# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2162 data_complex_3 #--------------------------------- _audit_creation_date 'Thu Jan 13 11:08:02 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ _cell_length_a 28.454(2) _cell_length_b 6.991(2) _cell_length_c 20.473(2) _cell_angle_alpha 90 _cell_angle_beta 106.756(6) _cell_angle_gamma 90 _cell_volume 3899.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 23.3 _cell_measurement_theta_max 29.1 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'opaque white' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 640.93 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H15 F6 Hg N2 O P S' _chemical_formula_moiety '(C17 H15 N2 O1 S1 Hg1) (P1F6)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2432.00 _exptl_absorpt_coefficient_mu 8.170 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.855 #--------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillationcounter _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -2.26 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3841 _reflns_number_total 3755 _reflns_number_observed 2168 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.26 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.02102 _diffrn_orient_matrix_UB_12 -0.01806 _diffrn_orient_matrix_UB_13 -0.03114 _diffrn_orient_matrix_UB_21 -0.02844 _diffrn_orient_matrix_UB_22 0.03417 _diffrn_orient_matrix_UB_23 -0.03998 _diffrn_orient_matrix_UB_31 0.00981 _diffrn_orient_matrix_UB_32 0.13771 _diffrn_orient_matrix_UB_33 0.00584 #------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_image _atom_type_scat_source C 0 136 0.003 0.002 'International Tables' H 0 120 0.000 0.000 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 8 0.011 0.006 'International Tables' F 0 48 0.017 0.010 'International Tables' P 0 8 0.102 0.094 'International Tables' S 0 8 0.125 0.123 'International Tables' Hg 0 8 -2.389 9.227 'International Tables' #------------------------------------------------------------------- loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Hg(1) 0.21362(1) 0.19687(5) 0.20632(2) 0.0632(1) Uij ? ? S(1) 0.26037(7) 0.0804(3) 0.31278(9) 0.0533(6) Uij ? ? P(1) 0.40259(8) -0.1169(5) 0.1313(1) 0.0743(8) Uij ? ? F(1) 0.4421(2) -0.117(1) 0.2025(3) 0.138(3) Uij ? ? F(2) 0.3620(2) -0.112(1) 0.0603(3) 0.121(2) Uij ? ? F(3) 0.4408(2) -0.028(1) 0.1008(3) 0.157(3) Uij ? ? F(4) 0.3625(2) -0.178(2) 0.1637(4) 0.199(4) Uij ? ? F(5) 0.4169(4) -0.313(1) 0.1181(6) 0.256(5) Uij ? ? F(6) 0.3871(3) 0.092(1) 0.1435(5) 0.187(4) Uij ? ? O(1) 0.4659(2) 0.3429(9) 0.3823(3) 0.081(2) Uij ? ? N(1) 0.2131(2) 0.1184(9) 0.0958(3) 