# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_yhw2011081203_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B4 K Li3 O8' _chemical_formula_weight 231.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 9.2106(12) _cell_length_b 9.2106(12) _cell_length_c 19.705(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1447.7(4) _cell_formula_units_Z 9 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3018 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.66 _reflns_number_total 757 _reflns_number_gt 694 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0320P)^2^+1.5642P] 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 SHELXL _refine_ls_extinction_coef 0.0055(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 757 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 K1 K 1.0000 1.0000 0.0000 0.0168(2) Uani 1 6 d S . . K2 K 0.3333 0.6667 -0.00594(3) 0.02063(19) Uani 1 3 d S . . Li1 Li 0.3333 0.6667 0.1667 0.0177(12) Uani 1 6 d S . . Li2 Li 0.3333 0.6667 -0.1643(2) 0.0184(9) Uani 1 3 d S . . Li3 Li 0.7369(3) 1.0501(3) -0.05078(12) 0.0164(5) Uani 1 1 d . . . B1 B 0.50350(17) 0.49195(17) -0.16576(7) 0.0088(3) Uani 1 1 d . . . B2 B 0.66233(19) 0.73645(18) -0.08717(8) 0.0097(3) Uani 1 1 d . . . O1 O 0.51407(12) 0.61535(12) -0.11637(5) 0.0121(3) Uani 1 1 d . . . O2 O 1.18586(12) 1.23578(12) 0.11482(5) 0.0110(2) Uani 1 1 d . . . O3 O 0.33126(11) 0.88111(12) 0.13201(5) 0.0094(2) Uani 1 1 d . . . O4 O 0.66133(12) 0.82344(12) -0.03350(5) 0.0111(2) Uani 1 1 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 K1 0.0122(3) 0.0122(3) 0.0259(4) 0.000 0.000 0.00611(13) K2 0.0159(2) 0.0159(2) 0.0301(3) 0.000 0.000 0.00795(11) Li1 0.0166(18) 0.0166(18) 0.020(3) 0.000 0.000 0.0083(9) Li2 0.0161(13) 0.0161(13) 0.023(2) 0.000 0.000 0.0081(7) Li3 0.0226(13) 0.0158(12) 0.0120(11) -0.0001(9) -0.0016(10) 0.0105(11) B1 0.0078(7) 0.0078(7) 0.0104(6) -0.0003(5) 0.0001(5) 0.0036(5) B2 0.0112(7) 0.0083(7) 0.0107(7) 0.0021(5) 0.0001(5) 0.0058(6) O1 0.0091(5) 0.0115(5) 0.0152(5) -0.0044(4) 0.0000(4) 0.0047(4) O2 0.0089(5) 0.0107(5) 0.0132(5) -0.0030(3) -0.0007(3) 0.0048(4) O3 0.0075(5) 0.0107(5) 0.0094(5) -0.0006(3) 0.0003(3) 0.0040(4) O4 0.0131(5) 0.0109(5) 0.0104(5) -0.0017(3) -0.0010(3) 0.0069(4) _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 K1 O4 2.7817(10) . ? K1 O4 2.7817(10) 10_775 ? K1 O4 2.7817(10) 3_675 ? K1 O4 2.7817(10) 12_655 ? K1 O4 2.7817(10) 11_565 ? K1 O4 2.7817(10) 2_765 ? K1 Li3 2.864(3) 11_565 ? K1 Li3 2.864(3) 2_765 ? K1 Li3 2.864(3) 3_675 ? K1 Li3 2.864(3) 12_655 ? K1 Li3 2.864(3) 10_775 ? K1 O2 3.0080(11) 10_775 ? K2 O4 2.6729(10) 2_665 ? K2 O4 2.6729(10) 3_565 ? K2 O4 2.6729(10) . ? K2 O1 2.9183(11) 3_565 ? K2 O1 2.9183(11) 2_665 ? K2 O1 2.9183(11) . ? K2 Li3 3.188(3) 10_675 ? K2 Li3 3.188(3) 11_455 ? K2 Li3 3.188(3) 12_655 ? K2 B2 3.1953(16) 2_665 ? K2 B2 3.1953(16) 3_565 ? K2 O3 3.3659(12) . ? Li1 O3 2.0990(10) 13_565 ? Li1 O3 2.0990(10) . ? Li1 O3 2.0990(10) 2_665 ? Li1 O3 2.0990(10) 3_565 ? Li1 O3 2.0990(10) 14_455 ? Li1 O3 2.0990(10) 15 ? Li1 B1 2.5668(15) 5 ? Li1 B1 2.5668(15) 6_565 ? Li1 B1 2.5668(15) 11_565 ? Li1 B1 2.5668(15) 12 ? Li1 B1 2.5668(15) 10_665 ? Li1 B1 2.5669(15) 4_455 ? Li2 O1 2.162(2) 2_665 ? Li2 O1 2.162(2) 3_565 ? Li2 O1 2.162(2) . ? Li2 O2 2.251(2) 8_654 ? Li2 O2 2.251(2) 7_444 ? Li2 O2 2.251(2) 9_564 ? Li2 B1 2.7513(15) 3_565 ? Li2 B1 2.7513(15) 2_665 ? Li2 K1 3.330(5) 7_444 ? Li3 O4 1.872(3) . ? Li3 O4 1.907(3) 11_565 ? Li3 O3 1.938(3) 10_675 ? Li3 O2 2.135(3) 12_655 ? Li3 B1 2.523(3) 16_664 ? Li3 B2 2.728(3) 11_565 ? Li3 K2 3.188(3) 10_675 ? Li3 Li3 3.348(3) 11_565 ? Li3 Li3 3.348(3) 12_655 ? B1 O1 1.4622(16) . ? B1 O3 1.4652(16) 12_655 ? B1 O3 1.4812(16) 7_544 ? B1 O2 1.4846(17) 9_564 ? B1 Li3 2.523(3) 16_664 ? B1 Li1 2.5669(15) 7_544 ? B2 O4 1.3297(18) . ? B2 O1 1.3845(17) . ? B2 O2 1.3999(17) 10_775 ? B2 Li3 2.728(3) 12_655 ? O2 B2 1.3999(17) 10_775 ? O2 B1 1.4847(17) 5_665 ? O2 Li3 2.135(3) 11_565 ? O2 Li2 2.251(2) 4 ? O3 B1 1.4652(17) 11_565 ? O3 B1 1.4812(16) 4_455 ? O3 Li3 1.938(3) 10_675 ? O4 Li3 1.907(3) 12_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 O4 K1 O4 180.00(4) . 