#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chi, Yun' 'Chou, Tsung-Yi' 'Lee, Gene-Hsiung' 'Liu, Chao-Shiuan' 'Peng, Shie-ming' 'Ranjan, Sudhir' _publ_contact_author_name 'Dr Yun Chi' _publ_contact_author_address ; Dr Yun Chi Department of Chemistry National Tsing Hua University Hsinchu Taiwan 30013 ; _publ_contact_author_email 'YCHI@MX.NTHU.EDU.TW' data_ic6957_complex_1 _database_code_CSD 163031 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H36 Cl4 F12 N2 O6 Sr' _chemical_formula_weight 881.95 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2804(2) _cell_length_b 11.4196(3) _cell_length_c 16.8509(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.152(1) _cell_angle_gamma 90.00 _cell_volume 1731.63(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular b' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method ? _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.968 _exptl_absorpt_correction_type ' empirical used sadabs' _exptl_absorpt_correction_T_min 0.4516 _exptl_absorpt_correction_T_max 0.5830 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10538 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3934 _reflns_number_observed 3525 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+2.5414P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3934 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_obs 0.0343 _refine_ls_wR_factor_all 0.0760 _refine_ls_wR_factor_obs 0.0734 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sr Sr 0.0000 0.0000 0.0000 0.01296(8) Uani 1 d S . F1 F 0.0867(2) -0.0310(2) 0.27859(10) 0.0408(4) Uani 1 d . . F2 F -0.0483(2) -0.18494(15) 0.26828(10) 0.0437(4) Uani 1 d . . F3 F -0.1131(2) -0.0279(2) 0.32149(9) 0.0462(5) Uani 1 d . . F4 F -0.3168(2) -0.18324(14) 0.17295(11) 0.0415(4) Uani 1 d . . F5 F -0.3758(2) -0.0161(2) 0.21360(11) 0.0463(5) Uani 1 d . . F6 F -0.3855(2) -0.04524(15) 0.08706(10) 0.0362(4) Uani 1 d . . O1 O 0.1748(2) 0.16331(15) 0.07778(10) 0.0238(4) Uani 1 d . . O2 O -0.2424(2) 0.12181(15) -0.07213(10) 0.0241(3) Uani 1 d . . O3 O -0.0811(2) -0.07646(13) 0.11691(9) 0.0203(3) Uani 1 d . . N1 N -0.1243(2) 0.1658(2) 0.09848(11) 0.0183(4) Uani 1 d . . C1 C 0.3320(3) 0.1574(2) 0.0858(2) 0.0315(6) Uani 1 d . . H1A H 0.3523(3) 0.1075(2) 0.0425(2) 0.047 Uiso 1 calc R . H1B H 0.3806(3) 0.1244(2) 0.1393(2) 0.047 Uiso 1 calc R . H1C H 0.3706(3) 0.2363(2) 0.0810(2) 0.047 Uiso 1 calc R . C2 C 0.1388(3) 0.2351(2) 0.13950(14) 0.0249(5) Uani 1 d . . H2A H 0.2010(3) 0.3067(2) 0.14735(14) 0.030 Uiso 1 calc R . H2B H 0.1591(3) 0.1921(2) 0.19205(14) 0.030 Uiso 1 calc