uani ? ? O211 -.1765(6) .0239(4) .6784(5) .104(5) Uani ? ? C212 -.4093(7) .1563(6) .5727(6) .064(5) Uani ? ? O212 -.4890(6) .1545(5) .5846(5) .104(5) Uani ? ? C213 -.2975(7) .0817(5) .4569(5) .060(5) Uani ? ? O213 -.3169(5) .0362(4) .3999(4) .091(5) Uani ? ? C221 -.3527(7) .3950(5) .5120(5) .056(5) Uani ? ? O221 -.4194(5) .4375(5) .5214(5) .098(5) Uani ? ? C222 -.1422(6) .4225(5) .5240(5) .049(4) Uani ? ? O222 -.0887(5) .4806(4) .5363(4) .080(4) Uani ? ? C223 -.2513(6) .3337(5) .3815(5) .051(4) Uani ? ? O223 -.2609(6) .3354(5) .3107(4) .087(5) Uani ? ? C231 .0384(6) .2756(5) .5160(4) .045(4) Uani ? ? O231 .1071(4) .3202(4) .5178(4) .068(4) Uani ? ? C232 .0083(7) .1065(5) .5630(5) .059(5) Uani ? ? O232 .0583(6) .0505(4) .5939(4) .097(5) Uani ? ? C233 -.1017(6) .1674(5) .4003(5) .051(4) Uani ? ? O233 -.1225(5) .1474(4) .3306(4) .080(4) Uani ? ? C21 -.2154(6) .2744(5) .6311(4) .043(4) Uani ? ? C22 -.1359(5) .2474(4) .6043(4) .037(4) Uani ? ? H11 .323(4) .170(4) .637(3) .026(16) Uiso ? ? H1 .431(5) .238(4) .833(4) .05(2) Uiso ? ? H21 -.243(6) .297(5) .674(5) .07(3) Uiso ? ? H2 -.329(6) .238(5) .471(5) .08(3) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru11 .0411(3) .0310(3) .0392(3) .0027(3) .0081(3) .0019(3) Ru12 .0372(3) .0324(3) .0396(3) -.0017(3) .0121(3) .0013(3) Ru13 .0335(3) .0369(3) .0360(3) .0006(3) .0090(2) -.0006(3) C111 .061(6) .045(5) .061(6) .003(4) .010(5) .008(4) O111 .113(6) .057(4) .109(6) -.037(4) .020(5) .004(4) C112 .056(5) .038(5) .080(6) .012(4) .001(5) -.004(4) O112 .076(5) .076(5) .143(7) .034(4) .024(5) -.021(5) C113 .064(6) .044(5) .049(5) .004(4) .008(4) .003(4) O113 .115(6) .114(6) .038(4) .023(5) .016(4) .010(4) C121 .050(5) .055(5) .070(6) -.010(4) .025(5) -.006(5) O121 .065(4) .107(6) .141(7) -.008(4) .058(5) -.008(5) C122 .061(5) .047(5) .046(5) -.010(4) .003(4) -.001(4) O122 .088(5) .058(4) .075(5) -.005(4) -.006(4) .024(3) C123 .040(4) .045(5) .062(5) -.003(4) .007(4) .002(4) O123 .082(5) .061(4) .075(4) -.006(4) .008(4) -.033(3) C131 .043(5) .068(6) .041(5) .001(4) .008(4) -.005(4) O131 .070(4) .056(4) .081(4) .021(3) -.005(3) -.000(3) C132 .050(5) .060(6) .056(5) -.006(4) .012(4) -.005(4) O132 .071(4) .081(5) .102(5) -.034(4) .035(4) -.007(4) C133 .049(5) .059(5) .040(4) -.000(4) .013(4) -.001(4) O133 .099(5) .084(5) .047(4) -.011(4) .022(4) -.018(3) C11 .053(5) .037(4) .037(4) -.001(4) .010(4) -.003(3) C12 .043(4) .031(4) .032(4) .001(3) .006(3) -.002(3) Ru21 .0425(4) .0326(3) .0429(4) -.0041(3) .0114(3) -.0002(3) Ru22 .0402(3) .0304(3) .0358(3) .0045(3) .0076(3) .0028(3) Ru23 .0372(3) .0344(3) .0372(3) .0039(3) .0097(3) -.0010(3) C211 .061(6) .048(5) .074(6) -.016(5) -.001(5) -.001(5) O211 .127(7) .058(4) .104(6) -.012(4) -.007(5) .030(4) C212 .063(6) .057(6) .076(6) -.014(5) .024(5) -.013(5) O212 .078(5) .110(6) .146(7) -.018(5) .067(5) -.018(5) C213 .065(6) .051(5) .064(6) .001(5) .014(5) -.001(4) O213 .090(5) .088(5) .089(5) -.017(4) .018(4) -.045(4) C221 .058(5) .045(5) .058(5) .005(4) .002(4) -.004(4) O221 .065(5) .089(5) .130(6) .035(4) .012(4) -.019(5) C222 .049(5) .049(5) .046(5) .002(4) .009(4) .014(4) O222 .082(5) .060(4) .088(5) -.029(4) .006(4) .010(4) C223 .060(5) .035(4) .055(5) .003(4) .011(4) .011(4) O223 .122(6) .100(6) .042(4) .015(5) .025(4) .010(4) C231 .042(4) .059(5) .038(4) .011(4) .015(3) -.004(4) O231 .054(4) .080(5) .071(4) -.020(3) .019(3) -.010(4) C232 .059(5) .054(5) .060(6) .006(4) .011(4) -.006(4) O232 .106(6) .062(5) .105(6) .037(4) .001(5) .013(4) C233 .045(5) .048(5) .059(5) .004(4) .011(4) .003(4) O233 .110(6) .082(5) .048(4) -.004(4) .019(4) -.016(3) C21 .055(5) .039(4) .036(4) -.002(4) .011(4) .003(3) C22 .042(4) .030(4) .034(4) -.004(3) .003(3) .005(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight_atomblock_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type atomblock #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 2886(163) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 4552 #ActaC _refine_ls_number_parameters 433 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .069 #ActaC _refine_ls_R_factor_obs .037 #ActaC _refine_ls_wR_factor_all .044 #ActaC _refine_ls_wR_factor_obs .036 #ActaC _refine_ls_goodness_of_fit_all 1.148 #ActaC _refine_ls_goodness_of_fit_obs 1.231 #ActaC _refine_ls_shift/esd_max .05 #ActaC _refine_ls_shift/esd_mean .003 #ActaC _refine_diff_density_min -.647 #ActaC _refine_diff_density_max .665 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru21 Ru22 2.7895(11) . . ? Ru21 Ru23 2.8148(12) . . ? Ru21 C211 1.889(8) . . ? Ru21 C212 1.951(10) . . ? Ru21 C213 1.902(9) . . ? Ru21 C21 2.229(7) . . ? Ru21 C22 2.221(6) . . ? Ru21 H2 1.78(7) . . ? Ru22 Ru23 2.8034(10) . . ? Ru22 C221 1.913(9) . . ? Ru22 C222 1.911(8) . . ? Ru22 C223 1.906(8) . . ? Ru22 C21 2.228(7) . . ? Ru22 C22 2.216(6) . . ? Ru22 H2 1.81(7) . . ? Ru23 C231 1.898(8) . . ? Ru23 C232 1.902(8) . . ? Ru23 C233 1.918(8) . . ? Ru23 C22 1.935(8) . . ? C211 O211 1.128(11) . . ? C212 O212 1.113(13) . . ? C213 O213 1.143(11) . . ? C221 O221 1.140(11) . . ? C222 O222 1.131(10) . . ? C223 O223 1.130(10) . . ? C231 O231 1.133(10) . . ? C232 O232 1.127(10) . . ? C233 O233 1.141(10) . . ? C21 C22 1.306(11) . . ? C21 H21 .94(8) . . ? Ru11 Ru12 2.7918(11) . . ? Ru11 Ru13 2.8029(10) . . ? Ru11 C111 1.905(8) . . ? Ru11 C112 1.916(9) . . ? Ru11 C113 1.913(8) . . ? Ru11 C11 2.232(7) . . ? Ru11 C12 2.213(6) . . ? Ru11 H1 1.79(6) . . ? Ru12 Ru13 2.8102(12) . . ? Ru12 C121 1.934(9) . . ? Ru12 C122 1.906(8) . . ? Ru12 C123 1.923(8) . . ? Ru12 C11 2.235(7) . . ? Ru12 C12 2.230(7) . . ? Ru12 H1 1.82(6) . . ? Ru13 C131 1.887(8) . . ? Ru13 C132 1.918(9) . . ? Ru13 C133 1.897(8) . . ? Ru13 C12 1.942(8) . . ? C111 O111 1.130(11) . . ? C112 O112 1.134(11) . . ? C113 O113 1.129(10) . . ? C121 O121 1.119(12) . . ? C122 O122 1.124(10) . . ? C123 O123 1.117(10) . . ? C131 O131 1.147(10) . . ? C132 O132 1.137(11) . . ? C133 O133 1.147(10) . . ? C11 C12 1.284(11) . . ? C11 H11 .83(6) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru11 O111 3.035(7) . . ? Ru11 O112 3.049(7) . . ? Ru11 O113 3.041(6) . . ? Ru11 C121 3.891(9) . . ? Ru11 C132 3.635(9) . . ? Ru11 C133 3.743(9) . . ? Ru11 H11 2.81(6) . . ? Ru12 C112 3.843(8) . . ? Ru12 C113 3.875(8) . . ? Ru12 O121 3.053(8) . . ? Ru12 O122 3.029(6) . . ? Ru12 O123 3.038(6) . . ? Ru12 C131 3.694(8) . . ? Ru12 C133 3.651(9) . . ? Ru12 H11 2.90(5) . . ? Ru13 C111 3.521(8) . . ? Ru13 C113 3.300(7) . . ? Ru13 C122 3.478(9) . . ? Ru13 C123 3.389(8) . . ? Ru13 O131 3.033(6) . . ? Ru13 O132 3.053(7) . . ? Ru13 O133 3.043(6) . . ? Ru13 C11 3.133(8) . . ? Ru13 H1 3.28(6) . . ? C111 C112 2.775(13) . . ? C111 C113 2.721(11) . . ? O111 O233 2.957(9) . 3_556 ? C112 H1 2.49(6) . . ? C113 H1 2.50(7) . . ? C121 C122 2.830(11) . . ? C121 C123 2.903(13) . . ? C122 C123 2.734(11) . . ? C131 C132 2.798(12) . . ? C131 C133 2.771(10) . . ? O131 O211 2.995(9) . 4_556 ? O131 O222 2.928(8) . . ? C132 C133 2.847(11) . . ? C12 H11 2.01(6) . . ? Ru21 O211 3.017(7) . . ? Ru21 O212 3.063(8) . . ? Ru21 O213 3.045(7) . . ? Ru21 C221 3.820(8) . . ? Ru21 C232 3.703(9) . . ? Ru21 C233 3.717(9) . . ? Ru21 H21 2.91(7) . . ? Ru22 C212 3.880(10) . . ? Ru22 O221 3.053(7) . . ? Ru22 O222 3.042(6) . . ? Ru22 O223 3.036(6) . . ? Ru22 C231 3.626(8) . . ? Ru22 C233 3.681(9) . . ? Ru22 H21 2.89(8) . . ? Ru23 C211 3.505(10) . . ? Ru23 C213 3.363(8) . . ? Ru23 C222 3.548(8) . . ? Ru23 C223 3.393(7) . . ? Ru23 O231 3.030(6) . . ? Ru23 O232 3.028(7) . . ? Ru23 O233 3.057(6) . . ? Ru23 C21 3.146(8) . . ? Ru23 H2 3.22(7) . . ? C211 C212 2.809(12) . . ? C211 C213 2.745(12) . . ? C211 C22 2.939(11) . . ? C212 C213 2.933(14) . . ? C213 H2 2.50(8) . . ? C221 C222 2.744(12) . . ? C221 C223 2.963(13) . . ? C221 C21 2.942(10) . . ? O221 O221 2.821(9) . 3_466 ? C222 C223 2.751(10) . . ? O222 O222 2.947(10) . 3_566 ? C223 H2 2.49(8) . . ? C231 C232 2.808(12) . . ? C231 C233 2.812(10) . . ? C232 C233 2.821(11) . . ? C22 H21 2.17(8) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru22 Ru21 Ru23 60.03(2) . . . ? Ru22 Ru21 C211 141.9(2) . . . ? Ru22 Ru21 C212 108.6(3) . . . ? Ru22 Ru21 C213 112.5(3) . . . ? Ru22 Ru21 C21 51.24(19) . . . ? Ru22 Ru21 C22 50.97(16) . . . ? Ru22 Ru21 H2 39(2) . . . ? Ru23 Ru21 C211 94.3(3) . . . ? Ru23 Ru21 C212 168.2(3) . . . ? Ru23 Ru21 C213 88.7(3) . . . ? Ru23 Ru21 C21 76.2(2) . . . ? Ru23 Ru21 C22 43.2(2) . . . ? Ru23 Ru21 H2 86(3) . . . ? C211 Ru21 C212 94.0(4) . . . ? C211 Ru21 C213 92.8(4) . . . ? C211 Ru21 C21 98.1(3) . . . ? C211 Ru21 C22 90.9(3) . . . ? C211 Ru21 H2 178(2) . . . ? C212 Ru21 C213 99.2(4) . . . ? C212 Ru21 C21 94.4(3) . . . ? C212 Ru21 C22 128.3(3) . . . ? C212 Ru21 H2 86(3) . . . ? C213 Ru21 C21 162.0(4) . . . ? C213 