10_775 ? O4 K1 O4 114.554(15) . 3_675 ? O4 K1 O4 65.446(15) 10_775 3_675 ? O4 K1 O4 65.446(15) . 12_655 ? O4 K1 O4 114.554(15) 10_775 12_655 ? O4 K1 O4 180.0 3_675 12_655 ? O4 K1 O4 65.446(15) . 11_565 ? O4 K1 O4 114.554(15) 10_775 11_565 ? O4 K1 O4 65.446(15) 3_675 11_565 ? O4 K1 O4 114.554(15) 12_655 11_565 ? O4 K1 O4 114.554(14) . 2_765 ? O4 K1 O4 65.446(15) 10_775 2_765 ? O4 K1 O4 114.554(15) 3_675 2_765 ? O4 K1 O4 65.446(15) 12_655 2_765 ? O4 K1 O4 180.0 11_565 2_765 ? O4 K1 Li3 103.91(6) . 11_565 ? O4 K1 Li3 76.09(6) 10_775 11_565 ? O4 K1 Li3 39.44(5) 3_675 11_565 ? O4 K1 Li3 140.56(5) 12_655 11_565 ? O4 K1 Li3 38.69(6) 11_565 11_565 ? O4 K1 Li3 141.31(6) 2_765 11_565 ? O4 K1 Li3 76.09(6) . 2_765 ? O4 K1 Li3 103.91(6) 10_775 2_765 ? O4 K1 Li3 140.56(5) 3_675 2_765 ? O4 K1 Li3 39.44(5) 12_655 2_765 ? O4 K1 Li3 141.31(6) 11_565 2_765 ? O4 K1 Li3 38.69(6) 2_765 2_765 ? Li3 K1 Li3 180.00(9) 11_565 2_765 ? O4 K1 Li3 140.56(5) . 3_675 ? O4 K1 Li3 39.44(5) 10_775 3_675 ? O4 K1 Li3 38.69(6) 3_675 3_675 ? O4 K1 Li3 141.31(6) 12_655 3_675 ? O4 K1 Li3 103.91(6) 11_565 3_675 ? O4 K1 Li3 76.09(6) 2_765 3_675 ? Li3 K1 Li3 71.52(5) 11_565 3_675 ? Li3 K1 Li3 108.48(5) 2_765 3_675 ? O4 K1 Li3 39.44(5) . 12_655 ? O4 K1 Li3 140.56(5) 10_775 12_655 ? O4 K1 Li3 141.31(6) 3_675 12_655 ? O4 K1 Li3 38.69(6) 12_655 12_655 ? O4 K1 Li3 76.09(6) 11_565 12_655 ? O4 K1 Li3 103.91(6) 2_765 12_655 ? Li3 K1 Li3 108.48(5) 11_565 12_655 ? Li3 K1 Li3 71.52(5) 2_765 12_655 ? Li3 K1 Li3 180.0 3_675 12_655 ? O4 K1 Li3 141.31(6) . 10_775 ? O4 K1 Li3 38.69(6) 10_775 10_775 ? O4 K1 Li3 103.91(6) 3_675 10_775 ? O4 K1 Li3 76.09(6) 12_655 10_775 ? O4 K1 Li3 140.56(5) 11_565 10_775 ? O4 K1 Li3 39.44(5) 2_765 10_775 ? Li3 K1 Li3 108.48(5) 11_565 10_775 ? Li3 K1 Li3 71.52(5) 2_765 10_775 ? Li3 K1 Li3 71.52(5) 3_675 10_775 ? Li3 K1 Li3 108.48(5) 12_655 10_775 ? O4 K1 O2 48.12(3) . 10_775 ? O4 K1 O2 131.88(3) 10_775 10_775 ? O4 K1 O2 115.07(3) 3_675 10_775 ? O4 K1 O2 64.93(3) 12_655 10_775 ? O4 K1 O2 106.95(3) 11_565 10_775 ? O4 K1 O2 73.05(3) 2_765 10_775 ? Li3 K1 O2 137.46(5) 11_565 10_775 ? Li3 K1 O2 42.54(5) 2_765 10_775 ? Li3 K1 O2 108.47(5) 3_675 10_775 ? Li3 K1 O2 71.53(5) 12_655 10_775 ? Li3 K1 O2 111.62(5) 10_775 10_775 ? O4 K2 O4 115.982(15) 2_665 3_565 ? O4 K2 O4 115.982(15) 2_665 . ? O4 K2 O4 115.982(15) 3_565 . ? O4 K2 O1 74.18(3) 2_665 3_565 ? O4 K2 O1 49.75(3) 3_565 3_565 ? O4 K2 O1 117.66(4) . 3_565 ? O4 K2 O1 49.75(3) 2_665 2_665 ? O4 K2 O1 117.66(4) 3_565 2_665 ? O4 K2 O1 74.18(3) . 2_665 ? O1 K2 O1 70.49(4) 3_565 2_665 ? O4 K2 O1 117.66(4) 2_665 . ? O4 K2 O1 74.18(3) 3_565 . ? O4 K2 O1 49.75(3) . . ? O1 K2 O1 70.49(4) 3_565 . ? O1 K2 O1 70.49(4) 2_665 . ? O4 K2 Li3 36.66(5) 2_665 10_675 ? O4 K2 Li3 138.57(5) 3_565 10_675 ? O4 K2 Li3 105.43(5) . 10_675 ? O1 K2 Li3 109.75(5) 3_565 10_675 ? O1 K2 Li3 71.75(5) 2_665 10_675 ? O1 K2 Li3 139.43(5) . 10_675 ? O4 K2 Li3 105.43(5) 2_665 11_455 ? O4 K2 Li3 36.66(5) 3_565 11_455 ? O4 K2 Li3 138.57(5) . 11_455 ? O1 K2 Li3 71.75(5) 3_565 11_455 ? O1 K2 Li3 139.43(5) 2_665 11_455 ? O1 K2 Li3 109.75(5) . 11_455 ? Li3 K2 Li3 108.40(5) 10_675 11_455 ? O4 K2 Li3 138.57(5) 2_665 12_655 ? O4 K2 Li3 105.43(5) 3_565 12_655 ? O4 K2 Li3 36.66(5) . 12_655 ? O1 K2 Li3 139.43(5) 3_565 12_655 ? O1 K2 Li3 109.75(5) 2_665 12_655 ? O1 K2 Li3 71.75(5) . 12_655 ? Li3 K2 Li3 108.40(5) 10_675 12_655 ? Li3 K2 Li3 108.40(5) 11_455 12_655 ? O4 K2 B2 24.15(3) 2_665 2_665 ? O4 K2 B2 121.15(4) 3_565 2_665 ? O4 K2 B2 95.15(3) . 