data_global data_C2C2ImT #TrackingRef 'WLU Hg extraction combined cif 04-10-13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 N2 O0 S' _chemical_formula_weight 156.25 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' S S 0.1246 0.1234 '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 6.495(2) _cell_length_b 14.431(5) _cell_length_c 8.949(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.467(3) _cell_angle_gamma 90.00 _cell_volume 837.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6718 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 32.75 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method none _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6416 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details 'Bruker AXScale' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21407 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 33.36 _reflns_number_total 3228 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0392P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3228 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.358 _refine_ls_restrained_S_all 1.358 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.74865(4) 0.921430(17) 0.82770(3) 0.02889(8) Uani 1 1 d . . . N3 N 0.52916(13) 0.78308(5) 0.67989(8) 0.02493(16) Uani 1 1 d . . . N1 N 0.35395(12) 0.90878(5) 0.70824(8) 0.02267(15) Uani 1 1 d . . . C2 C 0.54271(13) 0.87024(6) 0.73807(9) 0.02172(16) Uani 1 1 d . . . C7 C 0.3456(2) 1.07304(8) 0.63453(14) 0.0400(3) Uani 1 1 d . . . H7A H 0.309(3) 1.1358(13) 0.6714(17) 0.060 Uiso 1 1 d . . . H7B H 0.270(3) 1.0619(11) 0.538(2) 0.060 Uiso 1 1 d . . . H7C H 0.493(3) 1.0756(11) 0.620(2) 0.060 Uiso 1 1 d . . . C6 C 0.29598(15) 1.00236(6) 0.75121(11) 0.02697(19) Uani 1 1 d . . . H6A H 0.369(2) 1.0154(9) 0.8449(14) 0.032 Uiso 1 1 d . . . H6B H 0.149(2) 0.9999(9) 0.7652(14) 0.032 Uiso 1 1 d . . . C4 C 0.33395(16) 0.76862(7) 0.61336(11) 0.02935(19) Uani 1 1 d . . . H4A H 0.299(2) 0.7111(9) 0.5624(15) 0.035 Uiso 1 1 d . . . C8 C 0.69315(19) 0.71342(7) 0.69087(11) 0.0321(2) Uani 1 1 d . . . H8A H 0.638(2) 0.6583(9) 0.7421(15) 0.038 Uiso 1 1 d . . . H8B H 0.803(2) 0.7381(10) 0.7502(16) 0.038 Uiso 1 1 d . . . C5 C 0.22559(15) 0.84680(7) 0.63117(11) 0.02855(19) Uani 1 1 d . . . H5A H 0.085(2) 0.8615(9) 0.6066(14) 0.034 Uiso 1 1 d . . . C9 C 0.76572(19) 0.68637(8) 0.54045(12) 0.0349(2) Uani 1 1 d . . . H9A H 0.870(2) 0.6377(11) 0.5504(16) 0.052 Uiso 1 1 d . . . H9B H 0.827(2) 0.7403(11) 0.4929(18) 0.052 Uiso 1 1 d . . . H9C H 0.650(3) 0.6616(10) 0.4794(18) 0.052 Uiso 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 S 0.02481(13) 0.03163(14) 0.02986(13) 0.00002(8) -0.00148(8) -0.00147(9) N3 0.0302(4) 0.0224(3) 0.0225(3) -0.0011(3) 0.0038(3) 0.0035(3) N1 0.0225(3) 0.0227(3) 0.0230(3) -0.0010(2) 0.0034(3) 0.0005(3) C2 0.0242(4) 0.0225(4) 0.0189(3) 0.0015(3) 0.0047(3) 0.0006(3) C7 0.0568(8) 0.0268(5) 0.0374(5) 0.0045(4) 0.0102(5) 0.0077(5) C6 0.0281(4) 