0.052(2) Uij ? ? N(2) 0.1373(2) 0.2403(8) 0.1405(3) 0.047(2) Uij ? ? C(1) 0.3202(3) 0.181(1) 0.3285(4) 0.048(2) Uij ? ? C(2) 0.3411(3) 0.233(1) 0.2780(4) 0.054(2) Uij ? ? C(3) 0.3893(3) 0.289(1) 0.2934(4) 0.061(3) Uij ? ? C(4) 0.4174(3) 0.297(1) 0.3611(4) 0.059(2) Uij ? ? C(5) 0.3958(3) 0.253(1) 0.4127(4) 0.056(2) Uij ? ? C(6) 0.3478(3) 0.196(1) 0.3962(4) 0.052(2) Uij ? ? C(7) 0.4905(4) 0.373(2) 0.3313(6) 0.102(4) Uij ? ? C(8) 0.2511(3) 0.046(1) 0.0767(5) 0.069(3) Uij ? ? C(9) 0.2463(3) -0.002(1) 0.0101(5) 0.079(3) Uij ? ? C(10) 0.2019(4) 0.022(2) -0.0372(4) 0.086(4) Uij ? ? C(11) 0.1636(3) 0.095(1) -0.0186(4) 0.069(3) Uij ? ? C(12) 0.1699(3) 0.1399(10) 0.0485(4) 0.050(2) Uij ? ? C(13) 0.1280(3) 0.211(1) 0.0732(4) 0.049(2) Uij ? ? C(14) 0.0810(3) 0.234(1) 0.0303(4) 0.069(3) Uij ? ? C(15) 0.0441(3) 0.290(1) 0.0580(5) 0.074(3) Uij ? ? C(16) 0.0542(3) 0.321(1) 0.1261(5) 0.072(3) Uij ? ? C(17) 0.1012(3) 0.295(1) 0.1663(4) 0.057(2) Uij ? ? H(1) 0.3217 0.2292 0.2317 0.0644 Uij ? ? H(2) 0.4032 0.3219 0.2580 0.0734 Uij ? ? H(3) 0.4146 0.2624 0.4592 0.0672 Uij ? ? H(4) 0.3333 0.1664 0.4314 0.0626 Uij ? ? H(5) 0.5239 0.4049 0.3525 0.1223 Uij ? ? H(6) 0.4889 0.2598 0.3051 0.1223 Uij ? ? H(7) 0.4751 0.4749 0.3021 0.1223 Uij ? ? H(8) 0.2818 0.0269 0.1101 0.0826 Uij ? ? H(9) 0.2735 -0.0503 -0.0029 0.0946 Uij ? ? H(10) 0.1978 -0.0126 -0.0834 0.1036 Uij ? ? H(11) 0.1328 0.1144 -0.0516 0.0824 Uij ? ? H(12) 0.0741 0.2122 -0.0173 0.0827 Uij ? ? H(13) 0.0117 0.3076 0.0291 0.0893 Uij ? ? H(14) 0.0291 0.3597 0.1454 0.0864 Uij ? ? H(15) 0.1085 0.3158 0.2140 0.0678 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg(1) 0.0566(2) 0.0700(2) 0.0520(2) 0.0062(2) -0.0018(1) 0.0047(2) S(1) 0.050(1) 0.060(1) 0.046(1) 0.0031(10) 0.0067(8) 0.0044(10) P(1) 0.055(1) 0.108(2) 0.057(1) -0.002(1) 0.011(1) -0.005(1) F(1) 0.089(4) 0.228(8) 0.073(4) -0.037(5) -0.015(3) 0.027(5) F(2) 0.087(4) 0.199(7) 0.063(3) 0.013(4) -0.003(3) -0.019(4) F(3) 0.097(4) 0.27(1) 0.107(5) -0.024(6) 0.037(4) 0.039(6) F(4) 0.093(5) 0.39(2) 0.102(5) -0.060(7) 0.015(4) 0.078(7) F(5) 0.23(1) 0.111(7) 0.31(1) 0.079(7) -0.108(10) -0.075(8) F(6) 0.170(8) 0.186(9) 0.180(8) 0.041(7) 0.010(6) -0.067(7) O(1) 0.055(3) 0.105(5) 0.080(4) -0.004(3) 0.014(3) -0.010(4) N(1) 0.052(4) 0.050(4) 0.055(4) 0.001(3) 0.014(3) -0.006(3) N(2) 0.039(3) 0.056(4) 0.046(3) -0.004(3) 0.009(3) 0.001(3) C(1) 0.052(4) 0.044(4) 0.047(4) 0.004(4) 0.010(3) -0.006(4) C(2) 0.057(5) 0.056(5) 0.047(4) 0.007(4) 0.013(4) 0.001(4) C(3) 0.065(5) 0.059(5) 0.062(5) 0.001(5) 0.024(4) 0.000(5) C(4) 0.052(5) 0.051(5) 0.072(5) 0.006(4) 0.014(4) -0.007(5) C(5) 0.059(5) 0.051(5) 0.050(4) 0.007(4) 