2_665 ? O1 K2 B2 71.89(3) 3_565 2_665 ? O1 K2 B2 25.67(3) 2_665 2_665 ? O1 K2 B2 95.26(4) . 2_665 ? Li3 K2 B2 50.59(5) 10_675 2_665 ? Li3 K2 B2 124.83(5) 11_455 2_665 ? Li3 K2 B2 126.20(5) 12_655 2_665 ? O4 K2 B2 95.15(3) 2_665 3_565 ? O4 K2 B2 24.15(3) 3_565 3_565 ? O4 K2 B2 121.15(4) . 3_565 ? O1 K2 B2 25.66(3) 3_565 3_565 ? O1 K2 B2 95.26(4) 2_665 3_565 ? O1 K2 B2 71.89(3) . 3_565 ? Li3 K2 B2 126.20(5) 10_675 3_565 ? Li3 K2 B2 50.59(5) 11_455 3_565 ? Li3 K2 B2 124.83(5) 12_655 3_565 ? B2 K2 B2 97.10(4) 2_665 3_565 ? O4 K2 O3 69.79(3) 2_665 . ? O4 K2 O3 130.85(3) 3_565 . ? O4 K2 O3 100.58(3) . . ? O1 K2 O3 136.01(3) 3_565 . ? O1 K2 O3 102.64(3) 2_665 . ? O1 K2 O3 150.26(2) . . ? Li3 K2 O3 34.26(5) 10_675 . ? Li3 K2 O3 94.26(5) 11_455 . ? Li3 K2 O3 84.41(5) 12_655 . ? B2 K2 O3 84.48(3) 2_665 . ? B2 K2 O3 137.76(3) 3_565 . ? O3 Li1 O3 180.0 13_565 . ? O3 Li1 O3 70.05(2) 13_565 2_665 ? O3 Li1 O3 109.95(2) . 2_665 ? O3 Li1 O3 70.05(2) 13_565 3_565 ? O3 Li1 O3 109.95(2) . 3_565 ? O3 Li1 O3 109.95(2) 2_665 3_565 ? O3 Li1 O3 109.95(2) 13_565 14_455 ? O3 Li1 O3 70.05(2) . 14_455 ? O3 Li1 O3 180.0 2_665 14_455 ? O3 Li1 O3 70.05(2) 3_565 14_455 ? O3 Li1 O3 109.95(2) 13_565 15 ? O3 Li1 O3 70.05(2) . 15 ? O3 Li1 O3 70.05(2) 2_665 15 ? O3 Li1 O3 180.0 3_565 15 ? O3 Li1 O3 109.95(2) 14_455 15 ? O3 Li1 B1 34.81(4) 13_565 5 ? O3 Li1 B1 145.19(4) . 5 ? O3 Li1 B1 35.24(4) 2_665 5 ? O3 Li1 B1 90.14(4) 3_565 5 ? O3 Li1 B1 144.76(4) 14_455 5 ? O3 Li1 B1 89.86(4) 15 5 ? O3 Li1 B1 89.86(4) 13_565 6_565 ? O3 Li1 B1 90.14(4) . 6_565 ? O3 Li1 B1 145.19(4) 2_665 6_565 ? O3 Li1 B1 35.24(4) 3_565 6_565 ? O3 Li1 B1 34.81(4) 14_455 6_565 ? O3 Li1 B1 144.76(4) 15 6_565 ? B1 Li1 B1 119.997(1) 5 6_565 ? O3 Li1 B1 145.19(4) 13_565 11_565 ? O3 Li1 B1 34.81(4) . 11_565 ? O3 Li1 B1 144.76(4) 2_665 11_565 ? O3 Li1 B1 89.86(4) 3_565 11_565 ? O3 Li1 B1 35.24(4) 14_455 11_565 ? O3 Li1 B1 90.14(4) 15 11_565 ? B1 Li1 B1 180.0 5 11_565 ? B1 Li1 B1 60.004(1) 6_565 11_565 ? O3 Li1 B1 90.14(4) 13_565 12 ? O3 Li1 B1 89.86(4) . 12 ? O3 Li1 B1 34.81(4) 2_665 12 ? O3 Li1 B1 144.76(4) 3_565 12 ? O3 Li1 B1 145.19(4) 14_455 12 ? O3 Li1 B1 35.24(4) 15 12 ? B1 Li1 B1 60.004(1) 5 12 ? B1 Li1 B1 180.0 6_565 12 ? B1 Li1 B1 119.995(1) 11_565 12 ? O3 Li1 B1 35.24(4) 13_565 10_665 ? O3 Li1 B1 144.76(4) . 10_665 ? O3 Li1 B1 89.86(4) 2_665 10_665 ? O3 Li1 B1 34.81(4) 3_565 10_665 ? O3 Li1 B1 90.14(4) 14_455 10_665 ? O3 Li1 B1 145.19(4) 15 10_665 ? B1 Li1 B1 60.006(1) 5 10_665 ? B1 Li1 B1 60.006(1) 6_565 10_665 ? B1 Li1 B1 119.995(1) 11_565 10_665 ? B1 Li1 B1 119.995(1) 12 10_665 ? O3 Li1 B1 144.76(4) 13_565 4_455 ? O3 Li1 B1 35.24(4) . 4_455 ? O3 Li1 B1 90.14(4) 2_665 4_455 ? O3 Li1 B1 145.19(4) 3_565 4_455 ? O3 Li1 B1 89.86(4) 14_455 4_455 ? O3 Li1 B1 34.81(4) 15 4_455 ? B1 Li1 B1 119.994(1) 5 4_455 ? B1 Li1 B1 119.994(1) 6_565 4_455 ? B1 Li1 B1 60.005(1) 11_565 4_455 ? B1 Li1 B1 60.005(1) 12 4_455 ? B1 Li1 B1 180.0 10_665 4_455 ? O1 Li2 O1 102.32(13) 2_665 3_565 ? O1 Li2 O1 102.32(13) 2_665 . ? O1 Li2 O1 102.32(13) 3_565 . ? O1 Li2 O2 96.95(4) 2_665 8_654 ? O1 Li2 O2 64.46(4) 3_565 8_654 ? O1 Li2 O2 158.77(4) . 8_654 ? O1 Li2 O2 64.46(4) 2_665 7_444 ? O1 Li2 O2 158.77(4) 3_565 7_444 ? O1 Li2 O2 96.95(4) . 7_444 ? O2 Li2 O2 99.36(13) 8_654 7_444 ? O1 Li2 O2 158.77(4) 2_665 9_564 ? O1 Li2 O2 96.95(4) 3_565 9_564 ? O1 Li2 O2 64.46(4) . 9_564 ? O2 Li2 O2 99.36(13) 8_654 9_564 ? O2 Li2 O2 99.36(13) 7_444 9_564 ? O1 Li2 B1 100.78(6) 2_665 3_565 ? O1 Li2 B1 31.85(4) 3_565 3_565 ? O1 Li2 B1 132.52(11) . 3_565 ? O2 Li2 B1 32.62(4) 8_654 3_565 ? O2 Li2 B1 130.48(11) 7_444 3_565 ? O2 Li2 B1 100.29(7) 9_564 3_565 ? O1 Li2 B1 31.85(4) 2_665 2_665 ? O1 Li2 B1 132.52(11) 3_565 2_665 ? O1 Li2 B1 100.78(6) . 