0.0248(4) 0.0286(4) -0.0023(3) 0.0064(3) 0.0046(3) C4 0.0332(5) 0.0275(4) 0.0274(4) -0.0045(3) 0.0022(3) -0.0040(4) C8 0.0427(6) 0.0269(4) 0.0267(4) 0.0020(3) 0.0035(4) 0.0123(4) C5 0.0252(4) 0.0317(5) 0.0288(4) -0.0034(3) 0.0014(3) -0.0029(4) C9 0.0376(6) 0.0367(5) 0.0303(4) -0.0055(4) 0.0030(4) 0.0114(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 S C2 1.6878(10) . ? N3 C2 1.3621(12) . ? N3 C4 1.3836(14) . ? N3 C8 1.4636(13) . ? N1 C2 1.3580(12) . ? N1 C5 1.3788(12) . ? N1 C6 1.4597(12) . ? C7 C6 1.5084(15) . ? C4 C5 1.3443(15) . ? C8 C9 1.5045(15) . ? 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 C2 N3 C4 109.88(8) . . ? C2 N3 C8 125.35(9) . . ? C4 N3 C8 124.72(9) . . ? C2 N1 C5 110.13(8) . . ? C2 N1 C6 124.83(8) . . ? C5 N1 C6 125.03(8) . . ? N1 C2 N3 105.44(8) . . ? N1 C2 S 126.47(7) . . ? N3 C2 S 128.09(7) . . ? N1 C6 C7 111.96(8) . . ? C5 C4 N3 107.17(9) . . ? N3 C8 C9 112.60(8) . . ? C4 C5 N1 107.37(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.338 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.058 data_global #END data_Hg2Cl4(C2C2ImT)2 #TrackingRef 'WLU Hg extraction combined cif 04-10-13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Cl4 Hg2 N4 S2' _chemical_formula_weight 855.48 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' S S 0.1246 0.1234 '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' Hg Hg -2.3894 9.2266 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.258(5) _cell_length_b 9.365(5) _cell_length_c 14.749(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.015(8) _cell_angle_gamma 90.00 _cell_volume 1245.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3045 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.84 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.280 _exptl_crystal_density_method none _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 12.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2533 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'Bruker AXScale' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6212 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2182 _reflns_number_gt 1758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1018P)^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 0.0129(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2182 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 Hg1 Hg 0.42238(4) -0.02969(5) 0.87017(3) 0.0544(3) Uani 1 1 d . . . Cl1 Cl 0.3591(3) 0.1405(3) 1.00752(18) 0.0527(7) Uani 1 1 d . . . Cl2 Cl 0.2108(3) -0.1813(3) 0.8450(2) 0.0637(8) Uani 1 1 d . . . S1 S 0.5299(3) 0.1216(3) 0.76990(19) 0.0526(7) Uani 1 1 d . . . N1 N 0.7682(9) 0.2313(9) 0.8955(5) 0.0438(19) Uani 1 1 d . . . N2 N 0.8202(10) 0.0386(8) 0.8314(7) 0.045(2) Uani 1 1 d . . . C1 C 0.7092(9) 0.1289(10) 0.8356(7) 0.040(2) Uani 1 1 d . . . C2 C 0.9167(11) 0.2023(12) 0.9307(7) 0.054(3) Uani 1 1 d . . . H2 H 0.9844 0.2578 0.9748 0.065 Uiso 1 1 calc R . . C3 C 0.9466(11) 0.0810(15) 