0.003(4) -0.003(3) C(6) 0.059(5) 0.049(4) 0.046(4) 0.005(4) 0.010(3) -0.004(4) C(7) 0.079(7) 0.127(10) 0.110(8) -0.009(7) 0.044(6) -0.001(7) C(8) 0.056(5) 0.068(6) 0.090(6) 0.005(4) 0.032(5) -0.003(5) C(9) 0.081(6) 0.071(6) 0.100(7) -0.002(5) 0.051(6) -0.024(6) C(10) 0.109(8) 0.092(8) 0.067(6) -0.025(7) 0.041(6) -0.015(6) C(11) 0.067(5) 0.079(6) 0.061(5) -0.001(5) 0.020(4) -0.008(5) C(12) 0.065(5) 0.038(4) 0.049(4) -0.004(3) 0.019(4) -0.003(3) C(13) 0.055(4) 0.036(4) 0.052(4) -0.002(4) 0.011(3) 0.003(4) C(14) 0.058(5) 0.072(6) 0.062(5) -0.001(4) -0.008(4) -0.002(4) C(15) 0.038(4) 0.075(6) 0.096(7) -0.002(5) -0.004(4) -0.010(6) C(16) 0.050(5) 0.065(6) 0.104(7) 0.001(4) 0.026(5) -0.008(6) C(17) 0.057(5) 0.056(5) 0.063(5) -0.007(4) 0.028(4) -0.004(4) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2168 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0279 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0348 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.371 _refine_ls_shift/esd_max 0.0280 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.50 _refine_diff_density_max 0.73 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg(1) S(1) 2.348(2) ? ? yes Hg(1) S(1) 2.839(2) ? ? yes Hg(1) N(1) 2.325(6) ? ? yes Hg(1) N(2) 2.223(6) ? ? yes S(1) C(1) 1.782(7) ? ? yes P(1) F(1) 1.563(5) ? ? yes P(1) F(2) 1.574(6) ? ? yes P(1) F(3) 1.531(6) ? ? yes P(1) F(4) 1.536(7) ? ? yes P(1) F(5) 1.475(8) ? ? yes P(1) F(6) 1.565(9) ? ? yes O(1) C(4) 1.361(9) ? ? yes O(1) C(7) 1.43(1) ? ? yes N(1) C(8) 1.349(9) ? ? yes N(1) C(12) 1.336(9) ? ? yes N(2) C(13) 1.342(9) ? ? yes N(2) C(17) 1.338(9) ? ? yes C(1) C(2) 1.382(10) ? ? yes C(1) C(6) 1.386(10) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(3) C(4) 1.39(1) ? ? yes C(4) C(5) 1.40(1) ? ? yes C(5) C(6) 1.37(1) ? ? yes C(8) C(9) 1.37(1) ? ? yes C(9) C(10) 1.36(1) ? ? yes C(10) C(11) 1.35(1) ? ? yes C(11) C(12) 1.37(1) ? ? yes C(12) C(13) 1.509(10) ? ? yes C(13) C(14) 1.38(1) ? ? yes C(14) C(15) 1.38(1) ? ? yes C(15) C(16) 1.36(1) ? ? yes C(16) C(17) 1.37(1) ? ? yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Hg(1) S(1) 110.80(5) ? ? ? yes S(1) Hg(1) N(1) 131.6(2) ? ? ? yes S(1) Hg(1) N(2) 143.5(1) ? ? ? yes S(1) Hg(1) N(1) 91.0(2) ? ? ? yes S(1) Hg(1) N(2) 92.0(2) ? ? ? yes N(1) Hg(1) N(2) 73.2(2) ? ? ? yes Hg(1) S(1) Hg(1) 107.47(7) ? ? ? yes Hg(1) S(1) C(1) 106.7(2) ? ? ? yes Hg(1) S(1) C(1) 97.1(2) ? ? ? yes F(1) P(1) F(2) 178.5(4) ? ? ? yes F(1) P(1) F(3) 88.7(3) ? ? ? yes F(1) P(1) F(4) 91.2(4) ? ? ? yes F(1) P(1) F(5) 90.5(5) ? ? ? yes F(1) P(1) F(6) 90.7(5) ? ? ? yes F(2) P(1) F(3) 91.8(3) ? ? ? yes F(2) P(1) F(4) 88.1(4) ? ? ? yes