R . C3 C -0.0233(3) 0.2682(2) 0.11381(15) 0.0235(5) Uani 1 d . . H3A H -0.0479(3) 0.3172(2) 0.15715(15) 0.028 Uiso 1 calc R . H3B H -0.0404(3) 0.3161(2) 0.06335(15) 0.028 Uiso 1 calc R . C4 C -0.2730(3) 0.1294(2) -0.15924(14) 0.0288(5) Uani 1 d . . H4A H -0.2442(3) 0.0560(2) -0.18128(14) 0.043 Uiso 1 calc R . H4B H -0.2164(3) 0.1944(2) -0.17462(14) 0.043 Uiso 1 calc R . H4C H -0.3795(3) 0.1431(2) -0.18160(14) 0.043 Uiso 1 calc R . C5 C -0.2825(3) 0.2267(2) -0.03700(15) 0.0256(5) Uani 1 d . . H5A H -0.3849(3) 0.2501(2) -0.06543(15) 0.031 Uiso 1 calc R . H5B H -0.2141(3) 0.2909(2) -0.04284(15) 0.031 Uiso 1 calc R . C6 C -0.2732(3) 0.2044(2) 0.05241(15) 0.0245(5) Uani 1 d . . H6A H -0.2997(3) 0.2772(2) 0.07748(15) 0.029 Uiso 1 calc R . H6B H -0.3469(3) 0.1438(2) 0.05705(15) 0.029 Uiso 1 calc R . C7 C -0.1324(3) 0.1116(2) 0.17689(14) 0.0232(5) Uani 1 d . . H7A H -0.2215(3) 0.1417(2) 0.19267(14) 0.028 Uiso 1 calc R . H7B H -0.0441(3) 0.1356(2) 0.21980(14) 0.028 Uiso 1 calc R . C8 C -0.1400(2) -0.0270(2) 0.17380(13) 0.0185(4) Uani 1 d . . C9 C -0.0548(3) -0.0680(2) 0.26082(15) 0.0280(5) Uani 1 d . . C10 C -0.3041(3) -0.0677(2) 0.16239(15) 0.0245(5) Uani 1 d . . C11 C -0.1116(4) 0.6350(2) 0.1156(2) 0.0388(7) Uani 1 d . . H11A H -0.1696(4) 0.6263(2) 0.1574(2) 0.047 Uiso 1 calc R . H11B H -0.1036(4) 0.7197(2) 0.1046(2) 0.047 Uiso 1 calc R . Cl1 Cl 0.06971(9) 0.57542(6) 0.15390(5) 0.0451(2) Uani 1 d . . Cl2 Cl -0.20467(12) 0.56360(7) 0.02497(5) 0.0588(2) Uani 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 Sr 0.01396(13) 0.01279(13) 0.01262(13) -0.00021(11) 0.00421(9) -0.00081(11) F1 0.0281(8) 0.0547(11) 0.0345(9) 0.0008(7) -0.0020(6) 0.0063(7) F2 0.0571(11) 0.0352(9) 0.0367(9) 0.0176(7) 0.0074(8) 0.0115(8) F3 0.0554(10) 0.0689(13) 0.0181(7) 0.0058(7) 0.0164(7) 0.0197(9) F4 0.0360(9) 0.0256(8) 0.0661(12) 0.0116(8) 0.0182(8) -0.0049(7) F5 0.0305(8) 0.0610(12) 0.0560(11) -0.0189(9) 0.0273(8) -0.0034(8) F6 0.0274(8) 0.0398(9) 0.0362(9) 0.0025(7) -0.0019(6) -0.0047(7) O1 0.0188(8) 0.0256(8) 0.0271(9) -0.0107(7) 0.0061(6) -0.0035(7) O2 0.0263(8) 0.0250(8) 0.0201(8) 0.0032(7) 0.0039(6) 0.0060(7) O3 0.0273(8) 0.0177(7) 0.0200(8) 0.0011(6) 0.0135(6) 0.0024(6) N1 0.0213(9) 0.0152(9) 0.0196(9) 0.0003(7) 0.0073(7) -0.0006(7) C1 0.0192(12) 0.0319(13) 0.043(2) -0.0076(12) 0.0065(10) -0.0039(10) C2 0.0288(12) 0.0214(11) 0.0235(11) -0.0090(9) 0.0047(9) -0.0059(9) C3 0.0287(12) 0.0155(10) 0.0279(12) -0.0032(9) 0.0101(10) -0.0005(9) C4 0.0240(12) 0.0388(14) 0.0219(12) 0.0045(10) 0.0022(9) 0.0004(10) C5 0.0239(12) 0.0208(11) 0.0316(13) 0.0050(10) 0.0058(10) 