# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'B.P.Fokwa T.' ; Institute of Inorganic Chemistry RWTH Aachen University D-52056 Aachen Germany ; 'J.von Appen' ; Institute of Inorganic Chemistry RWTH Aachen University D-52056 Aachen Germany ; R.Dronskowski ; Institute of Inorganic Chemistry RWTH Aachen University D-52056 Aachen Germany ; _publ_contact_author_address ; Institute of Inorganic Chemistry RWTH Aachen University D-52056 Aachen Germany ; _publ_contact_author_email drons@hal9000.ac.rwth-aachen.de _publ_contact_author_fax 00492418092642 _publ_contact_author_phone 00492418093642 #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Richard Dronskowski' _publ_contact_letter ; Please consider this CIF submission for deposit material to a normal publi- cation in "chemical comminication". ; #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of a missing structural link: The first trigonal planar B4 units in the novel complex boride Ti1+xOs2_xRuB2 (x = 0.6) ; data_Ti1.6Os1.4RuB2 _database_code_depnum_ccdc_archive 'CCDC 612040' #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B2 Os1.42 Ru Ti1.58' _chemical_formula_weight 468.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P -6 2 m' _symmetry_space_group_name_Hall 'P -6 -2' _symmetry_Int_Tables_number 189 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 8.8554(14) _cell_length_b 8.8554(14) _cell_length_c 3.0336(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 206.02(7) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour silver _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 11.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 74.941 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS(Bruker, 2001)' _exptl_absorpt_correction_T_min 0.026 _exptl_absorpt_correction_T_max 0.232 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method 'integration method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2271 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 4.60 _diffrn_reflns_theta_max 35.98 _reflns_number_total 395 _reflns_number_gt 380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1c (K. Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2sigma(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^)+(0.0300P)^2^+8.9965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(4) _refine_ls_number_reflns 395 _refine_ls_number_parameters 23 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.46384(10) 0.27554(10) 0.5000 0.00653(18) Uani 0.689(12) 2 d SP . . Ti1 Ti 0.46384(10) 0.27554(10) 0.5000 0.00653(18) Uani 0.311(12) 2 d SP . . Ru1 Ru 0.1736(2) 0.1736(2) 0.0000 0.0129(6) Uani 1 4 d S . . Ti2 Ti 0.4190(5) 0.0000 0.0000 0.0079(10) Uani 0.959(7) 4 d SP . . Os2 Os 0.4190(5) 0.0000 0.0000 0.0079(10) Uani 0.041(7) 4 d SP . . B1 B 0.0000 0.0000 0.5000 0.05(2) Uiso 1 12 d S . . B2 B 0.0000 0.213(3) 0.5000 0.015(5) Uiso 1 4 d S . . B3 B 0.6667 0.3333 0.0000 0.013(6) Uiso 1 6 d S . . 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 Os1 0.0052(3) 0.0065(3) 0.0079(3) 0.000 0.000 0.0029(3) Ti1 0.0052(3) 0.0065(3) 0.0079(3) 0.000 0.000 0.0029(3) Ru1 0.0116(7) 0.0116(7) 0.0152(9) 0.000 0.000 0.0057(6) Ti2 0.0085(14) 0.0054(15) 0.0086(16) 0.000 0.000 0.0027(7) Os2 0.0085(14) 0.0054(15) 0.0086(16) 0.000 0.000 0.0027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 B3 2.2067(6) 1_556 ? Os1 B3 2.2067(6) . ? Os1 B2 2.338(13) 3 ? Os1 Ru1 2.7205(16) . ? Os1 Ru1 2.7205(16) 1_556 ? Os1 Ti2 2.7282(14) . ? Os1 Os2 2.7282(14) 1_556 ? Os1 Ti2 2.7282(14) 1_556 ? Os1 Os1 2.7761(14) 3_665 ? Os1 Ti1 2.7761(14) 3_665 ? Os1 Os1 2.7761(14) 2_655 ? Ru1 B1 2.1596(16) 1_554 ? Ru1 B1 2.1596(16) . ? Ru1 B2 2.308(15) 3_554 ? Ru1 B2 2.308(15) 1_554 ? Ru1 B2 2.308(15) . ? Ru1 B2 2.308(15) 3 ? Ru1 Ru1 2.663(4) 3 ? Ru1 Ru1 2.663(4) 2 ? Ru1 Os1 2.7205(16) 7_556 ? Ru1 Ti1 2.7205(16) 7_556 ? Ti2 B2 2.37(2) 3_554 ? Ti2 B2 2.37(2) 3 ? Ti2 B3 2.6551(12) 7_545 ? Ti2 B3 2.6551(12) . ? Ti2 Ti1 2.7282(14) 8 ? Ti2 Os1 2.7282(14) 8 ? Ti2 Ti1 2.7282(14) 8_556 ? Ti2 Os1 2.7282(14) 8_556 ? Ti2 Os1 2.7282(14) 1_554 ? Ti2 Ti1 2.7282(14) 1_554 ? B1 B2 1.89(3) 2 ? B1 B2 1.89(3) . ? B1 B2 1.89(3) 3 ? B1 Ru1 2.1596(16) 1_556 ? B1 Ru1 2.1596(16) 2 ? B1 Ru1 2.1596(16) 3 ? B1 Ru1 2.1596(16) 2_556 ? B1 Ru1 2.1596(16) 3_556 ? B2 Ru1 2.308(15) 2 ? B2 Ru1 