F(2) P(1) F(5) 90.9(5) ? ? ? yes F(2) P(1) F(6) 87.9(4) ? ? ? yes F(3) P(1) F(4) 172.4(6) ? ? ? yes F(3) P(1) F(5) 92.0(7) ? ? ? yes F(3) P(1) F(6) 87.3(5) ? ? ? yes F(4) P(1) F(5) 95.6(7) ? ? ? yes F(4) P(1) F(6) 85.1(6) ? ? ? yes F(5) P(1) F(6) 178.6(6) ? ? ? yes C(4) O(1) C(7) 117.9(7) ? ? ? yes Hg(1) N(1) C(8) 126.1(5) ? ? ? yes Hg(1) N(1) C(12) 115.1(5) ? ? ? yes C(8) N(1) C(12) 118.6(6) ? ? ? yes Hg(1) N(2) C(13) 118.1(4) ? ? ? yes Hg(1) N(2) C(17) 121.8(5) ? ? ? yes C(13) N(2) C(17) 120.2(6) ? ? ? yes S(1) C(1) C(2) 124.3(6) ? ? ? yes S(1) C(1) C(6) 116.6(6) ? ? ? yes C(2) C(1) C(6) 119.1(7) ? ? ? yes C(1) C(2) C(3) 121.4(7) ? ? ? yes C(2) C(3) C(4) 119.4(7) ? ? ? yes O(1) C(4) C(3) 124.6(8) ? ? ? yes O(1) C(4) C(5) 115.9(7) ? ? ? yes C(3) C(4) C(5) 119.6(7) ? ? ? yes C(4) C(5) C(6) 120.0(7) ? ? ? yes C(1) C(6) C(5) 120.4(7) ? ? ? yes N(1) C(8) C(9) 121.3(8) ? ? ? yes C(8) C(9) C(10) 119.0(8) ? ? ? yes C(9) C(10) C(11) 120.1(8) ? ? ? yes C(10) C(11) C(12) 119.1(8) ? ? ? yes N(1) C(12) C(11) 121.9(7) ? ? ? yes N(1) C(12) C(13) 116.5(6) ? ? ? yes C(11) C(12) C(13) 121.6(7) ? ? ? yes N(2) C(13) C(12) 117.0(6) ? ? ? yes N(2) C(13) C(14) 120.2(7) ? ? ? yes C(12) C(13) C(14) 122.7(7) ? ? ? yes C(13) C(14) C(15) 118.8(8) ? ? ? yes C(14) C(15) C(16) 120.3(8) ? ? ? yes C(15) C(16) C(17) 118.5(7) ? ? ? yes N(2) C(17) C(16) 122.0(7) ? ? ? yes #----------------------------------------------------------------------- data_complex_5 #--------------------------- _audit_creation_date 'Thu Jan 20 10:35:09 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC DiffractometerControl' _computing_cell_refinement 'MSC/AFC DiffractometerControl' _computing_data_reduction 'teXsan' _computing_structure_solution DIRDIF92(PATTY) _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ _cell_length_a 12.786(1) _cell_length_b 7.134(4) _cell_length_c 20.342(2) _cell_angle_alpha 90 _cell_angle_beta 95.977(8) _cell_angle_gamma 90 _cell_volume 1845(1) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 36.9 _cell_measurement_theta_max 42.6 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #----------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.368 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 657.81 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H13 F6 Hg N2 P Se' _chemical_formula_moiety '(C16 H13 N2 Se1 Hg1) (P1F6)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1224.00 _exptl_absorpt_coefficient_mu 10.483 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.557 #--------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-raytube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillationcounter _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -4.20 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3651 _reflns_number_total 3495 _reflns_number_observed 2187 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.38 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00749 _diffrn_orient_matrix_UB_12 -0.02395 _diffrn_orient_matrix_UB_13 -0.04870 _diffrn_orient_matrix_UB_21 0.07346 _diffrn_orient_matrix_UB_22 -0.04989 _diffrn_orient_matrix_UB_23 0.00340 _diffrn_orient_matrix_UB_31 -0.02706 _diffrn_orient_matrix_UB_32 -0.12880 _diffrn_orient_matrix_UB_33 0.00774 #------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.003 0.002 'InternationalTables' H 0 52 0.000 0.000 'International Tables' N 0 8 0.006 0.003 'International Tables' F 0 24 0.017 0.010 'International Tables' P 0 4 0.102 0.094 'International Tables' Se 0 4 -0.093 2.226 'International Tables' Hg 0 4 -2.389 9.227 'InternationalTables' #------------------------------------------------------------------- loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Hg(1) 0.08176(2) 0.00055(5) 0.28375(1) 0.0563(1) Uij ? ? Se(1) -0.02362(5) -0.1235(1) 0.18543(4) 0.0465(2) Uij ? ? P(1) 0.3234(2) 0.1033(5) 0.0995(1) 0.0721(8) Uij ? ? F(1) 0.3957(4) 0.092(2) 0.1651(3) 0.180(3) Uij ? ? F(2) 0.2479(5) 0.112(1) 0.0343(3) 0.129(3) Uij ? ? F(3) 0.3451(8) -0.105(1) 0.0890(5) 0.205(5) Uij ? ? F(4) 0.3006(7) 0.311(1) 0.1069(5) 0.192(4) Uij ? ? F(5) 0.2271(4) 0.061(1) 0.1388(3) 0.167(3) Uij ? ? F(6) 0.4192(4) 0.161(1) 0.0627(3) 0.149(3) Uij ? ? N(1) 0.0748(4) -0.0963(8) 0.3942(3) 0.047(2) Uij ? ? N(2) 0.2411(4) 0.0455(8) 0.3363(3) 0.043(2) Uij ? ? C(1) -0.0040(6) -0.185(1) 0.4181(4) 0.061(3) Uij ? ? C(2) 0.0002(7) -0.252(1) 0.4820(5) 0.066(3) Uij ? ? C(3) 0.0928(8) -0.227(1) 0.5212(4) 0.074(3) Uij ? ? C(4) 0.1753(6) -0.139(1) 0.4971(4) 0.064(3) Uij ? ? C(5) 0.1654(6) -0.073(1) 0.4331(4) 0.046(2) Uij ? ? C(6) 0.2538(5) 0.013(1) 0.4030(4) 0.047(2) Uij ? ? C(7) 0.3489(7) 0.059(1) 0.4379(4) 0.070(3) Uij ? ? C(8) 0.4284(6) 0.132(1) 0.4064(5) 0.074(3) Uij ? ? C(9) 0.4169(6) 0.156(1) 0.3390(5) 0.068(3) Uij ? ? C(10) 0.3195(6) 0.115(1) 0.3051(4) 0.055(2) Uij ? ? C(11) -0.1595(5) -0.0090(10) 0.1923(4) 0.049(2) Uij ? ? C(12) -0.2220(7) 0.014(1) 0.1328(5) 0.069(3) Uij ? ? C(13) -0.3226(7) 0.088(1) 0.1354(5) 0.075(3) Uij ? ? C(14) -0.3570(7) 0.140(1) 0.1953(7) 0.089(4) Uij ? ? C(15) -0.2932(7) 0.118(1) 0.2533(5) 0.079(3) Uij ? ? C(16) -0.1928(6) 0.042(1) 0.2517(4) 0.059(3) Uij ? ? H(1) -0.0671 -0.2025 0.3897 0.0727 Uij ? ? H(2) -0.0583 -0.3129 0.4978 0.0794 Uij ? ? H(3) 0.0995 -0.2714 0.5655 0.0884 Uij ? ? H(4) 0.2396 -0.1225 0.5244 