0.8906(8) 0.052(3) Uani 1 1 d . . . H3 H 1.0396 0.0335 0.9017 0.063 Uiso 1 1 calc R . . C4 C 0.8015(14) -0.0965(17) 0.7771(11) 0.085(4) Uani 1 1 d . . . H4A H 0.8756 -0.1670 0.8088 0.102 Uiso 1 1 calc R . . H4B H 0.7017 -0.1361 0.7751 0.102 Uiso 1 1 calc R . . C5 C 0.818(2) -0.076(2) 0.6876(15) 0.112(6) Uani 1 1 d . . . H5A H 0.7566 0.0046 0.6594 0.168 Uiso 1 1 calc R . . H5B H 0.7878 -0.1624 0.6509 0.168 Uiso 1 1 calc R . . H5C H 0.9225 -0.0552 0.6888 0.168 Uiso 1 1 calc R . . C6 C 0.6837(15) 0.3570(15) 0.9230(10) 0.077(4) Uani 1 1 d . . . H6A H 0.5856 0.3645 0.8794 0.092 Uiso 1 1 calc R . . H6B H 0.6673 0.3413 0.9863 0.092 Uiso 1 1 calc R . . C7 C 0.768(3) 0.4924(16) 0.9212(16) 0.109(7) Uani 1 1 d . . . H7A H 0.8395 0.5045 0.9806 0.163 Uiso 1 1 calc R . . H7B H 0.6986 0.5732 0.9112 0.163 Uiso 1 1 calc R . . H7C H 0.8203 0.4886 0.8705 0.163 Uiso 1 1 calc R . . 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 Hg1 0.0322(3) 0.0688(5) 0.0649(4) 0.0037(2) 0.0164(2) -0.00208(17) Cl1 0.0400(13) 0.0609(15) 0.0560(15) -0.0059(12) 0.0082(11) 0.0214(12) Cl2 0.0372(13) 0.0715(18) 0.087(2) -0.0286(15) 0.0233(13) -0.0085(13) S1 0.0321(13) 0.0723(17) 0.0521(15) 0.0133(13) 0.0067(11) 0.0018(12) N1 0.048(5) 0.045(5) 0.043(4) 0.006(4) 0.020(4) 0.008(4) N2 0.031(5) 0.046(5) 0.062(6) -0.006(4) 0.016(4) 0.000(3) C1 0.027(4) 0.042(5) 0.052(6) 0.005(4) 0.012(4) 0.000(4) C2 0.040(5) 0.071(7) 0.049(6) -0.003(5) 0.003(5) -0.003(5) C3 0.032(5) 0.065(7) 0.060(7) 0.001(6) 0.012(5) 0.007(5) C4 0.049(7) 0.097(10) 0.110(12) -0.041(10) 0.019(7) 0.002(7) C5 0.121(16) 0.104(12) 0.127(16) -0.036(13) 0.062(13) -0.017(12) C6 0.077(9) 0.079(9) 0.073(8) -0.013(7) 0.014(7) 0.029(8) C7 0.111(16) 0.067(9) 0.141(17) -0.056(10) 0.012(13) 0.008(9) _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 Hg1 Cl2 2.380(3) . ? Hg1 S1 2.418(3) . ? Hg1 Cl1 2.604(3) 3_657 ? Hg1 Cl1 2.743(3) . ? Cl1 Hg1 2.604(3) 3_657 ? S1 C1 1.725(9) . ? N1 C1 1.334(12) . ? N1 C2 1.383(12) . ? N1 C6 1.518(14) . ? N2 C1 1.343(12) . ? N2 C3 1.353(14) . ? N2 C4 1.486(17) . ? C2 C3 1.338(17) . ? C4 C5 1.38(2) . ? C6 C7 1.49(2) . ? 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 Cl2 Hg1 S1 133.79(10) . . ? Cl2 Hg1 Cl1 110.73(11) . 3_657 ? S1 Hg1 Cl1 107.13(9) . 3_657 ? Cl2 Hg1 Cl1 99.00(9) . . ? S1 Hg1 Cl1 107.28(11) . . ? Cl1 Hg1 Cl1 88.96(8) 3_657 . ? Hg1 Cl1 Hg1 91.04(8) 3_657 . ? C1 S1 Hg1 99.0(3) . . ? C1 N1 C2 109.4(8) . . ? C1 N1 C6 125.1(9) . . ? C2 N1 C6 125.5(9) . . ? C1 N2 C3 110.2(9) . . ? C1 N2 C4 124.3(9) . . ? C3 N2 C4 125.2(9) . . ? N1 C1 N2 106.2(8) . . ? N1 C1 S1 126.9(7) . . ? N2 C1 S1 126.7(8) . . ? C3 C2 N1 106.7(9) . . ? C2 C3 N2 107.4(9) . . ? C5 C4 N2 111.9(15) . . ? C7 C6 N1 110.6(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.086 _refine_diff_density_min -3.740 _refine_diff_density_rms 0.258 data_global #END data_HgCl2(C2C2ImT)2 #TrackingRef 'WLU Hg extraction combined cif 04-10-13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H24 