2.308(15) 1_556 ? B2 Ru1 2.308(15) 2_556 ? B2 Os1 2.338(13) 7_556 ? B2 Ti1 2.338(13) 7_556 ? B2 Os1 2.338(13) 2 ? B2 Ti1 2.338(13) 2 ? B2 Os2 2.37(2) 2_556 ? B2 Ti2 2.37(2) 2_556 ? B2 Ti2 2.37(2) 2 ? B3 Ti1 2.2067(6) 2_654 ? B3 Os1 2.2067(6) 2_654 ? B3 Ti1 2.2067(6) 2_655 ? B3 Os1 2.2067(6) 2_655 ? B3 Ti1 2.2067(6) 3_665 ? B3 Os1 2.2067(6) 3_665 ? B3 Os1 2.2067(6) 1_554 ? B3 Ti1 2.2067(6) 1_554 ? B3 Ti1 2.2067(6) 3_664 ? B3 Os1 2.2067(6) 3_664 ? 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 B3 Os1 B3 86.84(3) 1_556 . ? B3 Os1 B2 118.7(4) 1_556 3 ? B3 Os1 B2 118.7(4) . 3 ? B3 Os1 Ru1 169.92(4) 1_556 . ? B3 Os1 Ru1 102.60(2) . . ? B2 Os1 Ru1 53.6(5) 3 . ? B3 Os1 Ru1 102.60(2) 1_556 1_556 ? B3 Os1 Ru1 169.92(4) . 1_556 ? B2 Os1 Ru1 53.6(5) 3 1_556 ? Ru1 Os1 Ru1 67.77(5) . 1_556 ? B3 Os1 Ti2 109.10(8) 1_556 . ? B3 Os1 Ti2 64.08(6) . . ? B2 Os1 Ti2 55.2(5) 3 . ? Ru1 Os1 Ti2 72.68(8) . . ? Ru1 Os1 Ti2 108.80(8) 1_556 . ? B3 Os1 Os2 64.08(6) 1_556 1_556 ? B3 Os1 Os2 109.10(8) . 1_556 ? B2 Os1 Os2 55.2(5) 3 1_556 ? Ru1 Os1 Os2 108.80(8) . 1_556 ? Ru1 Os1 Os2 72.68(8) 1_556 1_556 ? Ti2 Os1 Os2 67.56(4) . 1_556 ? B3 Os1 Ti2 64.08(6) 1_556 1_556 ? B3 Os1 Ti2 109.10(8) . 1_556 ? B2 Os1 Ti2 55.2(5) 3 1_556 ? Ru1 Os1 Ti2 108.80(8) . 1_556 ? Ru1 Os1 Ti2 72.68(8) 1_556 1_556 ? Ti2 Os1 Ti2 67.56(4) . 1_556 ? Os2 Os1 Ti2 0.0 1_556 1_556 ? B3 Os1 Os1 51.023(12) 1_556 3_665 ? B3 Os1 Os1 51.023(12) . 3_665 ? B2 Os1 Os1 161.4(7) 3 3_665 ? Ru1 Os1 Os1 138.37(4) . 3_665 ? Ru1 Os1 Os1 138.37(4) 1_556 3_665 ? Ti2 Os1 Os1 110.39(8) . 3_665 ? Os2 Os1 Os1 110.39(8) 1_556 3_665 ? Ti2 Os1 Os1 110.39(8) 1_556 3_665 ? B3 Os1 Ti1 51.023(12) 1_556 3_665 ? B3 Os1 Ti1 51.023(12) . 3_665 ? B2 Os1 Ti1 161.4(7) 3 3_665 ? Ru1 Os1 Ti1 138.37(4) . 3_665 ? Ru1 Os1 Ti1 138.37(4) 1_556 3_665 ? Ti2 Os1 Ti1 110.39(8) . 3_665 ? Os2 Os1 Ti1 110.39(8) 1_556 3_665 ? Ti2 Os1 Ti1 110.39(8) 1_556 3_665 ? Os1 Os1 Ti1 0.00(5) 3_665 3_665 ? B3 Os1 Os1 51.023(12) 1_556 2_655 ? B3 Os1 Os1 51.023(12) . 2_655 ? B2 Os1 Os1 101.4(7) 3 2_655 ? Ru1 Os1 Os1 133.36(3) . 2_655 ? Ru1 Os1 Os1 133.36(3) 1_556 2_655 ? Ti2 Os1 Os1 61.36(8) . 