# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef 'gk98n.cif' # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; _publ_contact_author_email brian.skelton@uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'R.O. Fuller' . ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; 'C. S. Griffith' '' '' 'G.A. Koutsantonis' '' '' 'K.M. Lapere' '' '' 'B.W. Skelton' '' '' 'M.A. Spackman' '' '' 'A.H. White' '' '' 'D.A. Wild' '' '' _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gk98n _database_code_depnum_ccdc_archive 'CCDC 811630' #TrackingRef 'gk98n.cif' _audit_creation_date 2010-10-01T21:53:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C7 H5 Br O2 Ru, 1/2(C2 Br6)' _chemical_formula_sum 'C8 H5 Br4 O2 Ru' _chemical_formula_weight 553.83 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall '-p 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5104(7) _cell_length_b 11.9040(10) _cell_length_c 29.320(3) _cell_angle_alpha 90 _cell_angle_beta 96.9420(10) _cell_angle_gamma 90 _cell_volume 2602.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.2 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .38 _exptl_absorpt_correction_T_max .80 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_unetI/netI 0.0158 _diffrn_reflns_number 30436 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.935 _reflns_number_total 6633 _reflns_number_gt 5414 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Displacement parameters of the C atoms of the minor component of the disordered C2Br6 were restrained to reasonable values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+35.4584P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6633 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.509 _refine_diff_density_min -3.039 _refine_diff_density_rms 0.235 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.54821(6) 0.71355(4) 1.008134(15) 0.01475(10) Uani 1 1 d . . . Br1 Br 0.33215(8) 0.84156(6) 1.04284(2) 0.02495(14) Uani 1 1 d . . . C11 C 0.5626(9) 0.6257(7) 1.0626(3) 0.0326(16) Uani 1 1 d . . . O11 O 0.5755(9) 0.5756(6) 1.0953(2) 0.0516(17) Uani 1 1 d . . . C12 C 0.3479(9) 0.6322(6) 0.9810(2) 0.0278(14) Uani 1 1 d . . . O12 O 0.2243(7) 0.5861(5) 0.9633(2) 0.0432(14) Uani 1 1 d . . . C101 C 0.7305(9) 0.8591(6) 0.9960(3) 0.0297(15) Uani 1 1 d . . . H101 H 0.7208 0.9319 1.0088 0.036 Uiso 1 1 calc R . . C102 C 0.8363(9) 0.7693(6) 1.0164(3) 0.0302(15) Uani 1 1 d . . . H102 H 0.9098 0.7713 1.0451 0.036 Uiso 1 1 calc R . . C103 C 0.8125(9) 0.6755(6) 0.9860(3) 0.0292(15) Uani 1 1 d . . . H103 H 0.8658 0.6035 0.9911 0.035 Uiso 1 1 calc R . . C104 