2_665 ? O2 Li2 B1 100.29(7) 8_654 2_665 ? O2 Li2 B1 32.62(4) 7_444 2_665 ? O2 Li2 B1 130.48(11) 9_564 2_665 ? B1 Li2 B1 119.990(4) 3_565 2_665 ? O1 Li2 K1 115.92(11) 2_665 7_444 ? O1 Li2 K1 115.92(11) 3_565 7_444 ? O1 Li2 K1 115.92(11) . 7_444 ? O2 Li2 K1 61.69(10) 8_654 7_444 ? O2 Li2 K1 61.69(10) 7_444 7_444 ? O2 Li2 K1 61.69(10) 9_564 7_444 ? B1 Li2 K1 89.41(10) 3_565 7_444 ? B1 Li2 K1 89.41(10) 2_665 7_444 ? O4 Li3 O4 105.47(12) . 11_565 ? O4 Li3 O3 120.95(13) . 10_675 ? O4 Li3 O3 131.18(14) 11_565 10_675 ? O4 Li3 O2 118.76(13) . 12_655 ? O4 Li3 O2 100.64(12) 11_565 12_655 ? O3 Li3 O2 70.95(9) 10_675 12_655 ? O4 Li3 B1 121.72(12) . 16_664 ? O4 Li3 B1 126.39(13) 11_565 16_664 ? O3 Li3 B1 35.84(6) 10_675 16_664 ? O2 Li3 B1 35.97(6) 12_655 16_664 ? O4 Li3 B2 83.94(9) . 11_565 ? O4 Li3 B2 26.52(6) 11_565 11_565 ? O3 Li3 B2 141.51(13) 10_675 11_565 ? O2 Li3 B2 125.44(12) 12_655 11_565 ? B1 Li3 B2 152.39(12) 16_664 11_565 ? O4 Li3 K2 137.25(12) . 10_675 ? O4 Li3 K2 56.82(7) 11_565 10_675 ? O3 Li3 K2 77.91(8) 10_675 10_675 ? O2 Li3 K2 103.38(9) 12_655 10_675 ? B1 Li3 K2 96.25(8) 16_664 10_675 ? B2 Li3 K2 64.85(6) 11_565 10_675 ? O4 Li3 Li3 113.81(10) . 11_565 ? O4 Li3 Li3 27.36(8) 11_565 11_565 ? O3 Li3 Li3 124.04(12) 10_675 11_565 ? O2 Li3 Li3 73.86(6) 12_655 11_565 ? B1 Li3 Li3 104.03(9) 16_664 11_565 ? B2 Li3 Li3 51.77(9) 11_565 11_565 ? K2 Li3 Li3 69.63(8) 10_675 11_565 ? O4 Li3 Li3 27.91(5) . 12_655 ? O4 Li3 Li3 77.64(11) 11_565 12_655 ? O3 Li3 Li3 147.99(12) 10_675 12_655 ? O2 Li3 Li3 123.25(7) 12_655 12_655 ? B1 Li3 Li3 143.77(10) 16_664 12_655 ? B2 Li3 Li3 57.93(9) 11_565 12_655 ? K2 Li3 Li3 119.91(11) 10_675 12_655 ? Li3 Li3 Li3 87.94(10) 11_565 12_655 ? O1 B1 O3 109.96(10) . 12_655 ? O1 B1 O3 112.29(10) . 7_544 ? O3 B1 O3 109.71(12) 12_655 7_544 ? O1 B1 O2 106.09(10) . 9_564 ? O3 B1 O2 112.71(10) 12_655 9_564 ? O3 B1 O2 106.02(10) 7_544 9_564 ? O1 B1 Li3 112.21(10) . 16_664 ? O3 B1 Li3 137.72(10) 12_655 16_664 ? O3 B1 Li3 50.01(8) 7_544 16_664 ? O2 B1 Li3 57.62(8) 9_564 16_664 ? O1 B1 Li1 128.08(9) . 7_544 ? O3 B1 Li1 54.86(6) 12_655 7_544 ? O3 B1 Li1 54.86(6) 7_544 7_544 ? O2 B1 Li1 125.78(8) 9_564 7_544 ? Li3 B1 Li1 95.20(7) 16_664 7_544 ? O4 B2 O1 120.98(12) . . ? O4 B2 O2 120.44(12) . 10_775 ? O1 B2 O2 118.57(12) . 10_775 ? O4 B2 Li3 39.81(8) . 12_655 ? O1 B2 Li3 117.57(11) . 12_655 ? O2 B2 Li3 108.26(10) 10_775 12_655 ? B2 O1 B1 123.94(11) . . ? B2 O1 Li2 124.24(9) . . ? B1 O1 Li2 96.87(11) . . ? B2 O1 K2 88.42(8) . . ? B1 O1 K2 143.19(8) . . ? Li2 O1 K2 74.14(11) . . ? B2 O2 B1 123.34(11) 10_775 5_665 ? B2 O2 Li3 114.04(10) 10_775 11_565 ? B1 O2 Li3 86.42(10) 5_665 11_565 ? B2 O2 Li2 124.69(8) 10_775 4 ? B1 O2 Li2 92.54(11) 5_665 4 ? Li3 O2 Li2 108.21(10) 11_565 4 ? B2 O2 K1 89.72(8) 10_775 . ? B1 O2 K1 143.93(8) 5_665 . ? Li3 O2 K1 65.13(7) 11_565 . ? Li2 O2 K1 77.09(11) 4 . ? B1 O3 B1 121.20(6) 11_565 4_455 ? B1 O3 Li3 122.50(11) 11_565 10_675 ? B1 O3 Li3 94.14(11) 4_455 10_675 ? B1 O3 Li1 90.34(7) 11_565 . ? B1 O3 Li1 89.90(7) 4_455 . ? Li3 O3 Li1 137.16(9) 10_675 . ? B1 O3 K2 117.53(7) 11_565 . ? B1 O3 K2 118.49(7) 4_455 . ? Li3 O3 K2 67.83(8) 10_675 . ? Li1 O3 K2 72.85(3) . . ? B2 O4 Li3 114.61(11) . . ? B2 O4 Li3 113.67(12) . 12_655 ? Li3 O4 Li3 124.73(12) . 12_655 ? B2 O4 K2 100.52(8) . . ? Li3 O4 K2 109.21(9) . . ? Li3 O4 K2 86.52(8) 12_655 . ? B2 O4 K1 101.38(8) . . ? Li3 O4 K1 73.04(9) . . ? Li3 O4 K1 72.62(8) 12_655 . ? K2 O4 K1 154.39(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 969702' ####################################################################### # # 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_yhw2013050901_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B12 Cl F6 Li Na2 O24 Sr8' _chemical_formula_weight 1417.