2_655 ? Os2 Os1 Os1 61.36(8) 1_556 2_655 ? Ti2 Os1 Os1 61.36(8) 1_556 2_655 ? Os1 Os1 Os1 60.0 3_665 2_655 ? Ti1 Os1 Os1 60.0 3_665 2_655 ? B1 Ru1 B1 89.23(8) 1_554 . ? B1 Ru1 B2 49.9(7) 1_554 3_554 ? B1 Ru1 B2 106.18(19) . 3_554 ? B1 Ru1 B2 49.9(7) 1_554 1_554 ? B1 Ru1 B2 106.18(19) . 1_554 ? B2 Ru1 B2 90.2(11) 3_554 1_554 ? B1 Ru1 B2 106.18(19) 1_554 . ? B1 Ru1 B2 49.9(7) . . ? B2 Ru1 B2 150.2(10) 3_554 . ? B2 Ru1 B2 82.2(6) 1_554 . ? B1 Ru1 B2 106.18(19) 1_554 3 ? B1 Ru1 B2 49.9(7) . 3 ? B2 Ru1 B2 82.2(6) 3_554 3 ? B2 Ru1 B2 150.2(10) 1_554 3 ? B2 Ru1 B2 90.2(11) . 3 ? B1 Ru1 Ru1 51.94(3) 1_554 3 ? B1 Ru1 Ru1 51.94(3) . 3 ? B2 Ru1 Ru1 54.8(3) 3_554 3 ? B2 Ru1 Ru1 97.6(6) 1_554 3 ? B2 Ru1 Ru1 97.6(6) . 3 ? B2 Ru1 Ru1 54.8(3) 3 3 ? B1 Ru1 Ru1 51.94(3) 1_554 2 ? B1 Ru1 Ru1 51.94(3) . 2 ? B2 Ru1 Ru1 97.6(6) 3_554 2 ? B2 Ru1 Ru1 54.8(3) 1_554 2 ? B2 Ru1 Ru1 54.8(3) . 2 ? B2 Ru1 Ru1 97.6(6) 3 2 ? Ru1 Ru1 Ru1 60.0 3 2 ? B1 Ru1 Os1 147.773(18) 1_554 7_556 ? B1 Ru1 Os1 93.599(18) . 7_556 ? B2 Ru1 Os1 155.0(5) 3_554 7_556 ? B2 Ru1 Os1 98.9(7) 1_554 7_556 ? B2 Ru1 Os1 54.7(5) . 7_556 ? B2 Ru1 Os1 100.00(5) 3 7_556 ? Ru1 Ru1 Os1 144.90(3) 3 7_556 ? Ru1 Ru1 Os1 106.70(4) 2 7_556 ? B1 Ru1 Ti1 147.773(18) 1_554 7_556 ? B1 Ru1 Ti1 93.599(18) . 7_556 ? B2 Ru1 Ti1 155.0(5) 3_554 7_556 ? B2 Ru1 Ti1 98.9(7) 1_554 7_556 ? B2 Ru1 Ti1 54.7(5) . 7_556 ? B2 Ru1 Ti1 100.00(5) 3 7_556 ? Ru1 Ru1 Ti1 144.90(3) 3 7_556 ? Ru1 Ru1 Ti1 106.70(4) 2 7_556 ? Os1 Ru1 Ti1 0.00(3) 7_556 7_556 ? B1 Ru1 Os1 147.773(18) 1_554 . ? B1 Ru1 Os1 93.599(18) . . ? B2 Ru1 Os1 98.9(7) 3_554 . ? B2 Ru1 Os1 155.0(5) 1_554 . ? B2 Ru1 Os1 100.00(5) . . ? B2 Ru1 Os1 54.7(5) 3 . ? Ru1 Ru1 Os1 106.70(4) 3 . ? Ru1 Ru1 Os1 144.90(3) 2 . ? Os1 Ru1 Os1 64.12(5) 7_556 . ? Ti1 Ru1 Os1 64.12(5) 7_556 . ? B2 Ti2 B2 79.5(10) 3_554 3 ? B2 Ti2 B3 101.99(10) 3_554 7_545 ? B2 Ti2 B3 101.99(10) 3 7_545 ? B2 Ti2 B3 101.99(10) 3_554 . ? B2 Ti2 B3 101.99(10) 3 . ? B3 Ti2 B3 148.64(17) 7_545 . ? B2 Ti2 Ti1 54.02(15) 3_554 8 ? B2 Ti2 Ti1 97.1(3) 3 8 ? B3 Ti2 Ti1 48.376(15) 7_545 8 ? B3 Ti2 Ti1 145.816(16) . 8 ? B2 Ti2 Os1 54.02(15) 3_554 8 ? B2 Ti2 Os1 97.1(3) 3 8 ? B3 Ti2 Os1 48.376(15) 7_545 8 ? B3 Ti2 Os1 145.816(16) . 