C 0.6951(10) 0.7088(7) 0.9469(2) 0.0312(15) Uani 1 1 d . . . H104 H 0.6581 0.6634 0.9208 0.037 Uiso 1 1 calc R . . C105 C 0.6419(9) 0.8217(6) 0.9533(2) 0.0286(15) Uani 1 1 d . . . H105 H 0.5613 0.8644 0.9327 0.034 Uiso 1 1 calc R . . Ru2 Ru 0.84347(6) 0.43443(4) 0.819426(16) 0.01709(10) Uani 1 1 d . . . Br2 Br 0.60718(8) 0.58831(5) 0.81744(2) 0.02164(13) Uani 1 1 d . . . C21 C 0.8646(9) 0.4306(6) 0.8842(3) 0.0296(15) Uani 1 1 d . . . O21 O 0.8836(8) 0.4283(5) 0.92345(19) 0.0450(14) Uani 1 1 d . . . C22 C 0.6592(10) 0.3253(6) 0.8140(3) 0.0311(15) Uani 1 1 d . . . O22 O 0.5530(8) 0.2561(5) 0.8088(2) 0.0519(16) Uani 1 1 d . . . C201 C 1.0178(9) 0.5405(7) 0.7788(3) 0.0337(16) Uani 1 1 d . . . H201 H 1.0027 0.6192 0.7743 0.04 Uiso 1 1 calc R . . C202 C 1.1274(9) 0.4885(7) 0.8148(3) 0.0324(16) Uani 1 1 d . . . H202 H 1.2009 0.5259 0.8388 0.039 Uiso 1 1 calc R . . C203 C 1.1092(10) 0.3692(7) 0.8092(3) 0.0403(19) Uani 1 1 d . . . H203 H 1.1653 0.3133 0.8292 0.048 Uiso 1 1 calc R . . C204 C 0.9924(11) 0.3503(7) 0.7685(3) 0.042(2) Uani 1 1 d . . . H204 H 0.9592 0.2789 0.7558 0.05 Uiso 1 1 calc R . . C205 C 0.9331(10) 0.4544(8) 0.7500(3) 0.0367(18) Uani 1 1 d . . . H205 H 0.8512 0.4656 0.7231 0.044 Uiso 1 1 calc R . . Br11 Br 0.09103(10) 0.99829(8) 0.78224(2) 0.0408(2) Uani 1 1 d . . . Br12 Br 0.32097(9) 0.79839(6) 0.83946(3) 0.03000(15) Uani 1 1 d . . . Br13 Br 0.34868(10) 1.05854(7) 0.87293(3) 0.0407(2) Uani 1 1 d . . . Br21 Br -0.09836(10) 1.06350(7) 0.87470(3) 0.03602(18) Uani 1 1 d . . . Br22 Br -0.11667(9) 0.79863(6) 0.84450(2) 0.02514(14) Uani 1 1 d . . . Br23 Br 0.13329(9) 0.87246(6) 0.93351(2) 0.02665(15) Uani 1 1 d . . . C1 C 0.1917(13) 0.9379(9) 0.8421(3) 0.022(3) Uani 0.608(19) 1 d P A 1 C2 C 0.0361(13) 0.9168(8) 0.8713(3) 0.017(2) Uani 0.608(19) 1 d P A 1 C1' C 0.109(2) 1.0009(14) 0.8516(5) 0.020(4) Uiso 0.392(19) 1 d P A 2 C2' C 0.114(2) 0.8772(14) 0.8665(5) 0.013(4) Uiso 0.392(19) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0147(2) 0.0119(2) 0.0179(2) 0.00062(16) 0.00262(15) 0.00054(17) Br1 0.0219(3) 0.0249(3) 0.0285(3) -0.0063(3) 0.0050(2) 0.0021(2) C11 0.026(3) 0.037(4) 0.036(4) 0.007(3) 0.007(3) 0.005(3) O11 0.056(4) 0.061(4) 0.041(3) 0.026(3) 0.015(3) 0.009(3) C12 0.028(3) 0.021(3) 0.036(4) -0.004(3) 0.007(3) 0.002(3) O12 0.031(3) 0.025(3) 0.071(4) -0.008(3) -0.004(3) -0.008(2) C101 0.031(3) 0.024(4) 0.037(4) -0.003(3) 0.015(3) -0.006(3) C102 0.022(3) 0.036(4) 0.033(4) 0.001(3) 0.002(3) -0.007(3) C103 0.024(3) 0.027(4) 0.039(4) 0.006(3) 0.017(3) 0.004(3) C104 0.032(3) 0.038(4) 0.025(3) -0.007(3) 0.010(3) -0.005(3) C105 0.023(3) 0.029(4) 