0.0058(9) C6 0.0233(11) 0.0220(11) 0.0310(13) 0.0006(10) 0.0119(10) 0.0049(9) C7 0.0326(13) 0.0198(11) 0.0197(11) -0.0023(9) 0.0112(9) -0.0011(9) C8 0.0201(10) 0.0197(11) 0.0172(10) 0.0023(8) 0.0073(8) 0.0022(8) C9 0.0296(13) 0.0336(14) 0.0220(12) 0.0047(10) 0.0089(10) 0.0072(10) C10 0.0256(12) 0.0230(11) 0.0287(12) 0.0010(9) 0.0136(10) 0.0015(9) C11 0.057(2) 0.0232(13) 0.043(2) 0.0026(12) 0.0259(14) 0.0009(12) Cl1 0.0513(4) 0.0283(3) 0.0614(5) 0.0019(3) 0.0249(4) -0.0047(3) Cl2 0.0896(7) 0.0368(4) 0.0450(5) 0.0051(3) 0.0069(4) 0.0020(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 Sr O3 2.4362(15) 3 ? Sr O3 2.4362(15) . ? Sr O1 2.605(2) . ? Sr O1 2.605(2) 3 ? Sr O2 2.671(2) . ? Sr O2 2.672(2) 3 ? Sr N1 2.933(2) . ? Sr N1 2.933(2) 3 ? F1 C9 1.342(3) . ? F2 C9 1.341(3) . ? F3 C9 1.349(3) . ? F4 C10 1.341(3) . ? F5 C10 1.348(3) . ? F6 C10 1.334(3) . ? O1 C2 1.427(3) . ? O1 C1 1.434(3) . ? O2 C5 1.426(3) . ? O2 C4 1.428(3) . ? O3 C8 1.339(3) . ? N1 C6 1.477(3) . ? N1 C7 1.478(3) . ? N1 C3 1.482(3) . ? C2 C3 1.508(3) . ? C5 C6 1.510(3) . ? C7 C8 1.584(3) . ? C8 C10 1.558(3) . ? C8 C9 1.558(3) . ? C11 Cl2 1.761(3) . ? C11 Cl1 1.783(3) . ? 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 O3 Sr O3 180.0 3 . ? O3 Sr O1 82.69(5) 3 . ? O3 Sr O1 97.31(5) . . ? O3 Sr O1 97.31(5) 3 3 ? O3 Sr O1 82.69(5) . 3 ? O1 Sr O1 180.0 . 3 ? O3 Sr O2 80.67(5) 3 . ? O3 Sr O2 99.33(5) . . ? O1 Sr O2 101.98(5) . . ? O1 Sr O2 78.02(5) 3 . ? O3 Sr O2 99.33(5) 3 3 ? O3 Sr O2 80.67(5) . 3 ? O1 Sr O2 78.02(5) . 3 ? O1 Sr O2 101.98(5) 3 3 ? O2 Sr O2 180.0 . 3 ? O3 Sr N1 117.92(5) 3 . ? O3 Sr N1 62.08(5) . . ? O1 Sr N1 62.36(5) . . ? O1 Sr N1 117.64(5) 3 . ? O2 Sr N1 61.14(5) . . ? O2 Sr N1 118.86(5) 3 . ? O3 Sr N1 62.08(5) 3 3 ? O3 Sr N1 117.92(5) . 3 ? O1 Sr N1 117.64(5) . 3 ? O1 Sr N1 62.36(5) 3 3 ? O2 Sr N1 118.86(5) . 3 ? O2 Sr N1 61.14(5) 3 3 ? N1 Sr N1 180.0 . 3 ? C2 O1 C1 111.9(2) . . ? C2 O1 Sr 123.40(13) . . ? C1 O1 Sr 120.53(14) . . ? C5 O2 C4 111.7(2) . . ? C5 O2 Sr 121.67(13) . . ? C4 O2 Sr 115.67(14) . . ? C8 O3 Sr 133.51(13) . . ? C6 N1 C7 110.5(2) . . ? C6 N1 C3 109.0(2) . . ? C7 N1 C3 110.1(2) . . ? C6 N1 Sr 110.02(13) . . ? C7 N1 Sr 110.40(13) . . ? C3 N1 Sr 106.77(12) . . ? O1 C2 C3 109.2(2) . . ? N1 C3 C2 113.3(2) . . ? O2 C5 C6 108.4(2) . . ? N1 C6 C5 113.1(2) . . ? N1 C7 C8 113.6(2) . . ? O3 C8 C10 110.1(2) . . ? O3 C8 C9 110.2(2) . . ? C10 C8 C9 106.4(2) . . ? O3 C8 C7 115.0(2) . . ? C10 C8 C7 109.6(2) . . ? C9 C8 C7 105.2(2) . . ? F2 C9 F1 105.9(2) . . ? F2 C9 F3 106.5(2) . . ? F1 C9 F3 106.0(2) . . ? F2 C9 C8 112.9(2) . . ? F1 