8 ? Ti1 Ti2 Os1 0.00(3) 8 8 ? B2 Ti2 Os1 97.1(3) 3_554 . ? B2 Ti2 Os1 54.02(15) 3 . ? B3 Ti2 Os1 145.816(16) 7_545 . ? B3 Ti2 Os1 48.376(15) . . ? Ti1 Ti2 Os1 144.90(17) 8 . ? Os1 Ti2 Os1 144.90(17) 8 . ? B2 Ti2 Ti1 97.1(3) 3_554 8_556 ? B2 Ti2 Ti1 54.02(15) 3 8_556 ? B3 Ti2 Ti1 48.376(15) 7_545 8_556 ? B3 Ti2 Ti1 145.816(16) . 8_556 ? Ti1 Ti2 Ti1 67.56(4) 8 8_556 ? Os1 Ti2 Ti1 67.56(4) 8 8_556 ? Os1 Ti2 Ti1 101.53(7) . 8_556 ? B2 Ti2 Os1 97.1(3) 3_554 8_556 ? B2 Ti2 Os1 54.02(15) 3 8_556 ? B3 Ti2 Os1 48.376(15) 7_545 8_556 ? B3 Ti2 Os1 145.816(16) . 8_556 ? Ti1 Ti2 Os1 67.56(4) 8 8_556 ? Os1 Ti2 Os1 67.56(4) 8 8_556 ? Os1 Ti2 Os1 101.53(7) . 8_556 ? Ti1 Ti2 Os1 0.00(3) 8_556 8_556 ? B2 Ti2 Os1 54.02(15) 3_554 1_554 ? B2 Ti2 Os1 97.1(3) 3 1_554 ? B3 Ti2 Os1 145.816(16) 7_545 1_554 ? B3 Ti2 Os1 48.376(15) . 1_554 ? Ti1 Ti2 Os1 101.53(7) 8 1_554 ? Os1 Ti2 Os1 101.53(7) 8 1_554 ? Os1 Ti2 Os1 67.56(4) . 1_554 ? Ti1 Ti2 Os1 144.90(17) 8_556 1_554 ? Os1 Ti2 Os1 144.90(17) 8_556 1_554 ? B2 Ti2 Ti1 54.02(15) 3_554 1_554 ? B2 Ti2 Ti1 97.1(3) 3 1_554 ? B3 Ti2 Ti1 145.816(16) 7_545 1_554 ? B3 Ti2 Ti1 48.376(15) . 1_554 ? Ti1 Ti2 Ti1 101.53(7) 8 1_554 ? Os1 Ti2 Ti1 101.53(7) 8 1_554 ? Os1 Ti2 Ti1 67.56(4) . 1_554 ? Ti1 Ti2 Ti1 144.90(17) 8_556 1_554 ? Os1 Ti2 Ti1 144.90(17) 8_556 1_554 ? Os1 Ti2 Ti1 0.00(3) 1_554 1_554 ? B2 B1 B2 120.000(2) 2 . ? B2 B1 B2 120.000(1) 2 3 ? B2 B1 B2 120.000(3) . 3 ? B2 B1 Ru1 135.38(4) 2 1_556 ? B2 B1 Ru1 69.150(16) . 1_556 ? B2 B1 Ru1 69.150(16) 3 1_556 ? B2 B1 Ru1 69.150(16) 2 2 ? B2 B1 Ru1 69.150(16) . 2 ? B2 B1 Ru1 135.38(4) 3 2 ? Ru1 B1 Ru1 138.30(3) 1_556 2 ? B2 B1 Ru1 69.150(16) 2 3 ? B2 B1 Ru1 135.38(4) . 3 ? B2 B1 Ru1 69.150(16) 3 3 ? Ru1 B1 Ru1 138.30(3) 1_556 3 ? Ru1 B1 Ru1 76.12(6) 2 3 ? B2 B1 Ru1 69.150(16) 2 2_556 ? B2 B1 Ru1 69.150(16) . 2_556 ? B2 B1 Ru1 135.38(4) 3 2_556 ? Ru1 B1 Ru1 76.12(6) 1_556 2_556 ? Ru1 B1 Ru1 89.23(8) 2 2_556 ? Ru1 B1 Ru1 138.30(3) 3 2_556 ? B2 B1 Ru1 69.150(16) 2 3_556 ? B2 B1 Ru1 135.38(4) . 