0.034(4) 0.011(3) 0.005(3) -0.002(3) Ru2 0.0152(2) 0.0134(2) 0.0224(2) -0.00254(17) 0.00129(16) -0.00019(17) Br2 0.0193(3) 0.0184(3) 0.0270(3) -0.0025(2) 0.0019(2) 0.0010(2) C21 0.025(3) 0.027(4) 0.036(4) 0.004(3) 0.000(3) 0.002(3) O21 0.049(3) 0.053(4) 0.031(3) 0.006(3) -0.004(2) -0.003(3) C22 0.029(3) 0.028(4) 0.037(4) -0.002(3) 0.003(3) 0.003(3) O22 0.044(3) 0.033(3) 0.078(5) 0.000(3) 0.004(3) -0.022(3) C201 0.026(3) 0.035(4) 0.042(4) 0.003(3) 0.011(3) 0.000(3) C202 0.018(3) 0.038(4) 0.042(4) 0.000(3) 0.004(3) -0.004(3) C203 0.026(3) 0.038(4) 0.060(5) 0.010(4) 0.015(3) 0.011(3) C204 0.037(4) 0.038(5) 0.055(5) -0.027(4) 0.023(4) -0.003(4) C205 0.024(3) 0.054(5) 0.033(4) -0.005(4) 0.005(3) 0.002(3) Br11 0.0348(4) 0.0622(6) 0.0237(3) 0.0166(3) -0.0039(3) -0.0179(4) Br12 0.0256(3) 0.0230(3) 0.0407(4) -0.0049(3) 0.0013(3) 0.0064(3) Br13 0.0338(4) 0.0454(5) 0.0398(4) 0.0139(3) -0.0091(3) -0.0245(3) Br21 0.0297(3) 0.0456(5) 0.0331(4) -0.0022(3) 0.0053(3) 0.0181(3) Br22 0.0257(3) 0.0235(3) 0.0254(3) -0.0026(2) 0.0000(2) -0.0077(3) Br23 0.0287(3) 0.0308(4) 0.0197(3) 0.0035(3) 0.0002(2) -0.0062(3) C1 0.020(5) 0.022(6) 0.022(5) 0.002(4) -0.003(4) 0.004(4) C2 0.014(5) 0.010(5) 0.026(5) -0.003(4) -0.002(3) 0.006(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C12 1.883(7) . ? Ru1 C11 1.902(7) . ? Ru1 C103 2.208(6) . ? Ru1 C104 2.218(7) . ? Ru1 C105 2.238(7) . ? Ru1 C102 2.248(7) . ? Ru1 C101 2.263(7) . ? Ru1 Br1 2.5279(8) . ? C11 O11 1.123(9) . ? C12 O12 1.146(9) . ? C101 C105 1.416(10) . ? C101 C102 1.421(11) . ? C101 H101 0.95 . ? C102 C103 1.426(11) . ? C102 H102 0.95 . ? C103 C104 1.416(10) . ? C103 H103 0.95 . ? C104 C105 1.421(11) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? Ru2 C21 1.887(7) . ? Ru2 C22 1.891(8) . ? Ru2 C203 2.196(7) . ? Ru2 C204 2.210(7) . ? Ru2 C205 2.233(8) . ? Ru2 C202 2.247(7) . ? Ru2 C201 2.260(7) . ? Ru2 Br2 2.5463(8) . ? C21 O21 1.143(9) . ? C22 O22 1.144(9) . ? C201 C202 1.402(11) . ? C201 C205 1.427(11) . ? C201 H201 0.95 . ? C202 C203 1.435(12) . ? C202 H202 0.95 . ? C203 C204 1.411(12) . ? C203 H203 0.95 . ? C204 C205 1.404(13) . ? C204 H204 0.95 . ? C205 H205 0.95 . ? Br11 C1 1.962(10) . ? Br11 C1' 2.022(15) . ? Br12 C1 1.930(11) . ? Br12 C2' 2.057(17) . ? Br13 C1' 1.954(16) . ? Br13 C1 2.002(11) . ? Br21 C1' 1.925(16) . ? Br21 C2 2.025(10) . ? Br22 C2 1.922(10) . ? Br22 C2' 2.004(14) . ? Br23 C2' 1.953(14) . ? Br23 C2 1.955(10) . ? C1 C2 1.550(15) . ? C1' C2' 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ru1 C11 91.9(3) . . ? C12 Ru1 C103 118.1(3) . . ? C11 Ru1 C103 99.9(3) . . ? C12 Ru1 C104 95.4(3) . . ? C11 