# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_curucl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Cl2 Cu K2 Li O19 Ru2' _chemical_formula_sum 'C4 H4 Cl2 Cu K2 Li O19 Ru2' _chemical_formula_weight 777.7932 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/ncm' _symmetry_space_group_name_Hall '-P 4ac 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z+1/2' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z' '-x, y+1/2, -z+1/2' '-y, -x, -z' '-x, -y, -z' 'y-1/2, -x, -z-1/2' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z' 'x, -y-1/2, z-1/2' 'y, x, z' _cell_length_a 11.061(2) _cell_length_b 11.061(2) _cell_length_c 17.145(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2097.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 3.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5704 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16356 _diffrn_reflns_av_R_equivalents 0.1494 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1008 _reflns_number_gt 881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0939P)^2^+20.3942P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1008 _refine_ls_number_parameters 84 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ru1 Ru 0.53110(6) 0.53110(6) 0.94024(5) 0.0144(4) Uani 1 2 d S . . Cu1 Cu 0.5000 1.0000 1.0000 0.0158(5) Uani 1 4 d S . . Cl1 Cl 0.6083(2) 0.6083(2) 0.80806(18) 0.0308(8) Uani 1 2 d S . . O1 O 0.5202(6) 0.7042(6) 0.9778(3) 0.0260(15) Uani 1 1 d . . . O2 O 0.4581(6) 0.6440(5) 1.0964(3) 0.0220(14) Uani 1 1 d . . . O3 O 0.4714(6) 0.8373(6) 1.0687(4) 0.0344(18) Uani 1 1 d . . . O4 O 0.5892(6) 0.9108(6) 0.9167(5) 0.0200(19) Uani 1 2 d SD . . C1 C 0.4831(9) 0.7296(9) 1.0486(5) 0.026(2) Uani 1 1 d . . . O6 O 0.2500 0.2500 0.8617(10) 0.080(7) Uani 1 4 d S . . O5 O 0.3074(6) 0.6151(6) 0.6879(4) 0.0357(17) Uani 1 1 d . . . K1 K 0.3978(2) 0.3978(2) 0.75828(19) 0.0437(9) Uani 1 2 d S . . Li1 Li 0.2500 0.7500 0.7500 0.039(8) Uani 1 4 d S . . H1 H 0.661(3) 0.932(7) 0.929(4) 0.01(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0143(4) 0.0143(4) 0.0145(6) 0.0012(3) 0.0012(3) -0.0006(3) Cu1 0.0150(7) 0.0150(7) 0.0173(11) -0.0013(6) 0.0013(6) -0.0002(8) Cl1 0.0342(12) 0.0342(12) 0.0241(16) 