3_556 ? B2 B1 Ru1 69.150(16) 3 3_556 ? Ru1 B1 Ru1 76.12(6) 1_556 3_556 ? Ru1 B1 Ru1 138.30(3) 2 3_556 ? Ru1 B1 Ru1 89.23(8) 3 3_556 ? Ru1 B1 Ru1 76.12(6) 2_556 3_556 ? B2 B1 Ru1 135.38(4) 2 . ? B2 B1 Ru1 69.150(16) . . ? B2 B1 Ru1 69.150(16) 3 . ? Ru1 B1 Ru1 89.23(8) 1_556 . ? Ru1 B1 Ru1 76.12(6) 2 . ? Ru1 B1 Ru1 76.12(6) 3 . ? Ru1 B1 Ru1 138.30(3) 2_556 . ? Ru1 B1 Ru1 138.30(3) 3_556 . ? B1 B2 Ru1 61.0(7) . 2 ? B1 B2 Ru1 61.0(7) . 1_556 ? Ru1 B2 Ru1 122.0(13) 2 1_556 ? B1 B2 Ru1 61.0(7) . 2_556 ? Ru1 B2 Ru1 82.2(6) 2 2_556 ? Ru1 B2 Ru1 70.5(5) 1_556 2_556 ? B1 B2 Ru1 61.0(7) . . ? Ru1 B2 Ru1 70.5(5) 2 . ? Ru1 B2 Ru1 82.2(6) 1_556 . ? Ru1 B2 Ru1 122.0(13) 2_556 . ? B1 B2 Os1 115.3(7) . 7_556 ? Ru1 B2 Os1 136.79(11) 2 7_556 ? Ru1 B2 Os1 71.69(6) 1_556 7_556 ? Ru1 B2 Os1 136.79(11) 2_556 7_556 ? Ru1 B2 Os1 71.69(6) . 7_556 ? B1 B2 Ti1 115.3(7) . 7_556 ? Ru1 B2 Ti1 136.79(11) 2 7_556 ? Ru1 B2 Ti1 71.69(6) 1_556 7_556 ? Ru1 B2 Ti1 136.79(11) 2_556 7_556 ? Ru1 B2 Ti1 71.69(6) . 7_556 ? Os1 B2 Ti1 0.00(4) 7_556 7_556 ? B1 B2 Os1 115.3(7) . 2 ? Ru1 B2 Os1 71.69(6) 2 2 ? Ru1 B2 Os1 136.79(11) 1_556 2 ? Ru1 B2 Os1 71.69(6) 2_556 2 ? Ru1 B2 Os1 136.79(11) . 2 ? Os1 B2 Os1 129.4(14) 7_556 2 ? Ti1 B2 Os1 129.4(14) 7_556 2 ? B1 B2 Ti1 115.3(7) . 2 ? Ru1 B2 Ti1 71.69(6) 2 2 ? Ru1 B2 Ti1 136.79(11) 1_556 2 ? Ru1 B2 Ti1 71.69(6) 2_556 2 ? Ru1 B2 Ti1 136.79(11) . 2 ? Os1 B2 Ti1 129.4(14) 7_556 2 ? Ti1 B2 Ti1 129.4(14) 7_556 2 ? Os1 B2 Ti1 0.0 2 2 ? B1 B2 Os2 140.2(5) . 2_556 ? Ru1 B2 Os2 142.5(6) 2 2_556 ? Ru1 B2 Os2 87.3(2) 1_556 2_556 ? Ru1 B2 Os2 87.3(2) 2_556 2_556 ? Ru1 B2 Os2 142.5(6) . 2_556 ? Os1 B2 Os2 70.8(6) 7_556 2_556 ? Ti1 B2 Os2 70.8(6) 7_556 2_556 ? Os1 B2 Os2 70.8(6) 2 2_556 ? Ti1 B2 Os2 70.8(6) 2 2_556 ? B1 B2 Ti2 140.2(5) . 2_556 ? Ru1 B2 Ti2 142.5(6) 2 2_556 ? Ru1 B2 Ti2 87.3(2) 1_556 2_556 ? Ru1 B2 Ti2 87.3(2) 2_556 2_556 ? Ru1 B2 Ti2 142.5(6) . 2_556 ? Os1 B2 Ti2 70.8(6) 7_556 2_556 ? Ti1 B2 Ti2 70.8(6) 7_556 2_556 ? Os1 B2 Ti2 70.8(6) 2 2_556 ? Ti1 B2 Ti2 70.8(6) 2 2_556 ? Os2 B2 Ti2 0.0 2_556 2_556 ? B1 B2 Ti2 140.2(5) . 2 ? Ru1 B2 Ti2 87.3(2) 2 2 ? Ru1 B2 Ti2 142.5(6) 1_556 2 ? Ru1 B2 Ti2 142.5(6) 2_556 2 ? Ru1 B2 Ti2 87.3(2) . 