Ru1 C104 133.0(3) . . ? C103 Ru1 C104 37.3(3) . . ? C12 Ru1 C105 107.3(3) . . ? C11 Ru1 C105 158.3(3) . . ? C103 Ru1 C105 62.3(3) . . ? C104 Ru1 C105 37.2(3) . . ? C12 Ru1 C102 155.1(3) . . ? C11 Ru1 C102 96.7(3) . . ? C103 Ru1 C102 37.3(3) . . ? C104 Ru1 C102 61.9(3) . . ? C105 Ru1 C102 61.7(3) . . ? C12 Ru1 C101 142.6(3) . . ? C11 Ru1 C101 125.4(3) . . ? C103 Ru1 C101 61.9(3) . . ? C104 Ru1 C101 61.5(3) . . ? C105 Ru1 C101 36.7(3) . . ? C102 Ru1 C101 36.7(3) . . ? C12 Ru1 Br1 87.8(2) . . ? C11 Ru1 Br1 88.1(2) . . ? C103 Ru1 Br1 152.3(2) . . ? C104 Ru1 Br1 138.4(2) . . ? C105 Ru1 Br1 102.43(19) . . ? C102 Ru1 Br1 115.8(2) . . ? C101 Ru1 Br1 91.82(18) . . ? O11 C11 Ru1 177.9(8) . . ? O12 C12 Ru1 177.3(7) . . ? C105 C101 C102 108.3(6) . . ? C105 C101 Ru1 70.7(4) . . ? C102 C101 Ru1 71.1(4) . . ? C105 C101 H101 125.8 . . ? C102 C101 H101 125.8 . . ? Ru1 C101 H101 124 . . ? C101 C102 C103 107.7(6) . . ? C101 C102 Ru1 72.2(4) . . ? C103 C102 Ru1 69.8(4) . . ? C101 C102 H102 126.1 . . ? C103 C102 H102 126.1 . . ? Ru1 C102 H102 123.5 . . ? C104 C103 C102 107.8(6) . . ? C104 C103 Ru1 71.7(4) . . ? C102 C103 Ru1 72.9(4) . . ? C104 C103 H103 126.1 . . ? C102 C103 H103 126.1 . . ? Ru1 C103 H103 121.1 . . ? C103 C104 C105 108.4(6) . . ? C103 C104 Ru1 71.0(4) . . ? C105 C104 Ru1 72.2(4) . . ? C103 C104 H104 125.8 . . ? C105 C104 H104 125.8 . . ? Ru1 C104 H104 122.7 . . ? C101 C105 C104 107.8(6) . . ? C101 C105 Ru1 72.6(4) . . ? C104 C105 Ru1 70.6(4) . . ? C101 C105 H105 126.1 . . ? C104 C105 H105 126.1 . . ? Ru1 C105 H105 122.3 . . ? C21 Ru2 C22 92.3(3) . . ? C21 Ru2 C203 99.3(3) . . ? C22 Ru2 C203 114.4(3) . . ? C21 Ru2 C204 132.9(3) . . ? C22 Ru2 C204 93.2(3) . . ? C203 Ru2 C204 37.4(3) . . ? C21 Ru2 C205 157.2(3) . . ? C22 Ru2 C205 107.1(3) . . ? C203 Ru2 C205 62.2(3) . . ? C204 Ru2 C205 36.8(3) . . ? C21 Ru2 C202 95.9(3) . . ? C22 Ru2 C202 151.9(3) . . ? C203 Ru2 C202 37.7(3) . . ? C204 Ru2 C202 61.8(3) . . ? C205 Ru2 C202 61.4(3) . . ? C21 Ru2 C201 124.1(3) . . ? C22 Ru2 C201 143.5(3) . . ? C203 Ru2 C201 62.1(3) . . ? C204 Ru2 C201 61.6(3) . . ? C205 Ru2 C201 37.0(3) . . ? C202 Ru2 C201 36.2(3) . . ? C21 Ru2 Br2 90.8(2) . . ? C22 Ru2 Br2 89.5(2) . . ? C203 Ru2 Br2 153.4(2) . . ? C204 Ru2 Br2 135.9(3) . . ? C205 Ru2 Br2 100.9(2) . . ? C202 Ru2 Br2 117.1(2) . . ? C201 Ru2 Br2 91.9(2) . . ? O21 C21 Ru2 177.7(6) . . ? O22 C22 Ru2 175.9(7) . . ? C202 C201 C205 107.9(7) . . ? C202 C201 Ru2 71.4(4) . . ? C205 C201 Ru2 70.5(4) . . ? C202 C201 H201 126 . . ? C205 C201 H201 126 . . ? Ru2 C201 H201 123.8 . . ? C201 C202 C203 108.2(7) . . ? C201 C202 Ru2 72.4(4) . . ? C203 