0.0764 Uij ? ? H(5) 0.3589 0.0379 0.4843 0.0845 Uij ? ? H(6) 0.4926 0.1662 0.4313 0.0888 Uij ? ? H(7) 0.4734 0.2007 0.3163 0.0815 Uij ? ? H(8) 0.3085 0.1361 0.2587 0.0661 Uij ? ? H(9) -0.1973 -0.0190 0.0919 0.0820 Uij ? ? H(10) -0.3680 0.1032 0.0957 0.0903 Uij ? ? H(11) -0.4255 0.1908 0.1960 0.1074 Uij ? ? H(12) -0.3170 0.1548 0.2940 0.0949 Uij ? ? H(13) -0.1479 0.0258 0.2915 0.0708 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hg(1) 0.0473(2) 0.0723(2) 0.0462(2) -0.0061(2) -0.0103(1) -0.0004(2) Se(1) 0.0429(4) 0.0572(4) 0.0383(4) -0.0019(4) -0.0012(3) -0.0025(4) P(1) 0.050(1) 0.116(2) 0.049(1) 0.010(2) -0.0004(10) 0.001(2) F(1) 0.057(3) 0.43(1) 0.055(3) -0.017(6) -0.002(3) 0.031(6) F(2) 0.091(4) 0.217(8) 0.070(4) 0.001(5) -0.027(3) 0.017(5) F(3) 0.207(9) 0.136(7) 0.26(1) 0.078(7) -0.022(9) -0.013(8) F(4) 0.216(9) 0.123(7) 0.24(1) -0.006(7) 0.056(9) -0.068(7) F(5) 0.051(3) 0.34(1) 0.109(5) 0.011(5) 0.012(3) 0.086(6) F(6) 0.080(4) 0.29(1) 0.086(4) -0.001(5) 0.026(3) 0.048(6) N(1) 0.046(3) 0.051(4) 0.046(3) 0.000(3) 0.006(3) 0.004(3) N(2) 0.033(3) 0.053(4) 0.041(3) 0.002(3) 0.000(3) 0.008(3) C(1) 0.054(5) 0.052(5) 0.076(6) -0.003(4) 0.008(4) 0.000(4) C(2) 0.067(5) 0.058(5) 0.080(6) 0.000(5) 0.039(5) 0.013(5) C(3) 0.091(7) 0.076(6) 0.056(5) 0.009(6) 0.017(5) 0.023(5) C(4) 0.066(5) 0.081(6) 0.045(5) 0.001(5) 0.011(4) 0.012(5) C(5) 0.055(5) 0.042(4) 0.042(4) 0.005(4) 0.007(4) 0.004(4) C(6) 0.040(4) 0.051(4) 0.047(4) 0.005(4) -0.004(3) -0.001(4) C(7) 0.062(5) 0.083(7) 0.060(5) -0.010(5) -0.025(4) 0.006(5) C(8) 0.038(4) 0.089(7) 0.090(7) -0.005(5) -0.018(4) 0.007(6) C(9) 0.034(4) 0.084(6) 0.088(7) -0.003(4) 0.014(4) 0.003(6) C(10) 0.046(4) 0.065(5) 0.053(5) 0.005(4) 0.002(4) 0.001(5) C(11) 0.039(4) 0.047(4) 0.057(5) -0.003(4) -0.013(3) 0.004(4) C(12) 0.070(6) 0.053(5) 0.078(6) -0.005(5) -0.016(5) 0.017(5) C(13) 0.047(5) 0.069(6) 0.104(8) -0.009(5) -0.017(5) 0.025(6) C(14) 0.046(5) 0.070(6) 0.15(1) -0.002(5) 0.013(6) 0.017(8) C(15) 0.055(5) 0.080(7) 0.106(8) -0.007(5) 0.030(5) -0.014(7) C(16) 0.048(4) 0.073(6) 0.059(5) -0.007(4) 0.015(4) -0.011(4) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.73159 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2187 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0285 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0364 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.730 _refine_ls_shift/esd_max 0.0300 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.09 _refine_diff_density_max 1.09 #---------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg(1) Se(1) 2.4571(8) ? ? yes Hg(1) Se(1) 2.8695(8) ? ? yes Hg(1) N(1) 2.360(6) ? ? yes