Ru21 C22 131.9(3) . . . ? C213 Ru21 H2 86(2) . . . ? C21 Ru21 C22 34.1(3) . . . ? C21 Ru21 H2 84(2) . . . ? C22 Ru21 H2 90(2) . . . ? Ru21 Ru22 Ru23 60.44(3) . . . ? Ru21 Ru22 C221 107.2(3) . . . ? Ru21 Ru22 C222 145.1(2) . . . ? Ru21 Ru22 C223 111.5(2) . . . ? Ru21 Ru22 C21 51.27(18) . . . ? Ru21 Ru22 C22 51.12(17) . . . ? Ru21 Ru22 H2 38(2) . . . ? Ru23 Ru22 C221 165.7(3) . . . ? Ru23 Ru22 C222 95.8(2) . . . ? Ru23 Ru22 C223 90.1(2) . . . ? Ru23 Ru22 C21 76.5(2) . . . ? Ru23 Ru22 C22 43.4(2) . . . ? Ru23 Ru22 H2 86(2) . . . ? C221 Ru22 C222 91.7(3) . . . ? C221 Ru22 C223 101.8(3) . . . ? C221 Ru22 C21 90.2(3) . . . ? C221 Ru22 C22 124.0(3) . . . ? C221 Ru22 H2 88(3) . . . ? C222 Ru22 C223 92.2(3) . . . ? C222 Ru22 C21 101.1(3) . . . ? C222 Ru22 C22 94.0(3) . . . ? C222 Ru22 H2 176(2) . . . ? C223 Ru22 C21 161.9(3) . . . ? C223 Ru22 C22 133.5(3) . . . ? C223 Ru22 H2 84(2) . . . ? C21 Ru22 C22 34.2(3) . . . ? C21 Ru22 H2 83(2) . . . ? C22 Ru22 H2 90(2) . . . ? Ru21 Ru23 Ru22 59.54(3) . . . ? Ru21 Ru23 C231 154.8(2) . . . ? Ru21 Ru23 C232 101.7(3) . . . ? Ru21 Ru23 C233 101.8(2) . . . ? Ru21 Ru23 C22 51.8(2) . . . ? Ru22 Ru23 C231 99.1(2) . . . ? Ru22 Ru23 C232 157.4(3) . . . ? Ru22 Ru23 C233 100.8(2) . . . ? Ru22 Ru23 C22 51.92(18) . . . ? C231 Ru23 C232 95.3(4) . . . ? C231 Ru23 C233 94.9(3) . . . ? C231 Ru23 C22 105.4(3) . . . ? C232 Ru23 C233 95.2(4) . . . ? C232 Ru23 C22 107.4(3) . . . ? C233 Ru23 C22 147.7(3) . . . ? Ru21 C211 O211 179.3(9) . . . ? Ru21 C212 O212 178.7(8) . . . ? Ru21 C213 O213 177.2(7) . . . ? Ru22 C221 O221 177.3(7) . . . ? Ru22 C222 O222 178.1(6) . . . ? Ru22 C223 O223 178.0(7) . . . ? Ru23 C231 O231 178.0(7) . . . ? Ru23 C232 O232 177.0(8) . . . ? Ru23 C233 O233 176.0(7) . . . ? Ru21 C21 Ru22 77.5(2) . . . ? Ru21 C21 C22 72.6(4) . . . ? Ru21 C21 H21 128(5) . . . ? Ru22 C21 C22 72.4(4) . . . ? Ru22 C21 H21 127(4) . . . ? C22 C21 H21 151(4) . . . ? Ru21 C22 Ru22 77.9(2) . . . ? Ru21 C22 Ru23 85.0(2) . . . ? Ru21 C22 C21 73.3(4) . . . ? Ru22 C22 Ru23 84.7(3) . . . ? Ru22 C22 C21 73.4(4) . . . ? Ru23 C22 C21 151.7(5) . . . ? Ru21 H2 Ru22 102(3) . . . ? Ru12 Ru11 Ru13 60.30(3) . . . ? Ru12 Ru11 C111 145.5(2) . . . ? Ru12 Ru11 C112 108.0(3) . . . ? Ru12 Ru11 C113 109.5(2) . . . ? Ru12 Ru11 C11 51.38(18) . . . ? Ru12 Ru11 C12 51.34(17) . . . ? Ru12 Ru11 H1 39.7(18) . . . ? Ru13 Ru11 C111 94.9(3) . . . ? Ru13 Ru11 C112 167.1(3) . . . ? Ru13 Ru11 C113 86.7(2) . . . ? Ru13 Ru11 C11 76.0(2) . . . ? Ru13 Ru11 C12 43.6(2) . . . ? Ru13 Ru11 H1 88(2) . . . ? C111 Ru11 C112 93.2(4) . . . ? C111 Ru11 C113 90.9(4) . . . ? C111 Ru11 C11 102.2(3) . . . ? C111 Ru11 C12 94.2(3) . . . ? C111 Ru11 H1 174.6(19) . . . ? C112 Ru11 C113 103.3(4) . . . ? C112 Ru11 C11 92.4(3) . . . ? C112 Ru11 C12 125.7(3) . . . ? C112 Ru11 H1 85(2) . . . ? C113 Ru11 C11 158.9(3) . . . ? C113 Ru11 C12 130.2(3) . . . ? C113 Ru11 H1 85(2) . . . ? C11 Ru11 C12 33.6(3) . . . ? C11 Ru11 H1 83(2) . . . ? C12 Ru11 H1 91.1(18) . . . ? Ru11 Ru12 Ru13 60.04(2) . . . ? Ru11 Ru12 C121 109.5(3) . . . ? Ru11 Ru12 C122 143.6(2) . . . ? Ru11 Ru12 C123 111.0(2) . . . ? Ru11 Ru12 C11 51.26(19) . . . ? Ru11 Ru12 C12 50.79(16) . . . ? Ru11 Ru12 H1 39(2) . . . ? Ru13 Ru12 C121 169.2(3) . . . ? Ru13 Ru12 C122 93.1(3) . . . ? Ru13 Ru12 C123 89.4(3) . . . ? Ru13 Ru12 C11 75.8(2) . . . ? Ru13 Ru12 C12 43.4(2) . . . ? Ru13 Ru12 H1 87(2) . . . ? C121 Ru12 C122 95.0(4) . . . ? C121 Ru12 C123 97.7(4) . . . ? C121 Ru12 C11 95.5(3) . . . ? C121 Ru12 C12 128.6(3) . . . ? C121 Ru12 H1 85(2) . . . ? C122 Ru12 C123 91.1(3) . . . ? C122 Ru12 C11 101.3(3) . . . ? C122 Ru12 C12 92.9(3) . . . ? C122 Ru12 H1 177(2) . . . ? C123 Ru12 C11 161.0(3) . . . ? C123 Ru12 C12 132.8(3) . . . ? C123 Ru12 H1 86(2) . . . ? C11 Ru12 C12 33.4(3) . . . ? C11 Ru12 H1 82.0(19) . . . ? C12 Ru12 H1 90(2) . . . ? Ru11 Ru13 Ru12 59.65(3) . . . ? Ru11 Ru13 C131 155.9(3) . . . ? Ru11 Ru13 C132 99.0(3) . . . ? Ru11 Ru13 C133 103.9(2) . . . ? Ru11 Ru13 C12 51.80(18) . . . ? Ru12 Ru13 C131 101.9(3) . . . ? Ru12 Ru13 C132 155.6(3) . . . ? Ru12 Ru13 C133 99.9(3) . . . ? Ru12 Ru13 C12 52.2(2) . . . ? C131 Ru13 C132 94.7(3) . . . ? C131 Ru13 C133 94.1(3) . . . ? C131 Ru13 C12 105.2(3) . . . ? C132 Ru13 C133 96.5(4) . . . ? C132 Ru13 C12 106.4(3) . . . ? C133 Ru13 C12 148.4(3) . . . ? Ru11 C111 O111 179.3(7) . . . ? Ru11 C112 O112 