0.0077(10) 0.0077(10) 0.0009(15) O1 0.036(4) 0.020(3) 0.022(3) 0.000(3) 0.004(3) -0.004(3) O2 0.030(4) 0.016(3) 0.019(3) -0.003(3) 0.005(3) -0.002(3) O3 0.045(5) 0.022(4) 0.035(4) -0.007(3) 0.014(3) -0.002(3) O4 0.018(3) 0.018(3) 0.023(5) 0.003(3) -0.003(3) -0.001(4) C1 0.028(5) 0.024(5) 0.025(5) -0.011(4) 0.008(4) -0.007(4) O6 0.093(11) 0.093(11) 0.054(11) 0.000 0.000 -0.052(13) O5 0.032(4) 0.040(4) 0.035(4) -0.007(3) 0.006(3) -0.001(3) K1 0.0505(14) 0.0505(14) 0.0301(17) -0.0015(11) -0.0015(11) -0.0054(18) Li1 0.035(12) 0.035(12) 0.05(2) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.023(6) 16 ? Ru1 O1 2.023(6) . ? Ru1 O2 2.040(6) 8_667 ? Ru1 O2 2.040(6) 9_667 ? Ru1 Ru1 2.2683(18) 9_667 ? Ru1 Cl1 2.568(3) . ? Ru1 K1 3.753(4) . ? Cu1 O4 1.997(9) . ? Cu1 O4 1.997(9) 9_677 ? Cu1 O3 2.174(7) 14_775 ? Cu1 O3 2.174(7) 6_457 ? Cu1 O3 2.174(7) . ? Cu1 O3 2.174(7) 9_677 ? Cl1 K1 3.402(5) . ? Cl1 K1 3.398(4) 12_667 ? Cl1 K1 3.398(4) 10_667 ? O1 C1 1.313(10) . ? O2 C1 1.282(11) . ? O2 Ru1 2.040(6) 9_667 ? O2 K1 2.993(7) 9_667 ? O3 C1 1.246(12) . ? O4 K1 3.007(9) 12_667 ? O4 H1 0.86(2) . ? O6 K1 2.913(11) 3 ? O6 K1 2.913(11) . ? O5 Li1 1.940(6) . ? O5 K1 2.870(7) . ? K1 O5 2.870(7) 16 ? K1 O2 2.993(7) 8_667 ? K1 O2 2.993(7) 9_667 ? K1 O4 3.007(9) 10_567 ? K1 Cl1 3.398(4) 10_567 ? K1 Cl1 3.398(4) 12_657 ? K1 Li1 4.2275(16) 5_566 ? K1 Li1 4.2275(16) . ? Li1 O5 1.940(7) 12_667 ? Li1 O5 1.940(7) 10_567 ? Li1 O5 1.940(6) 3_565 ? Li1 K1 4.2275(16) 10_567 ? Li1 K1 4.2275(16) 12_667 ? Li1 K1 4.2275(16) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O1 90.7(4) 16 . ? O1 Ru1 O2 179.4(2) 16 8_667 ? O1 Ru1 O2 89.2(3) . 8_667 ? O1 Ru1 O2 89.2(3) 16 9_667 ? O1 Ru1 O2 179.4(2) . 9_667 ? O2 Ru1 O2 90.9(4) 8_667 9_667 ? O1 Ru1 Ru1 88.94(17) 16 9_667 ? O1 Ru1 Ru1 88.94(17) . 9_667 ? O2 Ru1 Ru1 90.48(17) 8_667 9_667 ? O2 Ru1 Ru1 90.48(17) 9_667 9_667 ? O1 Ru1 Cl1 89.20(18) 16 . ? O1 Ru1 Cl1 89.20(18) . . ? O2 Ru1 Cl1 91.38(17) 8_667 . ? O2 Ru1 Cl1 91.38(17) 9_667 . ? Ru1 Ru1 Cl1 177.35(11) 9_667 . ? O1 Ru1 K1 127.80(17) 16 . ? O1 Ru1 K1 127.80(17) . . ? O2 Ru1 K1 52.66(17) 8_667 . ? O2 Ru1 K1 52.66(17) 9_667 . ? Ru1 Ru1 K1 120.84(8) 9_667 . ? Cl1 Ru1 K1 61.82(10) . . ? O4 Cu1 O4 180.000(1) . 