C9 C8 111.0(2) . . ? F3 C9 C8 113.9(2) . . ? F6 C10 F4 105.5(2) . . ? F6 C10 F5 105.7(2) . . ? F4 C10 F5 105.8(2) . . ? F6 C10 C8 111.7(2) . . ? F4 C10 C8 113.1(2) . . ? F5 C10 C8 114.3(2) . . ? Cl2 C11 Cl1 110.9(2) . . ? _refine_diff_density_max 1.240 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.065 #===END data_ic6718_complex_2 _database_code_CSD 163032 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H32 Ba F12 N2 O6' _chemical_formula_weight 761.82 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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' 'Ba' 'Ba' -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.048(3) _cell_length_b 14.977(3) _cell_length_c 20.031(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.48(3) _cell_angle_gamma 90.00 _cell_volume 3005.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.06 _cell_measurement_theta_max 12.64 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method ? _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4145 _exptl_absorpt_correction_T_max 0.5926 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'NONIUS CAD4' _diffrn_measurement_method '\w--2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 25 _diffrn_reflns_number 5288 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5288 _reflns_number_observed 4202 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'NRCSDP DATRD2' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0434P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5288 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_obs 0.0286 _refine_ls_wR_factor_all 0.0761 _refine_ls_wR_factor_obs 0.0716 _refine_ls_goodness_of_fit_all 1.087 _refine_ls_goodness_of_fit_obs 1.158 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 1.158 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ba Ba 0.52292(2) 0.821901(13) 0.252087(8) 0.04226(9) Uani 1 d . . O1 O 0.6947(2) 0.9090(2) 0.32764(10) 0.0547(6) Uani 1 d . . O2 O 0.3052(3) 0.8031(2) 0.33623(14) 0.0790(8) Uani 1 d . . O3 O 0.6315(3) 0.6569(2) 0.30389(14) 0.0717(8) Uani 1 d . . O4 O 0.3275(2) 0.8932(2) 0.18188(11) 0.0566(6) Uani 1 d . . O5 O 0.7569(3) 0.8296(2) 0.18320(14) 0.0727(8) Uani 1 d . . O6 O 0.4072(3) 0.6783(2) 0.17606(14) 0.0713(7) Uani 1 d . . N1 N 0.5622(3) 0.7893(2) 0.40026(13) 0.0523(7) Uani 1 d . . N2 N 0.5161(3) 0.8254(2) 0.09811(13) 0.0517(7) Uani 1 d . . C1 C 0.6684(4) 0.9408(2) 0.3874(2) 0.0605(10) Uani 1 d . . C2 C 0.5963(5) 0.8735(3) 0.4333(2) 0.0701(11) Uani 1 d . . H2A H 0.6541(5) 0.8619(3) 0.4734(2) 0.084 Uiso 1 calc R . H2B H 0.5154(5) 0.9012(3) 0.4469(2) 