2 ? Os1 B2 Ti2 70.8(6) 7_556 2 ? Ti1 B2 Ti2 70.8(6) 7_556 2 ? Os1 B2 Ti2 70.8(6) 2 2 ? Ti1 B2 Ti2 70.8(6) 2 2 ? Os2 B2 Ti2 79.5(10) 2_556 2 ? Ti2 B2 Ti2 79.5(10) 2_556 2 ? Ti1 B3 Os1 0.00(4) 2_654 2_654 ? Ti1 B3 Ti1 86.84(3) 2_654 2_655 ? Os1 B3 Ti1 86.84(3) 2_654 2_655 ? Ti1 B3 Os1 86.84(3) 2_654 2_655 ? Os1 B3 Os1 86.84(3) 2_654 2_655 ? Ti1 B3 Os1 0.00(3) 2_655 2_655 ? Ti1 B3 Ti1 137.411(12) 2_654 3_665 ? Os1 B3 Ti1 137.411(12) 2_654 3_665 ? Ti1 B3 Ti1 77.95(2) 2_655 3_665 ? Os1 B3 Ti1 77.95(2) 2_655 3_665 ? Ti1 B3 Os1 137.411(12) 2_654 3_665 ? Os1 B3 Os1 137.411(12) 2_654 3_665 ? Ti1 B3 Os1 77.95(2) 2_655 3_665 ? Os1 B3 Os1 77.95(2) 2_655 3_665 ? Ti1 B3 Os1 0.00(4) 3_665 3_665 ? Ti1 B3 Os1 77.95(2) 2_654 1_554 ? Os1 B3 Os1 77.95(2) 2_654 1_554 ? Ti1 B3 Os1 137.411(12) 2_655 1_554 ? Os1 B3 Os1 137.411(12) 2_655 1_554 ? Ti1 B3 Os1 137.411(12) 3_665 1_554 ? Os1 B3 Os1 137.411(12) 3_665 1_554 ? Ti1 B3 Ti1 77.95(2) 2_654 1_554 ? Os1 B3 Ti1 77.95(2) 2_654 1_554 ? Ti1 B3 Ti1 137.411(12) 2_655 1_554 ? Os1 B3 Ti1 137.411(12) 2_655 1_554 ? Ti1 B3 Ti1 137.411(12) 3_665 1_554 ? Os1 B3 Ti1 137.411(12) 3_665 1_554 ? Os1 B3 Ti1 0.00(4) 1_554 1_554 ? Ti1 B3 Ti1 77.95(2) 2_654 3_664 ? Os1 B3 Ti1 77.95(2) 2_654 3_664 ? Ti1 B3 Ti1 137.411(12) 2_655 3_664 ? Os1 B3 Ti1 137.411(12) 2_655 3_664 ? Ti1 B3 Ti1 86.84(3) 3_665 3_664 ? Os1 B3 Ti1 86.84(3) 3_665 3_664 ? Os1 B3 Ti1 77.95(2) 1_554 3_664 ? Ti1 B3 Ti1 77.95(2) 1_554 3_664 ? Ti1 B3 Os1 77.95(2) 2_654 3_664 ? Os1 B3 Os1 77.95(2) 2_654 3_664 ? Ti1 B3 Os1 137.411(12) 2_655 3_664 ? Os1 B3 Os1 137.411(12) 2_655 3_664 ? Ti1 B3 Os1 86.84(3) 3_665 3_664 ? Os1 B3 Os1 86.84(3) 3_665 3_664 ? Os1 B3 Os1 77.95(2) 1_554 3_664 ? Ti1 B3 Os1 77.95(2) 1_554 3_664 ? Ti1 B3 Os1 0.00(4) 3_664 3_664 ? Ti1 B3 Os1 137.411(12) 2_654 . ? Os1 B3 Os1 137.411(12) 2_654 . ? Ti1 B3 Os1 77.95(2) 2_655 . ? Os1 B3 Os1 77.95(2) 2_655 . ? Ti1 B3 Os1 77.95(2) 3_665 . ? Os1 B3 Os1 77.95(2) 3_665 . ? Os1 B3 Os1 86.84(3) 1_554 . ? Ti1 B3 Os1 86.84(3) 1_554 . ? Ti1 B3 Os1 137.411(12) 3_664 . ? Os1 B3 Os1 137.411(12) 3_664 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 35.98 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.045 _refine_diff_density_min -2.740 _refine_diff_density_rms 0.599