9_677 ? O4 Cu1 O3 92.9(2) . 14_775 ? O4 Cu1 O3 87.1(2) 9_677 14_775 ? O4 Cu1 O3 87.1(2) . 6_457 ? O4 Cu1 O3 92.9(2) 9_677 6_457 ? O3 Cu1 O3 180.000(1) 14_775 6_457 ? O4 Cu1 O3 92.9(2) . . ? O4 Cu1 O3 87.1(2) 9_677 . ? O3 Cu1 O3 87.0(4) 14_775 . ? O3 Cu1 O3 93.0(4) 6_457 . ? O4 Cu1 O3 87.1(2) . 9_677 ? O4 Cu1 O3 92.9(2) 9_677 9_677 ? O3 Cu1 O3 93.0(4) 14_775 9_677 ? O3 Cu1 O3 87.0(4) 6_457 9_677 ? O3 Cu1 O3 180.000(2) . 9_677 ? Ru1 Cl1 K1 76.48(10) . . ? Ru1 Cl1 K1 127.02(9) . 12_667 ? K1 Cl1 K1 123.19(8) . 12_667 ? Ru1 Cl1 K1 127.02(9) . 10_667 ? K1 Cl1 K1 123.19(8) . 10_667 ? K1 Cl1 K1 85.70(13) 12_667 10_667 ? C1 O1 Ru1 121.0(6) . . ? C1 O2 Ru1 119.4(5) . 9_667 ? C1 O2 K1 122.1(6) . 9_667 ? Ru1 O2 K1 94.5(2) 9_667 9_667 ? C1 O3 Cu1 128.9(6) . . ? Cu1 O4 K1 139.6(4) . 12_667 ? Cu1 O4 H1 98(5) . . ? K1 O4 H1 102(5) 12_667 . ? O3 C1 O2 120.5(8) . . ? O3 C1 O1 119.4(9) . . ? O2 C1 O1 120.0(8) . . ? K1 O6 K1 105.0(6) 3 . ? Li1 O5 K1 121.8(3) . . ? O5 K1 O5 114.0(3) . 16 ? O5 K1 O6 122.05(16) . . ? O5 K1 O6 122.05(16) 16 . ? O5 K1 O2 81.38(18) . 8_667 ? O5 K1 O2 131.7(2) 16 8_667 ? O6 K1 O2 72.9(3) . 8_667 ? O5 K1 O2 131.7(2) . 9_667 ? O5 K1 O2 81.38(18) 16 9_667 ? O6 K1 O2 72.9(3) . 9_667 ? O2 K1 O2 58.1(2) 8_667 9_667 ? O5 K1 O4 63.69(16) . 10_567 ? O5 K1 O4 63.69(16) 16 10_567 ? O6 K1 O4 131.4(3) . 10_567 ? O2 K1 O4 144.30(17) 8_667 10_567 ? O2 K1 O4 144.30(17) 9_667 10_567 ? O5 K1 Cl1 76.73(17) . . ? O5 K1 Cl1 76.73(17) 16 . ? O6 K1 Cl1 128.0(3) . . ? O2 K1 Cl1 62.11(14) 8_667 . ? O2 K1 Cl1 62.11(14) 9_667 . ? O4 K1 Cl1 100.6(2) 10_567 . ? O5 K1 Cl1 63.10(15) . 10_567 ? O5 K1 Cl1 129.91(18) 16 10_567 ? O6 K1 Cl1 70.4(2) . 10_567 ? O2 K1 Cl1 98.26(13) 8_667 10_567 ? O2 K1 Cl1 141.02(17) 9_667 10_567 ? O4 K1 Cl1 73.28(15) 10_567 10_567 ? Cl1 K1 Cl1 137.93(7) . 10_567 ? O5 K1 Cl1 129.91(18) . 12_657 ? O5 K1 Cl1 63.10(15) 16 12_657 ? O6 K1 Cl1 70.4(2) . 12_657 ? O2 K1 Cl1 141.02(17) 8_667 12_657 ? O2 K1 Cl1 98.26(13) 9_667 12_657 ? O4 K1 Cl1 73.28(15) 10_567 12_657 ? Cl1 K1 Cl1 137.93(7) . 12_657 ? Cl1 K1 Cl1 81.43(13) 10_567 12_657 ? O5 K1 Ru1 99.05(16) . . ? O5 K1 Ru1 99.05(16) 16 . ? O6 K1 Ru1 86.3(3) . . ? O2 K1 Ru1 32.80(12) 8_667 . ? O2 K1 Ru1 32.80(12) 9_667 . ? O4 K1 Ru1 142.3(2) 10_567 . ? Cl1 K1 Ru1 41.70(7) . . ? Cl1 K1 Ru1 131.01(8) 10_567 . ? Cl1 K1 Ru1 131.01(8) 12_657 . ? O5 K1 Li1 129.10(18) . 