0.084 Uiso 1 calc R . C3 C 0.4500(4) 0.7458(3) 0.4260(2) 0.0826(13) Uani 1 d . . H3A H 0.4628(4) 0.7443(3) 0.4745(2) 0.099 Uiso 1 calc R . H3B H 0.4460(4) 0.6846(3) 0.4102(2) 0.099 Uiso 1 calc R . C4 C 0.3184(5) 0.7914(3) 0.4057(2) 0.0807(13) Uani 1 d . . H4A H 0.2452(5) 0.7553(3) 0.4195(2) 0.097 Uiso 1 calc R . H4B H 0.3152(5) 0.8489(3) 0.4277(2) 0.097 Uiso 1 calc R . C5 C 0.1787(5) 0.8396(4) 0.3133(3) 0.128(2) Uani 1 d . . H5A H 0.1742(5) 0.8464(4) 0.2655(3) 0.193 Uiso 1 calc R . H5B H 0.1678(5) 0.8967(4) 0.3339(3) 0.193 Uiso 1 calc R . H5C H 0.1091(5) 0.8001(4) 0.3251(3) 0.193 Uiso 1 calc R . C6 C 0.6830(4) 0.7323(3) 0.4064(2) 0.0781(12) Uani 1 d . . H6A H 0.7558(4) 0.7652(3) 0.3889(2) 0.094 Uiso 1 calc R . H6B H 0.7069(4) 0.7218(3) 0.4536(2) 0.094 Uiso 1 calc R . C7 C 0.6717(4) 0.6450(3) 0.3721(2) 0.0745(12) Uani 1 d . . H7A H 0.7572(4) 0.6147(3) 0.3767(2) 0.089 Uiso 1 calc R . H7B H 0.6071(4) 0.6081(3) 0.3928(2) 0.089 Uiso 1 calc R . C8 C 0.6415(6) 0.5763(3) 0.2674(3) 0.111(2) Uani 1 d . . H8A H 0.6134(6) 0.5866(3) 0.2211(3) 0.167 Uiso 1 calc R . H8B H 0.5855(6) 0.5317(3) 0.2852(3) 0.167 Uiso 1 calc R . H8C H 0.7325(6) 0.5561(3) 0.2712(3) 0.167 Uiso 1 calc R . C9 C 0.5735(7) 1.0200(3) 0.3767(2) 0.094(2) Uani 1 d . . C10 C 0.7997(6) 0.9706(4) 0.4263(2) 0.103(2) Uani 1 d . . C11 C 0.3406(3) 0.9376(2) 0.1253(2) 0.0508(8) Uani 1 d . . C12 C 0.4080(4) 0.8837(3) 0.0704(2) 0.0586(9) Uani 1 d . . H12A H 0.3409(4) 0.8476(3) 0.0457(2) 0.070 Uiso 1 calc R . H12B H 0.4436(4) 0.9252(3) 0.0392(2) 0.070 Uiso 1 calc R . C13 C 0.6460(4) 0.8558(3) 0.0765(2) 0.0686(11) Uani 1 d . . H13A H 0.6517(4) 0.9201(3) 0.0815(2) 0.082 Uiso 1 calc R . H13B H 0.6496(4) 0.8422(3) 0.0293(2) 0.082 Uiso 1 calc R . C14 C 0.7642(4) 0.8143(3) 0.1146(2) 0.0747(12) Uani 1 d . . H14A H 0.7654(4) 0.7506(3) 0.1059(2) 0.090 Uiso 1 calc R . H14B H 0.8458(4) 0.8399(3) 0.1001(2) 0.090 Uiso 1 calc R . C15 C 0.8782(4) 0.8124(3) 0.2209(2) 0.093(2) Uani 1 d . . H15A H 0.8679(4) 0.8239(3) 0.2674(2) 0.139 Uiso 1 calc R . H15B H 0.9466(4) 0.8505(3) 0.2058(2) 0.139 Uiso 1 calc R . H15C H 0.9029(4) 0.7511(3) 0.2153(2) 0.139 Uiso 1 calc R . C16 C 0.4917(5) 0.7327(3) 0.0764(2) 0.0720(11) Uani 1 d . . H16A H 0.5715(5) 0.6978(3) 0.0880(2) 0.086 Uiso 1 calc R . H16B H 0.4753(5) 0.7317(3) 0.0280(2) 0.086 Uiso 1 calc R . C17 C 0.3759(5) 0.6894(3) 0.1068(2) 0.0785(13) Uani 1 d . . H17A H 0.2970(5) 0.7264(3) 0.0992(2) 0.094 Uiso 1 calc R . H17B H 0.3574(5) 0.6318(3) 0.0860(2) 0.094 Uiso 1 calc R . C18 C 0.3068(6) 0.6334(4) 0.2080(3) 0.128(2) Uani 1 d . . H18A H 0.3333(6) 0.6277(4) 0.2549(3) 