# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # 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_1111 #TrackingRef 'Xray crystallographic file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B Ba Cl F4' _chemical_formula_weight 259.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.3244 2.2819 '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' B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 5.228(3) _cell_length_b 9.351(5) _cell_length_c 4.734(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 231.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1384 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.113 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.036 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 228 _exptl_absorpt_coefficient_mu 9.109 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3036 _exptl_absorpt_correction_T_max 0.5795 _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 '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 1427 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.53 _reflns_number_total 583 _reflns_number_gt 568 _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 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0188P)^2^+0.1086P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.105(4) _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 0.0(5) _refine_ls_number_reflns 583 _refine_ls_number_parameters 42 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.212 _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 Ba1 Ba 1.0000 0.70204(3) -0.0223 0.01399(16) Uani 1 2 d S . . Cl1 Cl 0.5000 0.51853(14) -0.0151(8) 0.0162(3) Uani 1 2 d S . . B1 B 0.5000 0.8673(8) 0.4030(16) 0.0204(18) Uani 1 2 d S . . F1 F 0.5000 0.8561(5) 0.1041(11) 0.0309(10) Uani 1 2 d S . . F2 F 1.2811(6) 0.7988(2) 0.468(4) 0.0336(10) Uani 1 1 d . . . F3 F 0.5000 1.0085(3) 0.477(3) 0.0344(9) Uani 1 2 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 Ba1 0.0150(2) 0.01226(19) 0.0147(2) -0.0003(4) 0.000 0.000 Cl1 0.0153(5) 0.0159(5) 0.0175(6) 0.0040(18) 0.000 0.000 B1 0.024(3) 0.016(3) 0.021(5) -0.001(2) 0.000 0.000 F1 0.038(3) 0.032(2) 0.023(2) 0.0003(18) 0.000 0.000 F2 0.0242(15) 0.0291(13) 0.047(3) -0.004(3) -0.014(5) -0.0081(9) F3 0.0378(19) 0.0153(16) 0.050(2) -0.008(6) 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 Ba1 F3 2.706(4) 2_674 ? Ba1 F2 2.892(15) . ? Ba1 F2 2.892(15) 4_755 ? Ba1 F2 2.967(17) 4_754 ? Ba1 F2 2.967(17) 1_554 ? Ba1 F1 3.044(3) 1_655 ? Ba1 F1 3.044(3) . ? Ba1 Cl1 3.114(3) 2_664 ? Ba1 Cl1 3.1272(15) . ? Ba1 Cl1 3.1272(15) 1_655 ? Ba1 Cl1 3.165(3) 2_665 ? Ba1 Ba1 4.734(3) 1_556 ? Cl1 Ba1 3.114(3) 2_665 ? Cl1 Ba1 3.1272(15) 1_455 ? Cl1 Ba1 3.165(3) 2_664 ? B1 F2 1.347(7) 1_455 ? B1 F2 1.347(7) 4_755 ? B1 F3 1.366(8) . ? B1 F1 1.419(8) . ? F1 Ba1 3.044(3) 1_455 ? F2 B1 1.347(7) 1_655 ? F2 Ba1 2.967(17) 1_556 ? F3 Ba1 2.706(4) 2_675 ? 