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 9.677(4) _cell_length_b 9.677(4) _cell_length_c 24.30(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1971(2) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 16.393 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4031 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.56 _reflns_number_total 1019 _reflns_number_gt 813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0242P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00062(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1019 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Sr1 Sr 0.69677(5) 0.74279(5) 0.125563(18) 0.00989(16) Uani 1 1 d . . . Sr2 Sr 0.6667 0.3333 0.10733(3) 0.0090(2) Uani 1 3 d S . . Na1 Na 0.3333 0.6667 0.03884(17) 0.0238(9) Uani 1 3 d S . . Li1 Li 1.0000 1.0000 0.0000 0.026(6) Uani 1 6 d S . . B1 B 0.3965(6) 0.3774(6) 0.0639(2) 0.0086(11) Uani 1 1 d . . . B2 B 0.6933(6) 0.8525(6) 0.0015(2) 0.0072(11) Uani 1 1 d . . . F1 F 0.9655(3) 0.8069(3) 0.14757(11) 0.0129(6) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.1667 0.0209(7) Uani 1 6 d S . . O1 O 0.7906(4) 0.7926(4) 0.02699(13) 0.0085(7) Uani 1 1 d . . . O2 O 0.6003(4) 0.8716(4) 0.04681(13) 0.0090(7) Uani 1 1 d . . . O3 O 0.4917(4) 0.4629(4) 0.10530(13) 0.0104(7) Uani 1 1 d . . . O4 O 0.8421(4) 0.5761(4) 0.03771(13) 0.0107(7) Uani 1 1 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 Sr1 0.0118(3) 0.0084(3) 0.0084(2) -0.00043(18) -0.00195(18) 0.0043(2) Sr2 0.0083(3) 0.0083(3) 0.0102(4) 0.000 0.000 0.00417(13) Na1 0.0154(12) 0.0154(12) 0.041(3) 0.000 0.000 0.0077(6) Li1 0.014(7) 0.014(7) 0.051(17) 0.000 0.000 0.007(3) B1 0.009(3) 0.005(3) 0.009(3) -0.001(2) 0.002(2) 0.002(2) B2 0.011(3) 0.005(3) 0.006(3) -0.002(2) -0.001(2) 0.004(2) F1 0.0096(14) 0.0134(14) 0.0137(15) -0.0004(12) -0.0004(11) 0.0043(12) Cl1 0.0198(10) 0.0198(10) 0.0230(18) 0.000 0.000 0.0099(5) O1 0.0128(17) 0.0116(17) 0.0054(16) 0.0008(13) -0.0005(14) 0.0094(14) O2 0.0088(16) 0.0069(16) 0.0103(17) 0.0000(13) 0.0024(13) 0.0032(14) O3 0.0107(17) 0.0076(16) 0.0114(18) -0.0029(13) -0.0012(14) 0.0035(14) O4 0.0072(17) 0.0104(17) 0.0128(19) 0.0037(14) -0.0001(14) 0.0032(14) _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 Sr1 F1 2.413(3) . ? Sr1 O3 2.478(3) . ? Sr1 F1 2.502(3) 3_675 ? Sr1 O1 2.521(4) . ? Sr1 F1 2.571(3) 13_665 ? Sr1 O3 2.616(4) 15 ? Sr1 O2 2.692(3) . ? Sr1 Cl1 3.3642(14) . ? Sr1 B1 3.439(5) 2_665 ? Sr1 Sr2 3.6687(18) 13_665 ? Sr1 Sr1 3.7830(16) 14_455 ? Sr1 Sr1 3.7831(16) 15 ? Sr2 O3 2.562(3) 3_665 ? Sr2 O3 2.562(3) 2_655 ? Sr2 O3 2.562(3) . ? Sr2 F1 2.572(3) 15_545 ? Sr2 F1 2.572(3) 14_455 ? Sr2 F1 2.572(3) 13_665 ? Sr2 O4 2.697(3) 3_665 ? Sr2 O4 2.697(3) 2_655 ? Sr2 O4 2.697(3) . ? Sr2 B1 3.041(6) 2_655 ? Sr2 B1 3.041(6) 3_665 ? Sr2 Na1 3.552(5) 10_665 ? Na1 O2 2.350(3) 2_665 ? Na1 O2 2.350(3) . ? Na1 O2 2.350(3) 3_565 ? Na1 O4 2.806(4) 12 ? Na1 O4 2.806(4) 10_665 ? Na1 O4 2.806(4) 11_565 ? Na1 Cl1 3.106(5) . ? Na1 B2 3.150(5) 2_665 ? Na1 B2 3.150(5) 3_565 ? Na1 Sr2 3.552(5) 10_665 ? Na1 Sr1 3.842(3) 2_665 ? Na1 Sr1 3.842(3) 3_565 ? Li1 O1 2.121(3) 12_655 ? Li1 O1 2.121(3) 10_775 ? Li1 O1 2.121(3) 3_675 ? Li1 O1 2.121(3) . ? Li1 O1 2.121(3) 11_565 ? Li1 O1 2.121(3) 2_765 ? Li1 B2 2.571(5) 12_655 ? Li1 B2 2.571(5) 3_675 ? Li1 B2 2.571(5) 10_775 ? Li1 B2 2.571(5) 2_765 ? Li1 B2 2.571(5) 11_565 ? Li1 Sr1 4.100(2) 3_675 ? B1 O3 1.335(6) . ? B1 O4 1.387(6) 2_655 ? B1 O2 1.396(6) 3_565 ? B1 Sr1 3.439(5) 3_565 ? B2 O1 1.452(6) 11_565 ? B2 O1 1.467(6) . ? B2 O4 1.486(6) 11_565 ? B2 O2 1.490(6) . ? F1 Sr1 2.502(3) 2_765 ? F1 Sr1 2.571(3) 13_665 ? F1 Sr2 2.572(3) 13_665 ? Cl1 Na1 3.106(5) 13_565 ? Cl1 Sr1 3.3642(14) 14_455 ? Cl1 Sr1 3.3642(14) 2_665 ? Cl1 Sr1 3.3642(14) 3_565 ? Cl1 Sr1 3.3643(14) 15 ? Cl1 Sr1 3.3643(14) 13_565 ? O1 B2 1.452(6) 12_655 ? O2 B1 1.396(6) 2_665 ? O3 Sr1 2.616(4) 14_455 ? O4 B1 1.387(6) 3_665 ? O4 B2 1.486(6) 12_655 ? O4 Na1 2.806(4) 10_665 ? 