0.192 Uiso 1 calc R . H18B H 0.2937(6) 0.5751(4) 0.1887(3) 0.192 Uiso 1 calc R . H18C H 0.2251(6) 0.6666(4) 0.2022(3) 0.192 Uiso 1 calc R . C19 C 0.4211(4) 1.0232(3) 0.1413(2) 0.0666(10) Uani 1 d . . C20 C 0.2012(4) 0.9648(3) 0.0928(2) 0.0750(12) Uani 1 d . . F1 F 0.4616(3) 0.9934(2) 0.3410(2) 0.1172(10) Uani 1 d . . F2 F 0.6232(4) 1.0862(2) 0.3408(2) 0.1291(12) Uani 1 d . . F3 F 0.5344(4) 1.0594(2) 0.4312(2) 0.1479(15) Uani 1 d . . F4 F 0.8654(4) 1.0318(2) 0.39391(15) 0.149(2) Uani 1 d . . F5 F 0.7786(5) 1.0076(2) 0.48662(14) 0.161(2) Uani 1 d . . F6 F 0.8813(3) 0.9054(3) 0.4389(2) 0.1300(13) Uani 1 d . . F7 F 0.5393(2) 1.0017(2) 0.17323(12) 0.0813(7) Uani 1 d . . F8 F 0.3655(3) 1.0798(2) 0.1809(2) 0.1147(10) Uani 1 d . . F9 F 0.4522(3) 1.0713(2) 0.08776(14) 0.1078(9) Uani 1 d . . F10 F 0.1315(3) 1.0139(2) 0.13306(15) 0.1135(10) Uani 1 d . . F11 F 0.2055(3) 1.0115(2) 0.03575(14) 0.1168(11) Uani 1 d . . F12 F 0.1272(3) 0.8941(2) 0.0775(2) 0.1090(9) Uani 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 Ba 0.04883(13) 0.04564(13) 0.03152(11) 0.00153(9) -0.00187(7) -0.00085(9) O1 0.071(2) 0.0550(14) 0.0382(12) -0.0026(11) 0.0039(11) -0.0138(12) O2 0.056(2) 0.118(2) 0.064(2) 0.013(2) 0.0089(13) -0.002(2) O3 0.091(2) 0.057(2) 0.064(2) 0.0006(13) -0.0058(15) 0.0216(14) O4 0.0564(14) 0.069(2) 0.0450(13) 0.0141(12) 0.0064(10) 0.0105(12) O5 0.0511(15) 0.108(2) 0.059(2) -0.005(2) 0.0040(12) 0.0117(15) O6 0.088(2) 0.061(2) 0.063(2) 0.0019(13) -0.0072(14) -0.0224(15) N1 0.065(2) 0.047(2) 0.043(2) 0.0074(13) -0.0037(13) -0.0103(14) N2 0.062(2) 0.055(2) 0.0378(14) -0.0004(13) 0.0047(12) 0.0109(14) C1 0.092(3) 0.050(2) 0.039(2) 0.000(2) 0.001(2) -0.023(2) C2 0.112(3) 0.061(3) 0.038(2) -0.003(2) 0.006(2) -0.021(2) C3 0.100(3) 0.088(3) 0.059(3) 0.020(2) 0.006(2) -0.029(3) C4 0.082(3) 0.100(3) 0.063(3) 0.012(2) 0.028(2) -0.004(3) C5 0.058(3) 0.203(7) 0.124(5) 0.060(5) 0.012(3) 0.023(4) C6 0.085(3) 0.078(3) 0.066(3) 0.017(2) -0.024(2) -0.001(2) C7 0.083(3) 0.062(2) 0.077(3) 0.013(2) -0.012(2) 0.013(2) C8 0.146(5) 0.092(4) 0.095(4) -0.018(3) 0.005(3) 0.050(4) C9 0.166(6) 0.055(3) 0.065(3) -0.007(2) 0.027(3) 0.006(3) C10 0.165(6) 0.087(4) 0.053(3) 0.012(3) -0.023(3) -0.068(4) C11 0.052(2) 0.060(2) 0.040(2) 0.006(2) 0.0035(14) 0.010(2) C12 0.072(2) 0.065(2) 0.037(2) 0.001(2) -0.005(2) 0.017(2) C13 0.071(3) 0.084(3) 0.052(2) 0.009(2) 0.018(2) 0.011(2) C14 0.065(3) 0.099(3) 0.063(3) 0.000(2) 0.019(2) 0.010(2) C15 0.059(3) 0.129(4) 0.088(3) -0.010(3) -0.010(2) 0.006(3) C16 0.105(3) 0.059(3) 0.051(2) -0.014(2) 0.000(2) 0.012(2) C17 0.097(3) 0.071(3) 