177.1(7) . . . ? Ru11 C113 O113 177.0(8) . . . ? Ru12 C121 O121 179.1(8) . . . ? Ru12 C122 O122 177.9(8) . . . ? Ru12 C123 O123 176.4(7) . . . ? Ru13 C131 O131 177.0(7) . . . ? Ru13 C132 O132 176.8(7) . . . ? Ru13 C133 O133 176.2(8) . . . ? Ru11 C11 Ru12 77.4(2) . . . ? Ru11 C11 C12 72.4(4) . . . ? Ru11 C11 H11 127(4) . . . ? Ru12 C11 C12 73.1(4) . . . ? Ru12 C11 H11 137(4) . . . ? C12 C11 H11 142(4) . . . ? Ru11 C12 Ru12 77.9(2) . . . ? Ru11 C12 Ru13 84.6(2) . . . ? Ru11 C12 C11 74.0(4) . . . ? Ru12 C12 Ru13 84.4(2) . . . ? Ru12 C12 C11 73.5(4) . . . ? Ru13 C12 C11 151.9(5) . . . ? Ru11 H1 Ru12 101(3) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -21 _reflns_limit_l_max 20 _reflns_number_total 7376 #ActaC _reflns_number_observed 4552 #ActaC _reflns_observed_criterion refl_observed_if_I_>3.000_sigma(I) _reflns_d_resolution_high .77 _reflns_d_resolution_low 12.6 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 5.9274 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_br432 _audit_creation_date 98-11-10 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common 'compound 4' #ActaC _chemical_formula_analytical C14_H2_O12_Ru4 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural Ru4(CO)12(C2H2) #ActaC _chemical_formula_sum C14_H2_O12_Ru4 #ActaC _chemical_formula_weight 766.5 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius software' #ActaC _computing_cell_refinement 'Enraf-Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ADDREF_ABSORB_SORTRF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 9.5580(10) #ActaC _cell_length_b 9.5580(10) #ActaC _cell_length_c 19.203(3) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 90.00000 #ActaC _cell_angle_gamma 120.0000 #ActaC _cell_volume 1519.3(4) #ActaC _cell_formula_units_Z 3 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 5 #ActaC _cell_measurement_theta_min 28.1 #ActaC _cell_measurement_theta_max 29.9 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting hexagonal #ActaC _symmetry_space_group_name_H-M p_62 #ActaC _symmetry_space_group_name_Hall p_62 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,+z -y,+x-y,2/3+z +y,-x+y,2/3+z -x+y,-x,1/3+z +x- y,+x,1/3+z _exptl_crystal_description rod #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour dark #ActaC _exptl_crystal_size_max 0.40 #ActaC _exptl_crystal_size_mid 0.21 #ActaC _exptl_crystal_size_min 0.18 #ActaC _exptl_crystal_density_diffrn 2.513 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 1074 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 2.98 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.75 #ActaC _exptl_absorpt_correction_T_max 0.78 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number 5 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 0 0 27 0 0 -27 11 0 0 -11 0 0 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 3427 #ActaC _diffrn_reflns_av_R_equivalents .03 #ActaC _diffrn_reflns_av_sigmaI/netI .027 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 11 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 11 #ActaC _diffrn_reflns_limit_l_min -26 #ActaC _diffrn_reflns_limit_l_max 26 #ActaC _diffrn_reflns_theta_min 2.46 #ActaC _diffrn_reflns_theta_max 29.99 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 42 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 6 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 12 -1.42 .836 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 36 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru1 .89482(4) .56176(5) .5606(2) .03587(17) Uani ? ? Ru2 .81960(4) .27959(4) .4905(2) .03619(17) Uani ? ? C11 .9881(7) .6575(7) .6492(3) .055(3) Uani ? ? O11 1.0469(6) .7145(7) .7008(3) .085(3) Uani ? ? C12 .8265(8) .7123(9) .5375(4) .066(4) Uani ? ? O12 .7915(9) .8059(8) .5238(3) .109(4) Uani ? ? C13 .6925(7) .4119(8) .5999(4) .061(3) Uani ? ? O13 .5698(6) .3341(6) .6256(3) .102(3) Uani ? ? C21 .6139(7) .2304(7) .4546(4) .052(3) Uani ? ? O21 .4920(6) .2048(7) .4342(3) .090(3) Uani ? ? C22 .7325(7) .1221(7) .5627(4) .050(3) Uani ? ? O22 .6781(6) .0289(6) .6056(3) .074(2) Uani ? ? C23 .8404(7) .1369(7) .4289(4) .056(3) Uani ? ? O23 .8563(6) .0562(5) .3899(3) .084(3) Uani ? ? C1 .9437(6) .5314(6) .4559(3) .035(2) Uani ? ? H1 .896(7) .565(7) .4128(13) .08(2) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru1 .03226(19) .0400(2) .03536(19) .01806(18) .00167(16) - .00319(16) Ru2 .0337(2) .0325(2) .03772(19) .01304(16) -.00343(16) - .00133(16) C11 .040(3) .062(3) .053(3) .019(3) .006(3) -.008(3) O11 .064(3) .113(4) .054(2) .028(3) -.006(2) -.034(3) C12 .081(5) .084(5) .061(4) .062(4) .013(3) .008(3) O12 .166(6) .126(5) .100(4) .122(5) -.000(4) .001(3) C13 .047(3) .066(4) .057(3) .017(3) .009(3) -.016(3) O13 .061(3) .093(4) .100(4) -.001(3) .040(3) -.023(3) C21 .048(3) .048(3) .049(3) .017(3) -.008(3) -.003(3) O21 .051(3) .118(5) .086(3) .031(3) -.017(3) .011(3) C22 .049(3) .047(3) .053(3) .023(3) -.005(3) -.000(3) O22 .073(3) .066(3) .064(3) .020(2) .005(2) .023(2) C23 .050(3) .045(3) .062(4) .016(3) .006(3) .001(3) O23 .099(4) .056(3) .089(3) .032(3) .024(3) -.018(2) C1 .035(2) .037(2) .032(2) .016(2) -.0036(19) .0019(18) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 3499(251) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 1360 #ActaC _refine_ls_number_parameters 140 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .025 #ActaC _refine_ls_R_factor_obs .021 #ActaC _refine_ls_wR_factor_all .02 #ActaC _refine_ls_wR_factor_obs .019 #ActaC _refine_ls_goodness_of_fit_all 1.251 #ActaC _refine_ls_goodness_of_fit_obs 1.24 #ActaC _refine_ls_shift/esd_max .099 #ActaC _refine_ls_shift/esd_mean .004 #ActaC _refine_diff_density_min -.355 #ActaC _refine_diff_density_max .329 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru1 Ru2 2.769(3) . . ? Ru1 C11 1.926(7) . . ? Ru1 C12 1.906(7) . . ? Ru1 C13 1.895(7) . . ? Ru1 C1 2.117(7) . . ? Ru1 Ru1 2.7947(6) . 2_765 ? Ru1 Ru2 2.725(3) . 2_765 ? Ru2 C21 1.907(6) . . ? Ru2 C22 1.906(7) . . ? Ru2 C23 1.889(7) . . ? Ru2 C1 2.188(5) . . ? Ru2 C1 2.176(5) . 2_765 ? C11 O11 1.135(8) . . ? C12 O12 1.132(10) . . ? C13 O13 1.140(8) . . ? C21 O21 1.134(8) . . ? C22 O22 1.130(9) . . ? C23 O23 1.138(8) . . ? C1 H1 1.07(4) . . ? C1 C1 1.472(6) . 2_765 ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru1 C11 3.299(6) . 2_765 ? Ru1 O11 3.061(6) . . ? Ru1 O12 3.037(7) . . ? Ru1 C13 3.899(6) . 2_765 ? Ru1 O13 3.031(5) . . ? Ru1 C21 3.589(7) . . ? Ru1 C22 3.326(6) . 2_765 ? Ru1 C22 3.681(6) . . ? Ru1 C23 3.716(7) . 2_765 ? Ru1 C1 2.932(6) . 2_765 ? Ru1 H1 2.84(2) . . ? Ru2 Ru2 3.8878(6) . 2_765 ? Ru2 C11 3.454(7) . 2_765 ? Ru2 C12 3.465(7) . 2_765 ? Ru2 C13 3.005(7) . . ? Ru2 O13 3.735(6) . . ? Ru2 O21 3.040(5) . . ? Ru2 O22 3.036(6) . . ? Ru2 O23 3.026(6) . . ? Ru2 H1 2.87(5) . . ? Ru2 H1 2.79(5) . 2_765 ? C11 C12 2.841(9) . . ? C11 C13 2.786(9) . . ? C11 C22 2.950(8) . 2_765 ? C12 C13 2.764(10) . . ? C12 C1 2.939(8) . . ? C21 C22 2.800(9) . . ? C21 C23 2.768(8) . . ? C22 C23 2.746(10) . . ? C23 C1 2.834(7) . 2_765 ? C1 H1 2.30(6) . 2_765 ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru2 Ru1 C11 136.5(3) . . . ? Ru2 Ru1 C12 127.0(3) . . . ? Ru2 Ru1 C13 77.7(2) . . . ? Ru2 Ru1 C1 51.11(16) . . . ? Ru2 Ru1 Ru1 58.65(6) . . 2_765 ? Ru2 Ru1 Ru2 90.08(11) . . 2_765 ? C11 Ru1 C12 95.7(3) . . . ? C11 Ru1 C13 93.6(3) . . . ? C11 Ru1 C1 145.4(2) . . . ? C11 Ru1 Ru1 86.6(3) . . 2_765 ? C11 Ru1 Ru2 94.32(18) . . 2_765 ? C12 Ru1 C13 93.3(3) . . . ? C12 Ru1 C1 93.7(3) . . . ? C12 Ru1 Ru1 155.4(2) . . 2_765 ? C12 Ru1 Ru2 95.2(2) . . 2_765 ? C13 Ru1 C1 119.1(3) . . . ? C13 Ru1 Ru1 111.0(3) . . 2_765 ? C13 Ru1 Ru2 167.7(3) . . 2_765 ? C1 Ru1 Ru1 71.8(2) . . 2_765 ? C1 Ru1 Ru2 51.57(14) . . 2_765 ? Ru1 Ru1 Ru2 60.20(6) 2_765 . 2_765 ? Ru1 Ru2 C21 98.6(2) . . . ? Ru1 Ru2 C22 102.3(3) . . . ? Ru1 Ru2 C23 159.71(18) . . . ? Ru1 Ru2 C1 48.87(16) . . . ? Ru1 Ru2 Ru1 61.15(6) . . 2_765 ? Ru1 Ru2 C1 71.60(16) . . 2_765 ? C21 Ru2 C22 94.5(3) . . . ? C21 Ru2 C23 93.7(3) . . . ? C21 Ru2 C1 95.0(2) . . . ? C21 Ru2 Ru1 159.7(2) . . 2_765 ? C21 Ru2 C1 127.6(3) . . 2_765 ? C22 Ru2 C23 92.7(3) . . . ? C22 Ru2 C1 150.8(3) . . . ? C22 Ru2 Ru1 90.0(2) . . 2_765 ? C22 Ru2 C1 137.8(3) . . 2_765 ? C23 Ru2 C1 114.2(3) . . . ? C23 Ru2 Ru1 105.9(2) . . 2_765 ? C23 Ru2 C1 88.1(2) . . 2_765 ? C1 Ru2 Ru1 72.35(15) . . 2_765 ? C1 Ru2 C1 39.4(2) . . 2_765 ? Ru1 Ru2 C1 49.66(16) 2_765 . 2_765 ? Ru1 C11 O11 178.2(6) . . . ? Ru1 C12 O12 177.5(6) . . . ? Ru1 C13 O13 173.5(7) . . . ? Ru2 C21 O21 178.1(7) . . . ? Ru2 C22 O22 178.7(7) . . . ? Ru2 C23 O23 177.1(6) . . . ? Ru1 C1 Ru2 80.0(2) . . . ? Ru1 C1 H1 122(4) . . . ? Ru1 C1 Ru2 78.8(2) . . 2_765 ? Ru1 C1 C1 108.2(4) . . 