5_566 ? O5 K1 Li1 22.95(13) 16 5_566 ? O6 K1 Li1 108.70(8) . 5_566 ? O2 K1 Li1 112.09(14) 8_667 5_566 ? O2 K1 Li1 58.49(12) 9_667 5_566 ? O4 K1 Li1 86.61(8) 10_567 5_566 ? Cl1 K1 Li1 69.03(5) . 5_566 ? Cl1 K1 Li1 148.15(10) 10_567 5_566 ? Cl1 K1 Li1 69.06(5) 12_657 5_566 ? Ru1 K1 Li1 79.49(5) . 5_566 ? O5 K1 Li1 22.95(13) . . ? O5 K1 Li1 129.10(18) 16 . ? O6 K1 Li1 108.70(8) . . ? O2 K1 Li1 58.49(12) 8_667 . ? O2 K1 Li1 112.09(14) 9_667 . ? O4 K1 Li1 86.61(8) 10_567 . ? Cl1 K1 Li1 69.03(5) . . ? Cl1 K1 Li1 69.06(5) 10_567 . ? Cl1 K1 Li1 148.15(10) 12_657 . ? Ru1 K1 Li1 79.49(5) . . ? Li1 K1 Li1 135.35(10) 5_566 . ? O5 Li1 O5 107.5(2) 12_667 . ? O5 Li1 O5 113.4(4) 12_667 10_567 ? O5 Li1 O5 107.5(2) . 10_567 ? O5 Li1 O5 107.5(2) 12_667 3_565 ? O5 Li1 O5 113.4(4) . 3_565 ? O5 Li1 O5 107.5(2) 10_567 3_565 ? O5 Li1 K1 148.6(2) 12_667 10_567 ? O5 Li1 K1 89.2(2) . 10_567 ? O5 Li1 K1 35.2(2) 10_567 10_567 ? O5 Li1 K1 88.7(2) 3_565 10_567 ? O5 Li1 K1 35.2(2) 12_667 12_667 ? O5 Li1 K1 88.7(2) . 12_667 ? O5 Li1 K1 148.6(2) 10_567 12_667 ? O5 Li1 K1 89.2(2) 3_565 12_667 ? K1 Li1 K1 176.15(9) 10_567 12_667 ? O5 Li1 K1 88.7(2) 12_667 3_565 ? O5 Li1 K1 148.6(2) . 3_565 ? O5 Li1 K1 89.2(2) 10_567 3_565 ? O5 Li1 K1 35.2(2) 3_565 3_565 ? K1 Li1 K1 90.065(3) 10_567 3_565 ? K1 Li1 K1 90.065(3) 12_667 3_565 ? O5 Li1 K1 89.2(2) 12_667 . ? O5 Li1 K1 35.2(2) . . ? O5 Li1 K1 88.7(2) 10_567 . ? O5 Li1 K1 148.6(2) 3_565 . ? K1 Li1 K1 90.065(3) 10_567 . ? K1 Li1 K1 90.065(3) 12_667 . ? K1 Li1 K1 176.15(9) 3_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.992 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 942178' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pccn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Br2 Cu K2 Li O19 Ru2' _chemical_formula_sum 'C4 H4 Br2 Cu K2 Li O19 Ru2' _chemical_formula_weight 866.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 10.9758(9) _cell_length_b 11.2844(10) _cell_length_c 17.2476(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2136.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 6.