0.065(3) -0.013(2) -0.015(2) -0.016(2) C18 0.140(5) 0.126(5) 0.118(5) 0.008(4) 0.011(4) -0.070(4) C19 0.080(3) 0.059(2) 0.061(2) 0.002(2) 0.009(2) 0.007(2) C20 0.063(3) 0.097(3) 0.064(3) 0.021(3) 0.001(2) 0.018(3) F1 0.127(3) 0.114(2) 0.111(2) 0.006(2) 0.013(2) 0.044(2) F2 0.217(4) 0.058(2) 0.118(2) 0.021(2) 0.047(2) 0.008(2) F3 0.259(4) 0.093(2) 0.100(2) -0.024(2) 0.066(3) 0.028(2) F4 0.193(3) 0.147(3) 0.099(2) 0.037(2) -0.042(2) -0.119(3) F5 0.272(5) 0.140(3) 0.064(2) -0.026(2) -0.027(2) -0.094(3) F6 0.114(2) 0.138(3) 0.129(3) 0.038(2) -0.051(2) -0.046(2) F7 0.079(2) 0.079(2) 0.083(2) -0.0059(13) -0.0096(13) -0.0120(13) F8 0.134(3) 0.076(2) 0.136(3) -0.041(2) 0.024(2) 0.017(2) F9 0.142(3) 0.085(2) 0.095(2) 0.036(2) 0.007(2) -0.026(2) F10 0.082(2) 0.149(3) 0.110(2) 0.006(2) 0.010(2) 0.060(2) F11 0.095(2) 0.167(3) 0.085(2) 0.061(2) -0.0105(15) 0.037(2) F12 0.062(2) 0.134(3) 0.128(2) 0.006(2) -0.0192(15) -0.003(2) _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 Ba O4 2.558(2) . ? Ba O1 2.562(2) . ? Ba O5 2.820(3) . ? Ba O6 2.832(3) . ? Ba O3 2.862(3) . ? Ba O2 2.878(3) . ? Ba N1 3.003(3) . ? Ba N2 3.080(3) . ? Ba F7 3.132(2) . ? Ba F1 3.212(3) . ? O1 C1 1.333(4) . ? O2 C4 1.398(5) . ? O2 C5 1.426(5) . ? O3 C7 1.406(5) . ? O3 C8 1.420(5) . ? O4 C11 1.330(4) . ? O5 C14 1.402(5) . ? O5 C15 1.407(5) . ? O6 C18 1.407(5) . ? O6 C17 1.408(5) . ? N1 C3 1.432(5) . ? N1 C2 1.453(4) . ? N1 C6 1.481(5) . ? N2 C12 1.468(4) . ? N2 C16 1.470(4) . ? N2 C13 1.479(5) . ? C1 C9 1.527(6) . ? C1 C10 1.545(6) . ? C1 C2 1.578(5) . ? C3 C4 1.515(6) . ? C6 C7 1.477(6) . ? C9 F3 1.326(5) . ? C9 F1 1.345(6) . ? C9 F2 1.344(5) . ? C10 F6 1.288(7) . ? C10 F4 1.329(5) . ? C10 F5 1.359(6) . ? C11 C19 1.536(5) . ? C11 C20 1.553(5) . ? C11 C12 1.560(5) . ? C13 C14 1.495(5) . ? C16 C17 1.501(6) . ? C19 F8 1.316(4) . ? C19 F7 1.343(4) . ? C19 F9 1.349(4) . ? C20 F12 1.315(5) . ? C20 F10 1.331(5) . ? C20 F11 1.343(5) . ? 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 Ba O1 124.41(9) . . ? O4 Ba O5 110.34(8) . . ? O1 Ba O5 73.69(8) . . ? O4 Ba O6 75.87(8) . . ? O1 Ba O6 159.03(8) . . ? O5 Ba O6 95.22(8) . . ? O4 Ba O3 144.49(8) . . ? O1 Ba O3 90.30(8) . . ? O5 Ba O3 84.51(8) . . ? O6 Ba O3 70.63(9) . . ? O4 Ba O2 77.10(7) . . ? O1 Ba O2 102.23(8) . . ? O5 Ba O2 172.57(8) . . ? O6 Ba O2 86.65(9) . . ? O3 Ba O2 89.35(8) . . ? O4 Ba N1 130.32(8) . . ? O1 Ba N1 57.90(7) . . ? O5 Ba N1 116.11(8) . . ? O6 Ba N1 115.13(8) . . ? O3 Ba N1 58.97(8) . . ? O2 Ba N1 56.80(8) . . ? O4 Ba N2 59.09(7) . . ? O1 Ba N2 122.97(8) . . ? O5 Ba N2 57.56(8) . . ? O6 Ba N2 59.88(8) . . ? O3 