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 F1 Sr1 O3 119.75(10) . . ? F1 Sr1 F1 74.92(12) . 3_675 ? O3 Sr1 F1 164.97(10) . 3_675 ? F1 Sr1 O1 85.57(10) . . ? O3 Sr1 O1 92.02(11) . . ? F1 Sr1 O1 92.44(9) 3_675 . ? F1 Sr1 F1 68.20(10) . 13_665 ? O3 Sr1 F1 63.49(10) . 13_665 ? F1 Sr1 F1 124.69(4) 3_675 13_665 ? O1 Sr1 F1 123.05(10) . 13_665 ? F1 Sr1 O3 83.08(9) . 15 ? O3 Sr1 O3 113.48(11) . 15 ? F1 Sr1 O3 62.51(9) 3_675 15 ? O1 Sr1 O3 154.45(10) . 15 ? F1 Sr1 O3 73.19(10) 13_665 15 ? F1 Sr1 O2 128.11(9) . . ? O3 Sr1 O2 95.22(10) . . ? F1 Sr1 O2 75.97(9) 3_675 . ? O1 Sr1 O2 53.92(10) . . ? F1 Sr1 O2 158.71(9) 13_665 . ? O3 Sr1 O2 118.69(10) 15 . ? F1 Sr1 Cl1 149.87(7) . . ? O3 Sr1 Cl1 68.99(7) . . ? F1 Sr1 Cl1 96.73(6) 3_675 . ? O1 Sr1 Cl1 124.12(7) . . ? F1 Sr1 Cl1 95.38(6) 13_665 . ? O3 Sr1 Cl1 67.69(7) 15 . ? O2 Sr1 Cl1 75.29(7) . . ? F1 Sr1 B1 120.93(11) . 2_665 ? O3 Sr1 B1 113.49(12) . 2_665 ? F1 Sr1 B1 55.43(11) 3_675 2_665 ? O1 Sr1 B1 68.44(11) . 2_665 ? F1 Sr1 B1 167.29(11) 13_665 2_665 ? O3 Sr1 B1 98.25(12) 15 2_665 ? O2 Sr1 B1 22.35(11) . 2_665 ? Cl1 Sr1 B1 72.41(9) . 2_665 ? F1 Sr1 Sr2 44.31(6) . 13_665 ? O3 Sr1 Sr2 143.66(8) . 13_665 ? F1 Sr1 Sr2 44.45(6) 3_675 13_665 ? O1 Sr1 Sr2 114.40(8) . 13_665 ? F1 Sr1 Sr2 80.83(7) 13_665 13_665 ? O3 Sr1 Sr2 44.30(7) 15 13_665 ? O2 Sr1 Sr2 120.24(7) . 13_665 ? Cl1 Sr1 Sr2 110.18(4) . 13_665 ? B1 Sr1 Sr2 99.76(10) 2_665 13_665 ? F1 Sr1 Sr1 108.57(7) . 14_455 ? O3 Sr1 Sr1 43.47(8) . 14_455 ? F1 Sr1 Sr1 132.24(7) 3_675 14_455 ? O1 Sr1 Sr1 134.95(7) . 14_455 ? F1 Sr1 Sr1 41.10(6) 13_665 14_455 ? O3 Sr1 Sr1 70.55(8) 15 14_455 ? O2 Sr1 Sr1 122.81(7) . 14_455 ? Cl1 Sr1 Sr1 55.789(8) . 14_455 ? B1 Sr1 Sr1 127.64(9) 2_665 14_455 ? Sr2 Sr1 Sr1 104.25(5) 13_665 14_455 ? F1 Sr1 Sr1 105.96(7) . 15 ? O3 Sr1 Sr1 124.35(7) . 15 ? F1 Sr1 Sr1 42.49(6) 3_675 15 ? O1 Sr1 Sr1 123.02(7) . 15 ? F1 Sr1 Sr1 112.73(8) 13_665 15 ? O3 Sr1 Sr1 40.66(7) 15 15 ? O2 Sr1 Sr1 78.19(8) . 15 ? Cl1 Sr1 Sr1 55.789(8) . 15 ? B1 Sr1 Sr1 57.70(10) 2_665 15 ? Sr2 Sr1 Sr1 62.20(3) 13_665 15 ? Sr1 Sr1 Sr1 94.69(4) 14_455 15 ? O3 Sr2 O3 119.963(5) 3_665 2_655 ? O3 Sr2 O3 119.963(5) 3_665 . ? O3 Sr2 O3 119.963(5) 2_655 . ? O3 Sr2 F1 62.35(9) 3_665 15_545 ? O3 Sr2 F1 81.12(9) 2_655 15_545 ? O3 Sr2 F1 131.39(10) . 15_545 ? O3 Sr2 F1 131.39(10) 3_665 14_455 ? O3 Sr2 F1 62.35(9) 2_655 14_455 ? O3 Sr2 F1 81.12(9) . 14_455 ? F1 Sr2 F1 71.10(10) 15_545 14_455 ? O3 Sr2 F1 81.12(9) 3_665 13_665 ? O3 Sr2 F1 131.39(10) 2_655 13_665 ? O3 Sr2 F1 62.35(9) . 13_665 ? F1 Sr2 F1 71.10(10) 15_545 13_665 ? F1 Sr2 F1 71.10(10) 14_455 13_665 ? O3 Sr2 O4 81.01(10) 3_665 3_665 ? O3 Sr2 O4 52.93(9) 2_655 3_665 ? O3 Sr2 O4 136.28(10) . 3_665 ? F1 Sr2 O4 92.03(10) 15_545 3_665 ? F1 Sr2 O4 114.91(9) 14_455 3_665 ? F1 Sr2 O4 159.70(9) 13_665 3_665 ? O3 Sr2 O4 136.28(10) 3_665 2_655 ? O3 Sr2 O4 81.01(10) 2_655 2_655 ? O3 Sr2 O4 52.93(10) . 2_655 ? F1 Sr2 O4 159.70(9) 15_545 2_655 ? F1 Sr2 O4 92.03(10) 14_455 2_655 ? F1 Sr2 O4 114.91(9) 13_665 2_655 ? O4 Sr2 O4 84.83(11) 3_665 2_655 ? O3 Sr2 O4 52.93(9) 3_665 . ? O3 Sr2 O4 136.28(10) 2_655 . ? O3 Sr2 O4 81.01(10) . . ? F1 Sr2 O4 114.91(9) 15_545 . ? F1 Sr2 O4 159.70(9) 14_455 . ? F1 Sr2 O4 92.03(10) 13_665 . ? O4 Sr2 O4 84.83(11) 3_665 . ? O4 Sr2 O4 84.83(11) 2_655 . ? O3 Sr2 B1 101.19(12) 3_665 2_655 ? O3 Sr2 B1 25.80(12) 2_655 2_655 ? O3 Sr2 B1 133.33(12) . 2_655 ? F1 Sr2 B1 85.51(12) 15_545 2_655 ? F1 Sr2 B1 87.91(12) 14_455 2_655 ? F1 Sr2 B1 152.42(12) 13_665 2_655 ? O4 Sr2 B1 27.14(12) 3_665 2_655 ? O4 Sr2 B1 82.59(12) 2_655 2_655 ? O4 Sr2 B1 111.47(13) . 2_655 ? O3 Sr2 B1 25.80(12) 3_665 3_665 ? O3 Sr2 B1 133.33(12) 2_655 3_665 ? O3 Sr2 B1 101.19(12) . 