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3831 _exptl_absorpt_correction_T_max 0.5584 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10043 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1901 _reflns_number_gt 1673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0316P)^2^+5.2341P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1901 _refine_ls_number_parameters 151 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _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 Ru1 Ru 0.47084(3) 0.53247(3) 0.440620(19) 0.01500(11) Uani 1 1 d . . . Cu1 Cu 0.0000 0.5000 0.5000 0.01977(18) Uani 1 2 d S . . Br1 Br 0.39208(4) 0.61401(4) 0.30212(3) 0.02883(14) Uani 1 1 d . . . K1 K 0.60213(11) 0.40356(11) 0.26051(7) 0.0385(3) Uani 1 1 d . . . Li1 Li 0.7500 0.7500 0.2502(7) 0.036(3) Uani 1 2 d S . . C1 C 0.2669(4) 0.4811(4) 0.5436(2) 0.0202(9) Uani 1 1 d . . . O1 O 0.5187(3) 0.2995(2) 0.52001(17) 0.0232(7) Uani 1 1 d . . . C2 C 0.4828(4) 0.2760(4) 0.4495(2) 0.0215(9) Uani 1 1 d . . . O2 O 0.4601(3) 0.3632(2) 0.40228(17) 0.0223(7) Uani 1 1 d . . . O3 O 0.3519(3) 0.4571(3) 0.59301(17) 0.0232(7) Uani 1 1 d . . . O4 O 0.2955(2) 0.5200(3) 0.47528(17) 0.0234(7) Uani 1 1 d . . . O5 O 0.1565(3) 0.4690(3) 0.56258(18) 0.0274(7) Uani 1 1 d . . . O6 O 0.0267(3) 0.3296(3) 0.42757(18) 0.0302(8) Uani 1 1 d . . . O7 O -0.0860(3) 0.4068(3) 0.58278(19) 0.0229(7) Uani 1 1 d D . . O8 O 0.6903(3) 0.6200(3) 0.1872(2) 0.0348(8) Uani 1 1 d . . . O9 O 0.3810(3) 0.3128(3) 0.1869(2) 0.0372(8) Uani 1 1 d . . . O10 O 0.7500 0.2500 0.3659(4) 0.084(2) Uani 1 2 d S . . H1 H -0.073(5) 0.339(3) 0.565(3) 0.044(17) Uiso 1 1 d D . . H2 H -0.160(2) 0.420(6) 0.574(4) 0.06(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01596(18) 0.01468(18) 0.01436(18) 0.00086(13) -0.00005(13) -0.00025(12) Cu1 0.0180(4) 0.0222(4) 0.0191(4) 0.0026(3) 0.0000(3) 0.0004(3) Br1 0.0314(3) 0.0300(3) 0.0251(3) 0.00712(19) -0.0060(2) -0.00169(19) K1 0.0408(7) 0.0412(7) 0.0334(6) -0.0030(5) 0.0066(5) 0.0043(5) Li1 0.037(7) 0.039(7) 0.031(6) 0.000 0.000 0.001(6) C1 0.022(2) 0.019(2) 0.019(2) -0.0016(17) 0.0000(18) -0.0004(17) O1 0.0343(17) 0.0161(15) 0.0192(16) -0.0006(12) -0.0069(13) 0.0016(13) C2 0.020(2) 0.022(2) 