Ba N2 110.84(8) . . ? O2 Ba N2 129.01(8) . . ? N1 Ba N2 169.50(8) . . ? O4 Ba F7 55.42(7) . . ? O1 Ba F7 78.50(7) . . ? O5 Ba F7 68.85(7) . . ? O6 Ba F7 114.65(7) . . ? O3 Ba F7 153.02(8) . . ? O2 Ba F7 116.86(8) . . ? N1 Ba F7 129.06(7) . . ? N2 Ba F7 58.57(7) . . ? O4 Ba F1 78.40(8) . . ? O1 Ba F1 54.19(8) . . ? O5 Ba F1 116.22(9) . . ? O6 Ba F1 144.77(9) . . ? O3 Ba F1 124.97(8) . . ? O2 Ba F1 64.29(9) . . ? N1 Ba F1 66.30(8) . . ? N2 Ba F1 123.47(7) . . ? F7 Ba F1 67.20(8) . . ? C1 O1 Ba 122.7(2) . . ? C4 O2 C5 112.4(4) . . ? C4 O2 Ba 125.3(2) . . ? C5 O2 Ba 118.2(3) . . ? C7 O3 C8 111.4(3) . . ? C7 O3 Ba 122.3(2) . . ? C8 O3 Ba 126.0(3) . . ? C11 O4 Ba 123.7(2) . . ? C14 O5 C15 112.8(3) . . ? C14 O5 Ba 125.6(2) . . ? C15 O5 Ba 116.7(3) . . ? C18 O6 C17 113.0(4) . . ? C18 O6 Ba 113.4(3) . . ? C17 O6 Ba 119.4(2) . . ? C3 N1 C2 113.2(3) . . ? C3 N1 C6 111.8(3) . . ? C2 N1 C6 107.5(3) . . ? C3 N1 Ba 112.6(2) . . ? C2 N1 Ba 108.5(2) . . ? C6 N1 Ba 102.7(2) . . ? C12 N2 C16 110.4(3) . . ? C12 N2 C13 110.5(3) . . ? C16 N2 C13 109.6(3) . . ? C12 N2 Ba 110.3(2) . . ? C16 N2 Ba 105.7(2) . . ? C13 N2 Ba 110.3(2) . . ? O1 C1 C9 108.5(3) . . ? O1 C1 C10 109.6(4) . . ? C9 C1 C10 110.2(4) . . ? O1 C1 C2 115.3(3) . . ? C9 C1 C2 105.4(4) . . ? C10 C1 C2 107.6(3) . . ? N1 C2 C1 113.0(3) . . ? N1 C3 C4 113.1(3) . . ? O2 C4 C3 109.7(3) . . ? C7 C6 N1 116.0(3) . . ? O3 C7 C6 110.2(3) . . ? F3 C9 F1 106.3(5) . . ? F3 C9 F2 104.9(4) . . ? F1 C9 F2 105.3(4) . . ? F3 C9 C1 117.0(4) . . ? F1 C9 C1 109.3(4) . . ? F2 C9 C1 113.1(5) . . ? F6 C10 F4 106.6(6) . . ? F6 C10 F5 106.0(4) . . ? F4 C10 F5 105.8(4) . . ? F6 C10 C1 112.6(4) . . ? F4 C10 C1 113.0(4) . . ? F5 C10 C1 112.4(5) . . ? O4 C11 C19 108.9(3) . . ? O4 C11 C20 110.0(3) . . ? C19 C11 C20 108.2(3) . . ? O4 C11 C12 114.8(3) . . ? C19 C11 C12 109.2(3) . . ? C20 C11 C12 105.5(3) . . ? N2 C12 C11 113.0(3) . . ? N2 C13 C14 114.0(3) . . ? O5 C14 C13 109.4(3) . . ? N2 C16 C17 113.9(3) . . ? O6 C17 C16 109.3(3) . . ? F8 C19 F7 105.6(3) . . ? F8 C19 F9 105.7(3) . . ? F7 C19 F9 104.8(3) . . ? F8 C19 C11 115.0(3) . . ? F7 C19 C11 109.3(3) . . ? F9 C19 C11 115.5(3) . . ? F12 C20 F10 105.7(4) . . ? F12 C20 F11 106.1(4) . . ? F10 C20 F11 106.3(4) . . ? F12 C20 C11 111.2(4) . . ? F10 C20 C11 113.0(3) . . ? F11 C20 C11 113.9(3) . . ? C9 F1 Ba 110.1(3) . . ? C19 F7 Ba 111.5(2) . . ? _refine_diff_density_max 0.457 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.066 #===END #----Original Message----- From: DALTON (shared) Sent: 30 April 2001 17:35 To: 'KRUHLAND@SYR.EDU' Subject: Dalton MS: B103310G <>