3_665 ? F1 Sr2 B1 87.91(12) 15_545 3_665 ? F1 Sr2 B1 152.42(12) 14_455 3_665 ? F1 Sr2 B1 85.51(12) 13_665 3_665 ? O4 Sr2 B1 82.59(12) 3_665 3_665 ? O4 Sr2 B1 111.47(13) 2_655 3_665 ? O4 Sr2 B1 27.14(12) . 3_665 ? B1 Sr2 B1 108.63(11) 2_655 3_665 ? O3 Sr2 Na1 88.90(7) 3_665 10_665 ? O3 Sr2 Na1 88.90(7) 2_655 10_665 ? O3 Sr2 Na1 88.90(7) . 10_665 ? F1 Sr2 Na1 137.83(7) 15_545 10_665 ? F1 Sr2 Na1 137.83(7) 14_455 10_665 ? F1 Sr2 Na1 137.83(7) 13_665 10_665 ? O4 Sr2 Na1 51.16(7) 3_665 10_665 ? O4 Sr2 Na1 51.16(7) 2_655 10_665 ? O4 Sr2 Na1 51.16(7) . 10_665 ? B1 Sr2 Na1 69.70(10) 2_655 10_665 ? B1 Sr2 Na1 69.70(10) 3_665 10_665 ? O2 Na1 O2 119.33(4) 2_665 . ? O2 Na1 O2 119.33(4) 2_665 3_565 ? O2 Na1 O2 119.33(4) . 3_565 ? O2 Na1 O4 54.48(11) 2_665 12 ? O2 Na1 O4 91.95(12) . 12 ? O2 Na1 O4 135.31(16) 3_565 12 ? O2 Na1 O4 91.95(12) 2_665 10_665 ? O2 Na1 O4 135.31(16) . 10_665 ? O2 Na1 O4 54.48(11) 3_565 10_665 ? O4 Na1 O4 80.84(14) 12 10_665 ? O2 Na1 O4 135.31(16) 2_665 11_565 ? O2 Na1 O4 54.48(11) . 11_565 ? O2 Na1 O4 91.95(12) 3_565 11_565 ? O4 Na1 O4 80.84(14) 12 11_565 ? O4 Na1 O4 80.84(14) 10_665 11_565 ? O2 Na1 Cl1 85.27(12) 2_665 . ? O2 Na1 Cl1 85.27(12) . . ? O2 Na1 Cl1 85.27(12) 3_565 . ? O4 Na1 Cl1 131.52(9) 12 . ? O4 Na1 Cl1 131.52(9) 10_665 . ? O4 Na1 Cl1 131.52(9) 11_565 . ? O2 Na1 B2 26.71(12) 2_665 2_665 ? O2 Na1 B2 104.67(12) . 2_665 ? O2 Na1 B2 135.33(12) 3_565 2_665 ? O4 Na1 B2 28.14(11) 12 2_665 ? O4 Na1 B2 89.35(14) 10_665 2_665 ? O4 Na1 B2 108.69(16) 11_565 2_665 ? Cl1 Na1 B2 106.74(12) . 2_665 ? O2 Na1 B2 104.67(12) 2_665 3_565 ? O2 Na1 B2 135.33(12) . 3_565 ? O2 Na1 B2 26.71(12) 3_565 3_565 ? O4 Na1 B2 108.69(16) 12 3_565 ? O4 Na1 B2 28.14(11) 10_665 3_565 ? O4 Na1 B2 89.35(14) 11_565 3_565 ? Cl1 Na1 B2 106.74(12) . 3_565 ? B2 Na1 B2 112.06(11) 2_665 3_565 ? O2 Na1 Sr2 94.73(12) 2_665 10_665 ? O2 Na1 Sr2 94.73(12) . 10_665 ? O2 Na1 Sr2 94.73(12) 3_565 10_665 ? O4 Na1 Sr2 48.48(9) 12 10_665 ? O4 Na1 Sr2 48.48(9) 10_665 10_665 ? O4 Na1 Sr2 48.48(9) 11_565 10_665 ? Cl1 Na1 Sr2 180.0 . 10_665 ? B2 Na1 Sr2 73.26(12) 2_665 10_665 ? B2 Na1 Sr2 73.26(12) 3_565 10_665 ? O2 Na1 Sr1 43.79(9) 2_665 2_665 ? O2 Na1 Sr1 82.64(9) . 2_665 ? O2 Na1 Sr1 135.58(15) 3_565 2_665 ? O4 Na1 Sr1 74.88(8) 12 2_665 ? O4 Na1 Sr1 135.63(7) 10_665 2_665 ? O4 Na1 Sr1 129.55(7) 11_565 2_665 ? Cl1 Na1 Sr1 56.74(6) . 2_665 ? B2 Na1 Sr1 53.40(11) 2_665 2_665 ? B2 Na1 Sr1 140.17(11) 3_565 2_665 ? Sr2 Na1 Sr1 123.26(6) 10_665 2_665 ? O2 Na1 Sr1 82.64(9) 2_665 3_565 ? O2 Na1 Sr1 135.58(15) . 3_565 ? O2 Na1 Sr1 43.79(9) 3_565 3_565 ? O4 Na1 Sr1 129.55(7) 12 3_565 ? O4 Na1 Sr1 74.88(8) 10_665 3_565 ? O4 Na1 Sr1 135.63(7) 11_565 3_565 ? Cl1 Na1 Sr1 56.74(6) . 3_565 ? B2 Na1 Sr1 107.59(10) 2_665 3_565 ? B2 Na1 Sr1 53.40(11) 3_565 3_565 ? Sr2 Na1 Sr1 123.26(6) 10_665 3_565 ? Sr1 Na1 Sr1 92.79(8) 2_665 3_565 ? O1 Li1 O1 110.89(8) 12_655 10_775 ? O1 Li1 O1 180.00(17) 12_655 3_675 ? O1 Li1 O1 69.11(8) 10_775 3_675 ? O1 Li1 O1 69.11(8) 12_655 . ? O1 Li1 O1 180.0 10_775 . ? O1 Li1 O1 110.89(8) 3_675 . ? O1 Li1 O1 110.89(8) 12_655 11_565 ? O1 Li1 O1 110.89(8) 10_775 11_565 ? O1 Li1 O1 69.11(8) 3_675 11_565 ? O1 Li1 O1 69.11(8) . 11_565 ? O1 Li1 O1 69.11(8) 12_655 2_765 ? O1 Li1 O1 69.11(8) 10_775 2_765 ? O1 Li1 O1 110.89(8) 3_675 2_765 ? O1 Li1 O1 110.89(8) . 2_765 ? O1 Li1 O1 180.00(16) 11_565 2_765 ? O1 Li1 B2 34.78(13) 12_655 12_655 ? O1 Li1 B2 145.63(13) 10_775 12_655 ? O1 Li1 B2 145.22(13) 3_675 12_655 ? O1 Li1 B2 34.37(13) . 12_655 ? O1 Li1 B2 89.01(13) 11_565 12_655 ? O1 Li1 B2 90.99(13) 2_765 12_655 ? O1 Li1 B2 145.22(13) 12_655 3_675 ? O1 Li1 B2 34.37(13) 10_775 3_675 ? O1 Li1 B2 34.78(13) 3_675 3_675 ? O1 Li1 B2 145.63(13) . 