0.022(2) -0.0008(18) 0.0003(18) -0.0002(17) O2 0.0327(17) 0.0169(15) 0.0174(16) -0.0007(12) -0.0031(13) -0.0018(13) O3 0.0213(15) 0.0293(17) 0.0190(16) 0.0023(13) 0.0017(13) 0.0010(13) O4 0.0153(15) 0.0340(18) 0.0209(16) 0.0072(13) 0.0006(12) 0.0028(13) O5 0.0174(16) 0.040(2) 0.0248(17) 0.0084(14) 0.0044(13) 0.0001(13) O6 0.051(2) 0.0149(15) 0.0244(18) 0.0039(13) 0.0088(15) 0.0004(14) O7 0.0214(17) 0.0207(17) 0.0267(18) -0.0018(14) -0.0044(14) 0.0032(14) O8 0.037(2) 0.0303(19) 0.037(2) -0.0064(15) -0.0097(16) 0.0036(15) O9 0.0306(19) 0.042(2) 0.039(2) 0.0107(17) 0.0080(16) 0.0047(16) O10 0.082(5) 0.112(6) 0.059(4) 0.000 0.000 0.046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 2.017(3) 5_666 ? Ru1 O4 2.021(3) . ? Ru1 O2 2.025(3) . ? Ru1 O3 2.033(3) 5_666 ? Ru1 Ru1 2.2677(7) 5_666 ? Ru1 Br1 2.7018(6) . ? Ru1 K1 3.7205(12) . ? Cu1 O7 2.009(3) 5_566 ? Cu1 O7 2.009(3) . ? Cu1 O5 2.058(3) 5_566 ? Cu1 O5 2.058(3) . ? Cu1 O6 2.312(3) . ? Cu1 O6 2.312(3) 5_566 ? Br1 K1 3.3667(13) 4_465 ? Br1 K1 3.3867(13) . ? Br1 K1 3.4420(13) 3_655 ? K1 O8 2.916(4) . ? K1 O9 2.924(4) . ? K1 O2 2.935(3) . ? K1 O10 2.990(4) . ? K1 O3 3.018(3) 5_666 ? K1 O7 3.071(3) 8_655 ? K1 Br1 3.3667(13) 4_565 ? K1 Br1 3.4420(13) 3_645 ? K1 Li1 4.2366(14) . ? K1 Li1 4.2396(13) 3_645 ? Li1 O9 1.935(7) 4_565 ? Li1 O9 1.935(7) 3_655 ? Li1 O8 1.940(7) . ? Li1 O8 1.940(7) 2_665 ? Li1 K1 4.2366(14) 2_665 ? Li1 K1 4.2396(13) 3_655 ? Li1 K1 4.2396(14) 4_565 ? C1 O5 1.263(5) . ? C1 O4 1.296(5) . ? C1 O3 1.293(5) . ? O1 C2 1.305(5) . ? O1 Ru1 2.017(3) 5_666 ? C2 O6 1.254(5) 2 ? C2 O2 1.301(5) . ? O3 Ru1 2.033(3) 5_666 ? O3 K1 3.018(3) 5_666 ? O6 C2 1.254(5) 2 ? O7 K1 3.071(3) 8_656 ? O7 H1 0.84(2) . ? O7 H2 0.84(2) . ? O9 Li1 1.935(7) 3_645 ? O10 K1 2.990(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 O4 91.14(13) 5_666 . ? O1 Ru1 O2 179.38(12) 5_666 . ? O4 Ru1 O2 88.60(12) . . ? O1 Ru1 O3 89.26(12) 5_666 5_666 ? O4 Ru1 O3 179.08(12) . 5_666 ? O2 Ru1 O3 90.99(12) . 5_666 ? O1 Ru1 Ru1 89.06(8) 5_666 5_666 ? O4 Ru1 Ru1 88.81(8) . 5_666 ? O2 Ru1 Ru1 90.37(8) . 