2_765 ? Ru2 C1 H1 119(3) . . . ? Ru2 C1 Ru2 126.0(3) . . 2_765 ? Ru2 C1 C1 69.8(3) . . 2_765 ? H1 C1 Ru2 114(3) . . 2_765 ? H1 C1 C1 129(4) . . 2_765 ? Ru2 C1 C1 70.7(2) 2_765 . 2_765 ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_number_total 1526 #ActaC _reflns_number_observed 1360 #ActaC _reflns_observed_criterion refl_observed_if_I____>_3.00_sigma(I___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 8.264 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 2.198 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? ------------------------------------- data_br511 _audit_creation_date 98-11-11 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common 'compound 7' #ActaC _chemical_formula_analytical C21_H6_Cl2_O16_Ru6 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural Ru6(CO)16(C2H2)2.CH2Cl2 #ActaC _chemical_formula_sum C21_H6_Cl2_O16_Ru6 #ActaC _chemical_formula_weight 1191.59 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf-Nonius software' #ActaC _computing_cell_refinement 'Enraf-Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 9.470(5) #ActaC _cell_length_b 9.470(5) #ActaC _cell_length_c 35.094(8) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 90.00000 #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 3147(3) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 4 #ActaC _cell_measurement_theta_min 21.5 #ActaC _cell_measurement_theta_max 21.5 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting tetragonal #ActaC _symmetry_space_group_name_H-M p_41_21_2 #ActaC _symmetry_space_group_name_Hall p_43n_2nw #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2+x,1/2-y,3/4-z -x,-y,1/2+z 1/2-x,1/2+y,1/4-z +y,+x,-z 1/2+y,1/2-x,3/4+z 1/2-y,1/2+x,1/4+z -y,-x,1/2-z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation block _exptl_crystal_colour dark #ActaC _exptl_crystal_size_max 0.32 #ActaC _exptl_crystal_size_mid 0.20 #ActaC _exptl_crystal_size_min 0.16 #ActaC _exptl_crystal_density_diffrn 2.515 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 2232 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 3.05 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.55 #ActaC _exptl_absorpt_correction_T_max 0.63 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'sealed tube' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 2theta/theta #ActaC _diffrn_standards_number 4 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 6 6 18 6 6 -18 -6 -6 -18 -6 -6 18 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 5215 #ActaC _diffrn_reflns_av_R_equivalents .027 #ActaC _diffrn_reflns_av_sigmaI/netI .026 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 13 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 13 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 49 #ActaC _diffrn_reflns_theta_min 2.23 #ActaC _diffrn_reflns_theta_max 29.98 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 84 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 64 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ru ? 0 24 -1.42 .836 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 8 .132 .159 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 24 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru1 .49794(7) .48565(7) .656840(10) .0447(3) Uani ? ? Ru2 .56161(7) .59905(6) .72709(2) .0396(3) Uani ? ? Ru3 .53613(7) .29133(6) .71752(2) .0411(3) Uani ? ? C11 .4569(9) .6582(9) .6311(2) .053(5) Uani ? ? O11 .4289(8) .7625(7) .61784(17) .081(5) Uani ? ? C12 .4276(10) .3751(10) .6161(2) .061(6) Uani ? ? O12 .3791(8) .3111(8) .59209(16) .091(5) Uani ? ? C13 .6916(10) .4712(12) .6398(2) .067(6) Uani ? ? O13 .8019(7) .4627(9) .62852(18) .092(5) Uani ? ? C21 .4628(10) .7645(9) .7225(2) .058(5) Uani ? ? O21 .3972(8) .8679(7) .72066(19) .098(6) Uani ? ? C22 .7099(11) .6861(11) .6990(2) .070(6) Uani ? ? O22 .7970(9) .7375(9) .68228(18) .110(6) Uani ? ? C31 .5414(10) .1572(9) .7586(2) .059(5) Uani ? ? O31 .5411(9) .0663(6) .77985(15) .089(5) Uani ? ? C32 .4262(10) .1791(9) .6845(2) .057(5) Uani ? ? O32 .3586(8) .1104(7) .66576(17) .086(5) Uani ? ? C33 .7039(10) .2213(10) .6950(2) .059(5) Uani ? ? O33 .8025(8) .1783(9) .68109(19) .098(6) Uani ? ? C1 .3969(7) .4661(7) .71244(18) .039(4) Uani ? ? C2 .2904(9) .4926(11) .6863(2) .051(5) Uani ? ? Cl .4153(4) .6133(5) .51513(12) .168(4) Uani ? ? C0 .4477(15) .4477(15) .50000 .165(14) Uani ? ? H2a .233(8) .426(7) .6813(17) .04(2) Uiso ? ? H2b .252(8) .581(7) .6846(18) .04(2) Uiso ? ? H0 .42548 .38217 .52050 .24000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru1 .0448(3) .0531(4) .0362(3) -.0003(3) -.0006(3) .0040(3) Ru2 .0408(3) .0404(3) .0377(3) -.0057(3) -.0016(3) .0051(3) Ru3 .0465(4) .0389(3) .0380(3) .0025(3) -.0006(3) -.0022(3) C11 .048(5) .064(6) .047(4) .004(5) -.001(4) .009(4) O11 .078(5) .078(5) .088(4) .001(4) -.009(4) .029(4) C12 .071(7) .068(6) .045(4) -.008(5) .010(5) -.003(4) O12 .113(6) .102(6) .057(4) -.031(5) -.007(4) -.027(4) C13 .065(6) .091(8) .045(4) .001(6) .012(4) .009(5) O13 .060(4) .132(7) .084(4) .010(5) .015(4) .012(5) C21 .065(6) .045(5) .064(5) -.005(5) -.007(5) .003(4) O21 .129(7) .054(4) .112(5) .022(5) -.040(5) .007(4) C22 .067(6) .077(7) .064(5) -.019(6) .003(5) .017(5) O22 .095(6) .139(8) .096(5) -.059(6) .028(5) .026(5) C31 .078(6) .054(5) .046(5) .003(6) -.003(5) -.008(4) O31 .149(7) .058(4) .060(4) -.011(5) -.010(5) .020(3) C32 .075(7) .046(5) .050(5) .001(5) -.010(5) .003(4) O32 .108(6) .070(5) .079(4) -.021(4) -.029(4) -.012(4) C33 .060(6) .064(6) .054(5) .003(5) -.001(5) -.011(5) O33 .065(5) .124(7) .104(5) .029(5) .010(4) -.039(5) C1 .038(4) .038(4) .042(4) .003(3) .008(3) .000(3) C2 .042(5) .064(6) .047(4) .002(6) -.008(4) -.005(4) Cl .124(3) .201(5) .179(4) .012(3) -.002(3) -.046(4) C0 .197(15) .197(15) .101(13) -.08(2) .062(12) -.062(12) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details ? _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type block #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method ? #ActaC _refine_ls_extinction_coef 0 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 1986 #ActaC _refine_ls_number_parameters 213 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all 0.050 #ActaC _refine_ls_R_factor_obs 0.033 #ActaC _refine_ls_wR_factor_all 0.032 #ActaC _refine_ls_wR_factor_obs 0.029 #ActaC _refine_ls_goodness_of_fit_all 1.371 #ActaC _refine_ls_goodness_of_fit_obs 1.455 #ActaC _refine_ls_shift/esd_max 0.0547 #ActaC _refine_ls_shift/esd_mean 0.00195 #ActaC _refine_diff_density_min -0.040 #ActaC _refine_diff_density_max 0.060 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru1 Ru2 2.7559(10) . . ? Ru1 Ru3 2.8376(11) . . ? Ru1 C11 1.908(8) . . ? Ru1 C12 1.893(8) . . ? Ru1 C13 1.933(9) . . ? Ru1 C1 2.181(6) . . ? Ru1 C2 2.222(9) . . ? Ru2 Ru3 2.9433(17) . . ? Ru2 C21 1.832(8) . . ? Ru2 C22 1.904(10) . . ? Ru2 C1 2.069(7) . . ? Ru2 Ru2 2.6861(11) . 8_666 ? Ru2 Ru3 2.7124(11) . 8_666 ? Ru2 C1 2.139(6) . 8_666 ? Ru3 C31 1.921(8) . . ? Ru3 C32 1.887(9) . . ? Ru3 C33 1.895(9) . . ? Ru3 C1 2.124(7) . . ? Ru3 Ru3 3.2460(12) . 8_666 ? C11 O11 1.123(11) . . ? C12 O12 1.135(10) . . ? C13 O13 1.120(11) . . ? C21 O21 1.161(11) . . ? C22 O22 1.122(12) . . ? C31 O31 1.140(10) . . ? C32 O32 1.124(11) . . ? C33 O33 1.129(12) . . ? C1 C2 1.386(11) . . ? C2 H2a .85(7) . . ? C2 H2b .91(7) . . ? Cl C0 1.684(14) . . ? C0 H0 .973(9) . . ? C0 H0 .973(9) . 5_556 ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru1 Ru2 4.1995(12) . 8_666 ? Ru1 O11 3.029(7) . . ? Ru1 O12 3.027(6) . . ? Ru1 O13 3.053(7) . . ? Ru1 C21 3.521(8) . . ? Ru1 C22 3.133(10) . . ? Ru1 C32 3.136(9) . . ? Ru1 C33 3.445(9) . . ? Ru1 H2a 2.71(7) . . ? Ru1 H2b 2.68(7) . . ? Ru2 C11 3.556(8) . . ? Ru2 C13 3.515(8) . . ? Ru2 O21 2.993(7) . . ? Ru2 O22 3.027(8) . . ? Ru2 C31 3.019(9) . 8_666 ? Ru2 C2 3.108(9) . . ? Ru2 C2 3.255(8) . 8_666 ? Ru2 Cl 4.497(5) . 7_655 ? Ru2 H2a 3.59(6) . 8_666 ? Ru2 H2a 3.87(7) . . ? Ru2 H2b 3.30(7) . . ? Ru2 H2b 3.66(7) . 8_666 ? Ru3 C13 3.536(9) . . ? Ru3 C31 3.413(9) . 8_666 ? Ru3 O31 3.054(6) . . ? Ru3 O32 3.011(7) . . ? Ru3 O33 3.023(8) . . ? Ru3 C2 3.201(9) . . ? Ru3 H2a 3.39(7) . . ? C11 C12 2.746(12) . . ? C11 C13 2.859(13) . . ? C11 C2 2.950(12) . . ? C11 H2b 2.80(7) . . ? O11 Cl 3.874(7) . . ? O11 H2a 2.78(7) . 4_556 ? C12 C13 2.788(14) . . ? C12 C2 2.999(12) . . ? C12 H2a 2.97(7) . . ? O12 H2b 2.68(7) . 4_546 ? O12 H0 2.638(6) . . ? C13 C22 2.912(13) . . ? C21 C22 2.591(14) . . ? C21 C1 2.915(11) . . ? C21 C1 2.829(10) . 8_666 ? C21 H2b 3.29(6) . 8_666 ? C21 H2b 2.97(7) . . ? O21 Cl 3.796(9) . 4_556 ? O21 H2b 3.30(7) . . ? O21 H0 3.074(8) . 4_556 ? O21 H0 3.218(8) . 7 ? C22 C31 2.906(13) . 8_666 ? C22 Cl 3.592(10) . 7_655 ? O22 Cl 3.465(8) . 