Hg(1) N(2) 2.223(5) ? ? yes Se(1) C(11) 1.938(7) ? ? yes P(1) F(1) 1.545(6) ? ? yes P(1) F(2) 1.558(6) ? ? yes P(1) F(3) 1.528(9) ? ? yes P(1) F(4) 1.520(8) ? ? yes P(1) F(5) 1.567(6) ? ? yes P(1) F(6) 1.555(6) ? ? yes N(1) C(1) 1.323(9) ? ? yes N(1) C(5) 1.343(9) ? ? yes N(2) C(6) 1.368(9) ? ? yes N(2) C(10) 1.337(9) ? ? yes C(1) C(2) 1.38(1) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(3) C(4) 1.36(1) ? ? yes C(4) C(5) 1.38(1) ? ? yes C(5) C(6) 1.476(10) ? ? yes C(6) C(7) 1.38(1) ? ? yes C(7) C(8) 1.36(1) ? ? yes C(8) C(9) 1.38(1) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(11) C(12) 1.39(1) ? ? yes C(11) C(16) 1.37(1) ? ? yes C(12) C(13) 1.40(1) ? ? yes C(13) C(14) 1.39(1) ? ? yes C(14) C(15) 1.37(1) ? ? yes C(15) C(16) 1.40(1) ? ? yes #----------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Hg(1) Se(1) 112.45(2) ? ? ? yes Se(1) Hg(1) N(1) 126.7(1) ? ? ? yes Se(1) Hg(1) N(2) 147.2(1) ? ? ? yes Se(1) Hg(1) N(1) 91.7(1) ? ? ? yes Se(1) Hg(1) N(2) 90.3(1) ? ? ? yes N(1) Hg(1) N(2) 73.0(2) ? ? ? yes Hg(1) Se(1) Hg(1) 106.94(3) ? ? ? yes Hg(1) Se(1) C(11) 102.1(2) ? ? ? yes Hg(1) Se(1) C(11) 97.1(2) ? ? ? yes F(1) P(1) F(2) 178.4(4) ? ? ? yes F(1) P(1) F(3) 88.2(6) ? ? ? yes F(1) P(1) F(4) 94.0(6) ? ? ? yes F(1) P(1) F(5) 88.8(3) ? ? ? yes F(1) P(1) F(6) 89.9(3) ? ? ? yes F(2) P(1) F(3) 91.5(5) ? ? ? yes F(2) P(1) F(4) 86.4(5) ? ? ? yes F(2) P(1) F(5) 89.6(4) ? ? ? yes F(2) P(1) F(6) 91.7(3) ? ? ? yes F(3) P(1) F(4) 177.7(6) ? ? ? yes F(3) P(1) F(5) 92.8(6) ? ? ? yes F(3) P(1) F(6) 91.4(5) ? ? ? yes F(4) P(1) F(5) 88.2(5) ? ? ? yes F(4) P(1) F(6) 87.8(5) ? ? ? yes F(5) P(1) F(6) 175.6(6) ? ? ? yes Hg(1) N(1) C(1) 126.5(5) ? ? ? yes Hg(1) N(1) C(5) 114.2(4) ? ? ? yes C(1) N(1) C(5) 119.0(7) ? ? ? yes Hg(1) N(2) C(6) 117.5(4) ? ? ? yes Hg(1) N(2) C(10) 121.3(5) ? ? ? yes C(6) N(2) C(10) 121.0(6) ? ? ? yes N(1) C(1) C(2) 123.7(8) ? ? ? yes C(1) C(2) C(3) 116.7(7) ? ? ? yes C(2) C(3) C(4) 120.4(8) ? ? ? yes C(3) C(4) C(5) 119.9(8) ? ? ? yes N(1) C(5) C(4) 120.3(7) ? ? ? yes N(1) C(5) C(6) 117.2(6) ? ? ? yes C(4) C(5) C(6) 122.3(7) ? ? ? yes N(2) C(6) C(5) 117.6(6) ? ? ? yes N(2) C(6) C(7) 118.5(7) ? ? ? yes C(5) C(6) C(7) 123.8(7) ? ? ? yes C(6) C(7) C(8) 120.6(8) ? ? ? yes C(7) C(8) C(9) 120.7(8) ? ? ? yes C(8) C(9) C(10) 117.7(7) ? ? ? yes N(2) C(10) C(9) 121.3(7) ? ? ? yes Se(1) C(11) C(12) 115.3(6) ? ? ? yes Se(1) C(11) C(16) 122.5(6) ? ? ? yes C(12) C(11) C(16) 122.2(8) ? ? ? yes C(11) C(12) C(13) 117.4(9) ? ? ? yes C(12) C(13) C(14) 120.8(9) ? ? ? yes C(13) C(14) C(15) 120.6(8) ? ? ? yes C(14) C(15) C(16) 119.4(9) ? ? ? yes C(11) C(16) C(15) 119.6(8) ? ? ? yes