5_666 ? O3 Ru1 Ru1 90.37(9) 5_666 5_666 ? O1 Ru1 Br1 89.76(8) 5_666 . ? O4 Ru1 Br1 88.88(8) . . ? O2 Ru1 Br1 90.80(8) . . ? O3 Ru1 Br1 91.95(8) 5_666 . ? Ru1 Ru1 Br1 177.38(2) 5_666 . ? O1 Ru1 K1 128.80(9) 5_666 . ? O4 Ru1 K1 126.07(9) . . ? O2 Ru1 K1 51.76(9) . . ? O3 Ru1 K1 54.13(9) 5_666 . ? Ru1 Ru1 K1 121.23(3) 5_666 . ? Br1 Ru1 K1 61.24(2) . . ? O7 Cu1 O7 180.00(15) 5_566 . ? O7 Cu1 O5 86.02(12) 5_566 5_566 ? O7 Cu1 O5 93.98(12) . 5_566 ? O7 Cu1 O5 93.98(12) 5_566 . ? O7 Cu1 O5 86.02(12) . . ? O5 Cu1 O5 180.000(1) 5_566 . ? O7 Cu1 O6 89.53(12) 5_566 . ? O7 Cu1 O6 90.47(12) . . ? O5 Cu1 O6 87.93(13) 5_566 . ? O5 Cu1 O6 92.07(13) . . ? O7 Cu1 O6 90.47(12) 5_566 5_566 ? O7 Cu1 O6 89.53(12) . 5_566 ? O5 Cu1 O6 92.07(13) 5_566 5_566 ? O5 Cu1 O6 87.93(13) . 5_566 ? O6 Cu1 O6 180.00(13) . 5_566 ? Ru1 Br1 K1 124.48(3) . 4_465 ? Ru1 Br1 K1 74.38(2) . . ? K1 Br1 K1 122.290(19) 4_465 . ? Ru1 Br1 K1 126.50(3) . 3_655 ? K1 Br1 K1 88.43(3) 4_465 3_655 ? K1 Br1 K1 125.914(19) . 3_655 ? O8 K1 O9 112.36(10) . . ? O8 K1 O2 131.88(9) . . ? O9 K1 O2 82.33(9) . . ? O8 K1 O10 124.69(8) . . ? O9 K1 O10 120.76(8) . . ? O2 K1 O10 72.05(11) . . ? O8 K1 O3 82.60(9) . 5_666 ? O9 K1 O3 133.19(10) . 5_666 ? O2 K1 O3 58.15(8) . 5_666 ? O10 K1 O3 72.69(11) . 5_666 ? O8 K1 O7 64.91(9) . 8_655 ? O9 K1 O7 61.52(9) . 8_655 ? O2 K1 O7 143.41(9) . 8_655 ? O10 K1 O7 130.17(12) . 8_655 ? O3 K1 O7 147.02(9) 5_666 8_655 ? O8 K1 Br1 66.20(7) . 4_565 ? O9 K1 Br1 128.66(8) . 4_565 ? O2 K1 Br1 139.47(7) . 4_565 ? O10 K1 Br1 69.38(8) . 4_565 ? O3 K1 Br1 98.13(6) 5_666 4_565 ? O7 K1 Br1 74.61(6) 8_655 4_565 ? O8 K1 Br1 74.36(7) . . ? O9 K1 Br1 76.85(7) . . ? O2 K1 Br1 64.59(6) . . ? O10 K1 Br1 130.32(11) . . ? O3 K1 Br1 64.59(6) 5_666 . ? O7 K1 Br1 99.44(7) 8_655 . ? Br1 K1 Br1 138.83(4) 4_565 . ? O8 K1 Br1 130.76(8) . 3_645 ? O9 K1 Br1 63.04(7) . 3_645 ? O2 K1 Br1 97.11(6) . 3_645 ? O10 K1 Br1 68.33(8) . 3_645 ? O3 K1 Br1 138.97(7) 5_666 3_645 ? O7 K1 Br1 72.49(6) 8_655 3_645 ? Br1 K1 Br1 79.98(3) 4_565 3_645 ? Br1 K1 Br1 138.14(4) . 3_645 ? O8 K1 Ru1 99.39(7) . . ? O9 K1 Ru1 100.25(7) . . ? O2 K1 Ru1 32.81(6) . . ? O10 K1 Ru1 85.94(11) . . ? O3 K1 Ru1 33.08(6) 5_666 . ? O7 K1 Ru1 143.76(7) 8_655 . ? Br1 K1 Ru1 131.08(4) 4_565 . ? Br1 K1 Ru1 44.377(17) . . ? Br1 K1 Ru1 129.82(4) 3_645 . ? O8 K1 Li1 23.33(17) . . ? O9 K1 Li1 128.54(12) . . ? O2 K1 Li1 112.43(15) . . ? O10 K1 Li1 110.62(11) . . ? O3 K1 Li1 59.35(17) 5_666 . ? O7 K1 Li1 88.23(17) 8_655 . ? Br1 K1 Li1 71.26(6) 4_565 . ? Br1 K1 Li1 67.83(5) . . ? Br1 K1 Li1 148.84(11) 3_645 . ? Ru1 K1 Li1 79.78(14) . . ? O8 K1 Li1 128.74(12) . 