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 F3 Ba1 F2 71.8(3) 2_674 . ? F3 Ba1 F2 71.8(3) 2_674 4_755 ? F2 Ba1 F2 61.1(4) . 4_755 ? F3 Ba1 F2 72.2(3) 2_674 4_754 ? F2 Ba1 F2 144.00(9) . 4_754 ? F2 Ba1 F2 107.79(10) 4_755 4_754 ? F3 Ba1 F2 72.2(3) 2_674 1_554 ? F2 Ba1 F2 107.79(10) . 1_554 ? F2 Ba1 F2 144.00(9) 4_755 1_554 ? F2 Ba1 F2 59.4(3) 4_754 1_554 ? F3 Ba1 F1 61.77(11) 2_674 1_655 ? F2 Ba1 F1 42.1(3) . 1_655 ? F2 Ba1 F1 97.51(16) 4_755 1_655 ? F2 Ba1 F1 116.15(12) 4_754 1_655 ? F2 Ba1 F1 65.8(2) 1_554 1_655 ? F3 Ba1 F1 61.77(11) 2_674 . ? F2 Ba1 F1 97.51(16) . . ? F2 Ba1 F1 42.1(3) 4_755 . ? F2 Ba1 F1 65.8(2) 4_754 . ? F2 Ba1 F1 116.15(12) 1_554 . ? F1 Ba1 F1 118.34(17) 1_655 . ? F3 Ba1 Cl1 131.4(3) 2_674 2_664 ? F2 Ba1 Cl1 143.94(10) . 2_664 ? F2 Ba1 Cl1 143.94(10) 4_755 2_664 ? F2 Ba1 Cl1 65.96(18) 4_754 2_664 ? F2 Ba1 Cl1 65.96(18) 1_554 2_664 ? F1 Ba1 Cl1 117.43(9) 1_655 2_664 ? F1 Ba1 Cl1 117.43(9) . 2_664 ? F3 Ba1 Cl1 123.28(3) 2_674 . ? F2 Ba1 Cl1 126.0(3) . . ? F2 Ba1 Cl1 74.82(12) 4_755 . ? F2 Ba1 Cl1 76.24(11) 4_754 . ? F2 Ba1 Cl1 126.2(2) 1_554 . ? F1 Ba1 Cl1 167.27(10) 1_655 . ? F1 Ba1 Cl1 62.60(10) . . ? Cl1 Ba1 Cl1 69.19(4) 2_664 . ? F3 Ba1 Cl1 123.28(3) 2_674 1_655 ? F2 Ba1 Cl1 74.82(12) . 1_655 ? F2 Ba1 Cl1 126.0(3) 4_755 1_655 ? F2 Ba1 Cl1 126.2(2) 4_754 1_655 ? F2 Ba1 Cl1 76.24(11) 1_554 1_655 ? F1 Ba1 Cl1 62.60(10) 1_655 1_655 ? F1 Ba1 Cl1 167.27(10) . 1_655 ? Cl1 Ba1 Cl1 69.19(4) 2_664 1_655 ? Cl1 Ba1 Cl1 113.42(6) . 1_655 ? F3 Ba1 Cl1 130.8(3) 2_674 2_665 ? F2 Ba1 Cl1 66.1(2) . 2_665 ? F2 Ba1 Cl1 66.1(2) 4_755 2_665 ? F2 Ba1 Cl1 144.66(8) 4_754 2_665 ? F2 Ba1 Cl1 144.66(8) 1_554 2_665 ? F1 Ba1 Cl1 99.17(9) 1_655 2_665 ? F1 Ba1 Cl1 99.17(9) . 2_665 ? Cl1 Ba1 Cl1 97.85(6) 2_664 2_665 ? Cl1 Ba1 Cl1 68.54(4) . 2_665 ? Cl1 Ba1 Cl1 68.54(4) 1_655 2_665 ? F3 Ba1 Ba1 90.1(3) 2_674 1_556 ? F2 Ba1 Ba1 36.6(3) . 1_556 ? F2 Ba1 Ba1 36.6(3) 4_755 1_556 ? F2 Ba1 Ba1 144.4(2) 4_754 1_556 ? F2 Ba1 Ba1 144.4(2) 1_554 1_556 ? F1 Ba1 Ba1 78.67(10) 1_655 1_556 ? F1 Ba1 Ba1 78.67(10) . 1_556 ? Cl1 Ba1 Ba1 138.52(6) 2_664 1_556 ? Cl1 Ba1 Ba1 89.38(7) . 1_556 ? Cl1 Ba1 Ba1 89.38(7) 1_655 1_556 ? Cl1 Ba1 Ba1 40.67(5) 2_665 1_556 ? Ba1 Cl1 Ba1 111.81(8) 2_665 . ? Ba1 Cl1 Ba1 111.81(8) 2_665 1_455 ? Ba1 Cl1 Ba1 113.42(6) . 1_455 ? Ba1 Cl1 Ba1 97.85(6) 2_665 2_664 ? Ba1 Cl1 Ba1 110.45(8) . 2_664 ? Ba1 Cl1 Ba1 110.45(8) 1_455 2_664 ? F2 B1 F2 116.3(8) 1_455 4_755 ? F2 B1 F3 113.7(5) 1_455 . ? F2 B1 F3 113.7(5) 4_755 . ? F2 B1 F1 101.1(9) 1_455 . ? F2 B1 F1 101.1(9) 4_755 . ? F3 B1 F1 109.1(7) . . ? B1 F1 Ba1 103.35(19) . 1_455 ? B1 F1 Ba1 103.35(19) . . ? Ba1 F1 Ba1 118.34(17) 1_455 . ? B1 F2 Ba1 113.4(11) 1_655 . ? B1 F2 Ba1 138.7(11) 1_655 1_556 ? Ba1 F2 Ba1 107.79(10) . 1_556 ? B1 F3 Ba1 165.3(9) . 2_675 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.590 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.187 _database_code_depnum_ccdc_archive 'CCDC 908748'