C202 Ru2 69.2(4) . . ? C201 C202 H202 125.9 . . ? C203 C202 H202 125.9 . . ? Ru2 C202 H202 124.1 . . ? C204 C203 C202 107.2(7) . . ? C204 C203 Ru2 71.9(4) . . ? C202 C203 Ru2 73.1(4) . . ? C204 C203 H203 126.4 . . ? C202 C203 H203 126.4 . . ? Ru2 C203 H203 120.4 . . ? C205 C204 C203 108.8(7) . . ? C205 C204 Ru2 72.5(4) . . ? C203 C204 Ru2 70.8(4) . . ? C205 C204 H204 125.6 . . ? C203 C204 H204 125.6 . . ? Ru2 C204 H204 122.8 . . ? C204 C205 C201 107.9(7) . . ? C204 C205 Ru2 70.7(4) . . ? C201 C205 Ru2 72.5(4) . . ? C204 C205 H205 126.1 . . ? C201 C205 H205 126.1 . . ? Ru2 C205 H205 122.4 . . ? C2 C1 Br12 107.4(7) . . ? C2 C1 Br11 108.5(6) . . ? Br12 C1 Br11 114.9(5) . . ? C2 C1 Br13 108.0(7) . . ? Br12 C1 Br13 111.3(5) . . ? Br11 C1 Br13 106.5(5) . . ? C1 C2 Br22 110.3(7) . . ? C1 C2 Br23 109.7(6) . . ? Br22 C2 Br23 108.7(5) . . ? C1 C2 Br21 107.5(7) . . ? Br22 C2 Br21 112.0(5) . . ? Br23 C2 Br21 108.6(5) . . ? C2' C1' Br21 105.1(10) . . ? C2' C1' Br13 105.0(10) . . ? Br21 C1' Br13 120.3(8) . . ? C2' C1' Br11 105.6(10) . . ? Br21 C1' Br11 113.6(8) . . ? Br13 C1' Br11 106.0(7) . . ? C1' C2' Br23 108.1(10) . . ? C1' C2' Br22 111.6(11) . . ? Br23 C2' Br22 105.5(7) . . ? C1' C2' Br12 108.6(10) . . ? Br23 C2' Br12 114.0(8) . . ? Br22 C2' Br12 109.1(7) . . ? #===END # Attachment 'gk98p.cif' data_gk98p _database_code_depnum_ccdc_archive 'CCDC 811631' #TrackingRef 'gk98p.cif' _audit_creation_date 2010-10-04T09:03:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C7 H5 Br O2 Ru,0.5(C2 Br6)' _chemical_formula_sum 'C8 H5 Br4 O2 Ru' _chemical_formula_weight 553.83 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.767(2) _cell_length_b 7.475(2) _cell_length_c 13.172(4) _cell_angle_alpha 85.299(4) _cell_angle_beta 89.063(4) _cell_angle_gamma 72.030(4) _cell_volume 631.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3276 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.7 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 506 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .29 _exptl_absorpt_correction_T_max .83 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_number 7149 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 29.08 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.906 _reflns_number_total 3073 _reflns_number_gt 2574 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution SIR92 _computing_structure_refinement ORTEPII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1190P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3073 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.895 _refine_diff_density_min -2.827 _refine_diff_density_rms 0.34 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.58598(8) 0.60886(8) 0.18950(4) 0.01845(18) Uani 1 1 d . . . Br1 Br 0.28901(12) 0.46698(11) 0.20976(6) 0.0264(2) Uani 1 1 d . . . C11 C 0.6301(11) 0.5837(11) 0.3344(5) 0.0243(15) Uani 1 1 d . . . O11 O 0.6553(9) 0.5816(8) 0.4188(4) 0.0315(12) Uani 1 1 d . . . C12 C 0.7768(12) 0.3704(11) 0.1705(5) 0.0265(15) Uani 1 1 d . . . O12 O 0.8953(10) 0.2305(8) 0.1509(5) 0.0382(14) Uani 1 1 d . . . C101 C 0.3828(14) 0.8561(12) 0.0938(7) 0.039(2) Uani 1 1 d . . . H101 H 0.2387 0.8762 0.0834 0.047 Uiso 1 1 calc R . . C102 C 0.4679(19) 0.9247(12) 0.1713(7) 0.046(3) Uani 1 1 d . . . H102 H 0.393 1.0009 0.2221 0.056 Uiso 1 1 calc R . . C103 C 0.6844(18) 0.8613(14) 0.1611(7) 0.047(3) Uani 1 1 d . . . H103 H 0.7827 0.8853 0.2045 0.056 Uiso 1 1 calc R . . C104 C 0.7304(15) 0.7554(13) 0.0749(7) 0.043(2) Uani 1 1 d . . . H104 H 0.8648 0.6963 0.0493 0.051 Uiso 1 1 calc R . . C105 C 0.5411(17) 0.7539(13) 0.0342(6) 0.040(2) Uani 1 1 d . . . H105 H 0.5243 0.6933 -0.0242 0.048 Uiso 1 1 calc R . . Br2 Br 0.87344(12) 0.78995(11) 0.60213(6) 0.0293(2) Uani 1 1 d . . . Br3 Br 0.67866(10) 1.10513(10) 0.41678(5) 0.0230(2) Uani 1 1 d . . . Br4 Br 1.08763(11) 0.77491(11) 0.38007(6) 0.0273(2) Uani 1 1 d . . . C1 C 0.9336(16) 0.9396(15) 0.4825(8) 0.0198(19) Uani 0.645(15) 1 d P . 1 C1' C 0.982(3) 1.019(3) 0.4429(15) 0.0198(19) Uani 0.355(15) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0245(3) 0.0179(3) 0.0144(3) -0.0021(2) -0.0003(2) -0.0086(2) Br1 0.0319(4) 0.0272(4) 0.0253(4) -0.0068(3) 0.0051(3) -0.0160(3) C11 0.028(3) 0.026(4) 0.022(3) 0.002(3) -0.001(3) -0.014(3) O11 0.038(3) 0.037(3) 0.018(3) -0.002(2) -0.004(2) -0.008(3) C12 0.036(4) 0.026(4) 0.021(3) -0.003(3) -0.002(3) -0.013(3) O12 0.039(3) 0.027(3) 0.045(4) -0.011(3) 0.005(3) -0.004(3) C101 0.033(4) 0.033(5) 0.050(5) 0.016(4) -0.009(4) -0.010(4) C102 0.090(8) 0.013(4) 0.032(4) -0.001(3) 0.019(5) -0.011(4) C103 0.073(7) 0.043(5) 0.040(5) 0.018(4) -0.024(5) -0.047(5) C104 0.039(4) 0.034(5) 0.050(5) 0.018(4) 0.009(4) -0.010(4) C105 0.079(7) 0.032(5) 0.014(3) 0.002(3) -0.005(4) -0.026(5) Br2 0.0342(4) 0.0218(4) 0.0306(4) 0.0018(3) 0.0108(3) -0.0084(3) Br3 0.0205(3) 0.0249(4) 0.0220(4) -0.0014(3) -0.0042(3) -0.0048(3) Br4 0.0258(4) 0.0294(4) 0.0256(4) -0.0136(3) -0.0015(3) -0.0039(3) C1 0.018(4) 0.019(5) 0.023(5) -0.002(4) 0.004(4) -0.006(3) C1' 0.018(4) 0.019(5) 0.023(5) -0.002(4) 0.004(4) -0.006(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C12 1.884(8) . ? Ru1 C11 1.922(7) . ? Ru1 C104 2.186(8) . ? Ru1 C103 2.190(8) . ? Ru1 C105 