3_645 ? O9 K1 Li1 23.25(17) . 3_645 ? O2 K1 Li1 59.26(17) . 3_645 ? O10 K1 Li1 106.53(10) . 3_645 ? O3 K1 Li1 113.69(15) 5_666 3_645 ? O7 K1 Li1 84.77(17) 8_655 3_645 ? Br1 K1 Li1 145.45(11) 4_565 3_645 ? Br1 K1 Li1 71.05(4) . 3_645 ? Br1 K1 Li1 67.36(6) 3_645 3_645 ? Ru1 K1 Li1 80.98(14) . 3_645 ? Li1 K1 Li1 136.43(3) . 3_645 ? O9 Li1 O9 111.9(6) 4_565 3_655 ? O9 Li1 O8 106.75(15) 4_565 . ? O9 Li1 O8 109.85(14) 3_655 . ? O9 Li1 O8 109.85(14) 4_565 2_665 ? O9 Li1 O8 106.75(15) 3_655 2_665 ? O8 Li1 O8 111.8(6) . 2_665 ? O9 Li1 K1 91.71(15) 4_565 2_665 ? O9 Li1 K1 85.60(14) 3_655 2_665 ? O8 Li1 K1 148.3(5) . 2_665 ? O8 Li1 K1 36.52(17) 2_665 2_665 ? O9 Li1 K1 85.60(14) 4_565 . ? O9 Li1 K1 91.71(15) 3_655 . ? O8 Li1 K1 36.52(17) . . ? O8 Li1 K1 148.3(5) 2_665 . ? K1 Li1 K1 175.2(3) 2_665 . ? O9 Li1 K1 148.4(5) 4_565 3_655 ? O9 Li1 K1 36.61(17) 3_655 3_655 ? O8 Li1 K1 88.65(14) . 3_655 ? O8 Li1 K1 88.54(14) 2_665 3_655 ? K1 Li1 K1 88.505(13) 2_665 3_655 ? K1 Li1 K1 91.705(13) . 3_655 ? O9 Li1 K1 36.61(17) 4_565 4_565 ? O9 Li1 K1 148.4(5) 3_655 4_565 ? O8 Li1 K1 88.54(14) . 4_565 ? O8 Li1 K1 88.65(14) 2_665 4_565 ? K1 Li1 K1 91.705(13) 2_665 4_565 ? K1 Li1 K1 88.505(13) . 4_565 ? K1 Li1 K1 175.0(3) 3_655 4_565 ? O5 C1 O4 120.3(4) . . ? O5 C1 O3 119.9(4) . . ? O4 C1 O3 119.7(4) . . ? C2 O1 Ru1 121.5(3) . 5_666 ? O6 C2 O2 120.8(4) 2 . ? O6 C2 O1 120.0(4) 2 . ? O2 C2 O1 119.2(4) . . ? C2 O2 Ru1 119.8(3) . . ? C2 O2 K1 122.5(3) . . ? Ru1 O2 K1 95.43(11) . . ? C1 O3 Ru1 119.4(3) . 5_666 ? C1 O3 K1 124.3(3) . 5_666 ? Ru1 O3 K1 92.79(11) 5_666 5_666 ? C1 O4 Ru1 121.5(3) . . ? C1 O5 Cu1 130.3(3) . . ? C2 O6 Cu1 128.0(3) 2 . ? Cu1 O7 K1 137.97(14) . 8_656 ? Cu1 O7 H1 97(4) . . ? K1 O7 H1 112(4) 8_656 . ? Cu1 O7 H2 104(5) . . ? K1 O7 H2 97(4) 8_656 . ? H1 O7 H2 105(6) . . ? Li1 O8 K1 120.1(3) . . ? Li1 O9 K1 120.1(3) 3_645 . ? K1 O10 K1 105.1(2) 2_655 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.587 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 942179'