3_675 ? O1 Li1 B2 90.99(13) 11_565 3_675 ? O1 Li1 B2 89.01(13) 2_765 3_675 ? B2 Li1 B2 180.0(2) 12_655 3_675 ? O1 Li1 B2 89.01(13) 12_655 10_775 ? O1 Li1 B2 34.78(13) 10_775 10_775 ? O1 Li1 B2 90.99(13) 3_675 10_775 ? O1 Li1 B2 145.22(13) . 10_775 ? O1 Li1 B2 145.63(13) 11_565 10_775 ? O1 Li1 B2 34.37(13) 2_765 10_775 ? B2 Li1 B2 119.980(6) 12_655 10_775 ? B2 Li1 B2 60.020(6) 3_675 10_775 ? O1 Li1 B2 34.37(13) 12_655 2_765 ? O1 Li1 B2 90.99(13) 10_775 2_765 ? O1 Li1 B2 145.63(13) 3_675 2_765 ? O1 Li1 B2 89.01(13) . 2_765 ? O1 Li1 B2 145.22(13) 11_565 2_765 ? O1 Li1 B2 34.78(13) 2_765 2_765 ? B2 Li1 B2 60.020(6) 12_655 2_765 ? B2 Li1 B2 119.980(7) 3_675 2_765 ? B2 Li1 B2 60.020(6) 10_775 2_765 ? O1 Li1 B2 145.63(13) 12_655 11_565 ? O1 Li1 B2 89.01(13) 10_775 11_565 ? O1 Li1 B2 34.37(13) 3_675 11_565 ? O1 Li1 B2 90.99(13) . 11_565 ? O1 Li1 B2 34.78(13) 11_565 11_565 ? O1 Li1 B2 145.22(13) 2_765 11_565 ? B2 Li1 B2 119.980(6) 12_655 11_565 ? B2 Li1 B2 60.020(6) 3_675 11_565 ? B2 Li1 B2 119.980(6) 10_775 11_565 ? B2 Li1 B2 180.0(2) 2_765 11_565 ? O1 Li1 Sr1 149.29(8) 12_655 3_675 ? O1 Li1 Sr1 80.94(9) 10_775 3_675 ? O1 Li1 Sr1 30.71(8) 3_675 3_675 ? O1 Li1 Sr1 99.06(9) . 3_675 ? O1 Li1 Sr1 89.32(9) 11_565 3_675 ? O1 Li1 Sr1 90.68(9) 2_765 3_675 ? B2 Li1 Sr1 128.65(12) 12_655 3_675 ? B2 Li1 Sr1 51.35(12) 3_675 3_675 ? B2 Li1 Sr1 86.05(11) 10_775 3_675 ? B2 Li1 Sr1 121.60(12) 2_765 3_675 ? B2 Li1 Sr1 58.40(12) 11_565 3_675 ? O3 B1 O4 119.1(4) . 2_655 ? O3 B1 O2 120.8(4) . 3_565 ? O4 B1 O2 120.1(4) 2_655 3_565 ? O3 B1 Sr1 96.0(3) . 3_565 ? O4 B1 Sr1 126.1(3) 2_655 3_565 ? O2 B1 Sr1 47.2(2) 3_565 3_565 ? O1 B2 O1 111.1(4) 11_565 . ? O1 B2 O4 109.4(4) 11_565 11_565 ? O1 B2 O4 111.0(4) . 11_565 ? O1 B2 O2 111.6(4) 11_565 . ? O1 B2 O2 106.5(4) . . ? O4 B2 O2 107.1(4) 11_565 . ? Sr1 F1 Sr1 149.67(12) . 2_765 ? Sr1 F1 Sr1 111.80(10) . 13_665 ? Sr1 F1 Sr1 96.41(9) 2_765 13_665 ? Sr1 F1 Sr2 94.74(9) . 13_665 ? Sr1 F1 Sr2 92.60(9) 2_765 13_665 ? Sr1 F1 Sr2 96.95(10) 13_665 13_665 ? Na1 Cl1 Na1 180.0 . 13_565 ? Na1 Cl1 Sr1 107.273(17) . 14_455 ? Na1 Cl1 Sr1 72.728(17) 13_565 14_455 ? Na1 Cl1 Sr1 72.729(17) . 2_665 ? Na1 Cl1 Sr1 107.271(18) 13_565 2_665 ? Sr1 Cl1 Sr1 180.0 14_455 2_665 ? Na1 Cl1 Sr1 72.729(18) . 3_565 ? Na1 Cl1 Sr1 107.272(17) 13_565 3_565 ? Sr1 Cl1 Sr1 68.422(16) 14_455 3_565 ? Sr1 Cl1 Sr1 111.579(16) 2_665 3_565 ? Na1 Cl1 Sr1 72.729(17) . . ? Na1 Cl1 Sr1 107.272(17) 13_565 . ? Sr1 Cl1 Sr1 68.422(16) 14_455 . ? Sr1 Cl1 Sr1 111.579(16) 2_665 . ? Sr1 Cl1 Sr1 111.579(16) 3_565 . ? Na1 Cl1 Sr1 107.272(17) . 15 ? Na1 Cl1 Sr1 72.727(17) 13_565 15 ? Sr1 Cl1 Sr1 111.578(16) 14_455 15 ? Sr1 Cl1 Sr1 68.421(16) 2_665 15 ? Sr1 Cl1 Sr1 180.0 3_565 15 ? Sr1 Cl1 Sr1 68.423(16) . 15 ? Na1 Cl1 Sr1 107.272(17) . 13_565 ? Na1 Cl1 Sr1 72.727(17) 13_565 13_565 ? Sr1 Cl1 Sr1 111.578(16) 14_455 13_565 ? Sr1 Cl1 Sr1 68.421(16) 2_665 13_565 ? Sr1 Cl1 Sr1 68.422(16) 3_565 13_565 ? Sr1 Cl1 Sr1 180.0 . 13_565 ? Sr1 Cl1 Sr1 111.577(16) 15 13_565 ? B2 O1 B2 123.6(2) 12_655 . ? B2 O1 Li1 90.1(3) 12_655 . ? B2 O1 Li1 89.7(2) . . ? B2 O1 Sr1 122.3(3) 12_655 . ? B2 O1 Sr1 103.6(3) . . ? Li1 O1 Sr1 123.86(14) . . ? B1 O2 B2 123.5(4) 2_665 . ? B1 O2 Na1 115.4(3) 2_665 . ? B2 O2 Na1 108.2(3) . . ? B1 O2 Sr1 110.5(3) 2_665 . ? B2 O2 Sr1 95.6(2) . . ? Na1 O2 Sr1 99.06(13) . . ? B1 O3 Sr1 139.0(3) . . ? B1 O3 Sr2 97.5(3) . . ? Sr1 O3 Sr2 99.61(11) . . ? B1 O3 Sr1 121.1(3) . 14_455 ? Sr1 O3 Sr1 95.87(11) . 14_455 ? Sr2 O3 Sr1 90.21(10) . 14_455 ? B1 O4 B2 121.7(4) 3_665 12_655 ? B1 O4 Sr2 90.4(3) 3_665 . ? B2 O4 Sr2 145.6(3) 12_655 . ? B1 O4 Na1 125.9(3) 3_665 10_665 ? B2 O4 Na1 88.9(3) 12_655 10_665 ? Sr2 O4 Na1 80.36(12) . 10_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.680 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.185 _database_code_depnum_ccdc_archive 'CCDC 969703'