2.215(7) . ? Ru1 C101 2.237(8) . ? Ru1 C102 2.240(8) . ? Ru1 Br1 2.5468(11) . ? C11 O11 1.125(9) . ? C12 O12 1.150(10) . ? C101 C105 1.384(13) . ? C101 C102 1.387(14) . ? C101 H101 0.95 . ? C102 C103 1.402(16) . ? C102 H102 0.95 . ? C103 C104 1.414(15) . ? C103 H103 0.95 . ? C104 C105 1.400(14) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? Br2 C1 1.968(11) . ? Br2 C1' 2.01(2) 2_776 ? Br3 C1 1.953(11) . ? Br3 C1' 1.979(19) . ? Br4 C1 1.963(11) . ? Br4 C1' 1.99(2) . ? C1 C1 1.56(2) 2_776 ? C1' C1' 1.52(4) 2_776 ? C1' Br2 2.01(2) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ru1 C11 93.7(3) . . ? C12 Ru1 C104 93.5(3) . . ? C11 Ru1 C104 127.1(4) . . ? C12 Ru1 C103 119.3(4) . . ? C11 Ru1 C103 95.7(3) . . ? C104 Ru1 C103 37.7(4) . . ? C12 Ru1 C105 103.6(3) . . ? C11 Ru1 C105 156.4(3) . . ? C104 Ru1 C105 37.1(4) . . ? C103 Ru1 C105 61.9(3) . . ? C12 Ru1 C101 138.1(3) . . ? C11 Ru1 C101 128.1(3) . . ? C104 Ru1 C101 61.3(3) . . ? C103 Ru1 C101 61.1(3) . . ? C105 Ru1 C101 36.2(4) . . ? C12 Ru1 C102 154.7(4) . . ? C11 Ru1 C102 97.1(3) . . ? C104 Ru1 C102 61.8(4) . . ? C103 Ru1 C102 36.9(4) . . ? C105 Ru1 C102 60.9(3) . . ? C101 Ru1 C102 36.1(4) . . ? C12 Ru1 Br1 91.1(2) . . ? C11 Ru1 Br1 91.2(2) . . ? C104 Ru1 Br1 140.9(3) . . ? C103 Ru1 Br1 148.2(3) . . ? C105 Ru1 Br1 104.3(3) . . ? C101 Ru1 Br1 90.4(2) . . ? C102 Ru1 Br1 111.5(3) . . ? O11 C11 Ru1 175.2(7) . . ? O12 C12 Ru1 174.4(7) . . ? C105 C101 C102 109.1(9) . . ? C105 C101 Ru1 71.1(5) . . ? C102 C101 Ru1 72.1(5) . . ? C105 C101 H101 125.4 . . ? C102 C101 H101 125.4 . . ? Ru1 C101 H101 123 . . ? C101 C102 C103 107.7(8) . . ? C101 C102 Ru1 71.8(5) . . ? C103 C102 Ru1 69.6(5) . . ? C101 C102 H102 126.2 . . ? C103 C102 H102 126.2 . . ? Ru1 C102 H102 124 . . ? C102 C103 C104 107.8(8) . . ? C102 C103 Ru1 73.5(5) . . ? C104 C103 Ru1 71.0(5) . . ? C102 C103 H103 126.1 . . ? C104 C103 H103 126.1 . . ? Ru1 C103 H103 121.2 . . ? C105 C104 C103 107.3(8) . . ? C105 C104 Ru1 72.6(5) . . ? C103 C104 Ru1 71.3(5) . . ? C105 C104 H104 126.4 . . ? C103 C104 H104 126.4 . . ? Ru1 C104 H104 121.5 . . ? C101 C105 C104 108.1(8) . . ? C101 C105 Ru1 72.7(5) . . ? C104 C105 Ru1 70.3(5) . . ? C101 C105 H105 125.9 . . ? C104 C105 H105 125.9 . . ? Ru1 C105 H105 122.7 . . ? C1 C1 Br3 109.5(9) 2_776 . ? C1 C1 Br4 109.3(9) 2_776 . ? Br3 C1 Br4 107.1(5) . . ? C1 C1 Br2 108.6(9) 2_776 . ? Br3 C1 Br2 111.5(5) . . ? Br4 C1 Br2 110.9(5) . . ? C1' C1' Br3 108.2(17) 2_776 . ? C1' C1' Br4 108.0(18) 2_776 . ? Br3 C1' Br4 105.1(9) . . ? C1' C1' Br2 105.9(17) 2_776 2_776 ? Br3 C1' Br2 114.6(10) . 2_776 ? Br4 C1' Br2 114.8(9) . 2_776 ? #===END