7_655 ? C31 C32 2.828(11) . . ? C31 C33 2.778(12) . . ? O31 Cl 3.608(9) . 7_645 ? O31 H2a 3.16(7) . 8_656 ? C32 C33 2.686(14) . . ? C32 C1 2.904(11) . . ? C32 Cl 3.738(10) . 4_546 ? C32 H2a 2.97(7) . . ? O32 Cl 3.551(8) . 4_546 ? O32 H2a 3.26(7) . . ? O33 Cl 3.330(9) . 4_646 ? C1 H2a 1.93(7) . . ? C1 H2b 2.01(7) . . ? Cl Cl 2.857(6) . 5_556 ? Cl H2a 3.78(7) . 4_556 ? Cl H0 2.199(5) . . ? Cl H0 2.197(5) . 5_556 ? H2a H2b 1.48(10) . . ? H0 H0 1.5514(3) . 5_556 ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru2 Ru1 Ru3 63.48(3) . . . ? Ru2 Ru1 C11 97.7(2) . . . ? Ru2 Ru1 C12 165.5(3) . . . ? Ru2 Ru1 C13 95.5(2) . . . ? Ru2 Ru1 C1 47.83(18) . . . ? Ru2 Ru1 C2 76.4(2) . . . ? Ru3 Ru1 C11 159.6(2) . . . ? Ru3 Ru1 C12 104.7(3) . . . ? Ru3 Ru1 C13 93.7(3) . . . ? Ru3 Ru1 C1 47.90(18) . . . ? Ru3 Ru1 C2 77.4(2) . . . ? C11 Ru1 C12 92.5(4) . . . ? C11 Ru1 C13 96.2(4) . . . ? C11 Ru1 C1 114.0(3) . . . ? C11 Ru1 C2 90.8(4) . . . ? C12 Ru1 C13 93.5(4) . . . ? C12 Ru1 C1 118.3(3) . . . ? C12 Ru1 C2 93.2(4) . . . ? C13 Ru1 C1 133.3(3) . . . ? C13 Ru1 C2 170.0(3) . . . ? C1 Ru1 C2 36.7(3) . . . ? Ru1 Ru2 Ru3 59.61(2) . . . ? Ru1 Ru2 C21 98.2(3) . . . ? Ru1 Ru2 C22 82.3(3) . . . ? Ru1 Ru2 C1 51.37(18) . . . ? Ru1 Ru2 Ru2 101.00(4) . . 8_666 ? Ru1 Ru2 Ru3 124.72(4) . . 8_666 ? Ru1 Ru2 C1 150.20(19) . . 8_666 ? Ru3 Ru2 C21 142.6(3) . . . ? Ru3 Ru2 C22 115.4(3) . . . ? Ru3 Ru2 C1 46.2(2) . . . ? Ru3 Ru2 Ru2 57.39(3) . . 8_666 ? Ru3 Ru2 Ru3 69.91(3) . . 8_666 ? Ru3 Ru2 C1 96.94(18) . . 8_666 ? C21 Ru2 C22 87.8(4) . . . ? C21 Ru2 C1 96.5(3) . . . ? C21 Ru2 Ru2 104.3(3) . . 8_666 ? C21 Ru2 Ru3 136.8(3) . . 8_666 ? C21 Ru2 C1 90.5(3) . . 8_666 ? C22 Ru2 C1 133.7(3) . . . ? C22 Ru2 Ru2 166.7(3) . . 8_666 ? C22 Ru2 Ru3 101.4(3) . . 8_666 ? C22 Ru2 C1 126.7(3) . . 8_666 ? C1 Ru2 Ru2 51.48(18) . . 8_666 ? C1 Ru2 Ru3 106.14(19) . . 8_666 ? C1 Ru2 C1 99.5(3) . . 8_666 ? Ru2 Ru2 Ru3 66.08(4) 8_666 . 8_666 ? Ru2 Ru2 C1 49.20(18) 8_666 . 8_666 ? Ru3 Ru2 C1 50.24(19) 8_666 . 8_666 ? Ru1 Ru3 Ru2 56.91(3) . . . ? Ru1 Ru3 C31 174.1(3) . . . ? Ru1 Ru3 C32 80.4(3) . . . ? Ru1 Ru3 C33 91.2(3) . . . ? Ru1 Ru3 C1 49.64(17) . . . ? Ru1 Ru3 Ru2 98.32(4) . . 8_666 ? Ru1 Ru3 Ru3 105.35(4) . . 8_666 ? Ru2 Ru3 C31 124.5(2) . . . ? Ru2 Ru3 C32 132.3(3) . . . ? Ru2 Ru3 C33 109.0(3) . . . ? Ru2 Ru3 C1 44.66(19) . . . ? Ru2 Ru3 Ru2 56.53(3) . . 8_666 ? Ru2 Ru3 Ru3 51.70(2) . . 8_666 ? C31 Ru3 C32 95.9(4) . . . ? C31 Ru3 C33 93.4(4) . . . ? C31 Ru3 C1 126.5(3) . . . ? C31 Ru3 Ru2 79.3(2) . . 8_666 ? C31 Ru3 Ru3 78.1(3) . . 8_666 ? C32 Ru3 C33 90.5(4) . . . ? C32 Ru3 C1 92.6(3) . . . ? C32 Ru3 Ru2 118.0(3) . . 8_666 ? C32 Ru3 Ru3 173.3(2) . . 8_666 ? C33 Ru3 C1 139.3(3) . . . ? C33 Ru3 Ru2 151.0(3) . . 8_666 ? C33 Ru3 Ru3 92.7(3) . . 8_666 ? C1 Ru3 Ru2 50.72(17) . . 8_666 ? C1 Ru3 Ru3 88.80(18) . . 8_666 ? Ru2 Ru3 Ru3 58.39(3) 8_666 . 8_666 ? Ru1 C11 O11 175.9(7) . . . ? Ru1 C12 O12 176.7(9) . . . ? Ru1 C13 O13 177.2(7) . . . ? Ru2 C21 O21 177.6(8) . . . ? Ru2 C22 O22 179.7(8) . . . ? Ru3 C31 O31 172.2(7) . . . ? Ru3 C32 O32 177.8(7) . . . ? Ru3 C33 O33 178.8(8) . . . ? Ru1 C1 Ru2 80.8(2) . . . ? Ru1 C1 Ru3 82.5(2) . . . ? Ru1 C1 C2 73.3(4) . . . ? Ru1 C1 Ru2 152.9(3) . . 8_666 ? Ru2 C1 Ru3 89.2(3) . . . ? Ru2 C1 C2 127.1(6) . . . ? Ru2 C1 Ru2 79.3(2) . . 8_666 ? Ru3 C1 C2 130.4(6) . . . ? Ru3 C1 Ru2 79.0(2) . . 8_666 ? C2 C1 Ru2 133.8(5) . . 8_666 ? Ru1 C2 C1 70.1(4) . . . ? Ru1 C2 H2a 116(5) . . . ? Ru1 C2 H2b 111(5) . . . ? C1 C2 H2a 118(5) . . . ? C1 C2 H2b 120(4) . . . ? H2a C2 H2b 114(7) . . . ? Cl C0 H0 108.7(6) . . . ? Cl C0 Cl 116.1(8) . . 5_556 ? Cl C0 H0 108.6(10) . . 5_556 ? H0 C0 Cl 108.6(10) . . 5_556 ? H0 C0 H0 105.7(13) . . 5_556 ? Cl C0 H0 108.7(6) 5_556 . 5_556 ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 49 _reflns_number_total 2747 #ActaC _reflns_number_observed 1988 #ActaC _reflns_observed_criterion refl_observed_if_I____>3.000_sigma(I___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 9.143 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 3.6727 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 #ActaC _publ_contact_author_fax (61)-8-9380-1005 #ActaC _publ_contact_author_email bws@crystal.uwa.edu.au #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #======================================================================= # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?