Cl2 Hg N4 O0 S2' _chemical_formula_weight 583.98 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' S S 0.1246 0.1234 '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' Hg Hg -2.3894 9.2266 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9363(6) _cell_length_b 11.8914(6) _cell_length_c 13.1361(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.657(2) _cell_angle_gamma 90.00 _cell_volume 2018.56(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9812 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 32.91 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method none _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 8.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4248 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details 'Bruker AXScale' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48754 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 33.08 _reflns_number_total 7616 _reflns_number_gt 6704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+2.6396P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7616 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _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 Hg Hg 0.239853(8) 0.511644(8) 0.751564(7) 0.01938(4) Uani 1 1 d . . . Cl1 Cl 0.13715(6) 0.33688(6) 0.76494(6) 0.03072(15) Uani 1 1 d . . . Cl2 Cl 0.30487(6) 0.50908(6) 0.57151(5) 0.02470(13) Uani 1 1 d . . . S1A S 0.13759(5) 0.69206(5) 0.74791(5) 0.01875(11) Uani 1 1 d . . . S1B S 0.38959(5) 0.51422(5) 0.87999(6) 0.02127(12) Uani 1 1 d . . . N1A N -0.02246(16) 0.61024(18) 0.62500(16) 0.0165(4) Uani 1 1 d . . . N1B N 0.38040(17) 0.28992(18) 0.93061(17) 0.0186(4) Uani 1 1 d . . . N3A N 0.08459(17) 0.71407(19) 0.54432(16) 0.0180(4) Uani 1 1 d . . . N3B N 0.5043(2) 0.3291(2) 0.8309(2) 0.0266(5) Uani 1 1 d . . . C2A C 0.06540(18) 0.6704(2) 0.63628(18) 0.0153(4) Uani 1 1 d . . . C2B C 0.42405(19) 0.3744(2) 0.8791(2) 0.0184(4) Uani 1 1 d . . . C4A C 0.0068(2) 0.6824(2) 0.4746(2) 0.0200(5) Uani 1 1 d . . . H4AA H 0.0011 0.7025 0.4046 0.024 Uiso 1 1 calc R . . C4B C 0.5111(3) 0.2154(3) 0.8525(3) 0.0308(6) Uani 1 1 d . . . H4BA H 0.5608 0.1643 0.8284 0.037 Uiso 1 1 calc R . . C5A C -0.0600(2) 0.6170(2) 0.52494(19) 0.0190(4) Uani 1 1 d . . . H5AA H -0.1210 0.5824 0.4967 0.023 Uiso 1 1 calc R . . C5B C 0.4337(2) 0.1911(2) 0.9141(2) 0.0245(5) Uani 1 1 d . . . H5BA H 0.4185 0.1192 0.9413 0.029 Uiso 1 1 calc R . . C6B C 0.2920(2) 0.2992(2) 0.9949(2) 0.0238(5) Uani 1 1 d . . . H6BA H 0.2563 0.2257 0.9968 0.029 Uiso 1 1 calc R . . H6BB H 0.2426 0.3548 0.9646 0.029 Uiso 1 1 calc R . . C6A C -0.0691(2) 0.5496(2) 0.7088(2) 0.0220(5) Uani 1 1 d . . . H6AA H -0.0668 0.5979 0.7702 0.026 Uiso 1 1 calc R . . H6AB H -0.0279 0.4812 0.7249 0.026 Uiso 1 1 calc R . . C7A C -0.1796(3) 0.5161(3) 0.6831(3) 0.0309(6) Uani 1 1 d . . . H7AA H -0.2077 0.4771 0.7414 0.046 Uiso 1 1 calc R . . H7AB H -0.1820 0.4660 0.6239 0.046 Uiso 1 1 calc R . . H7AC H -0.2209 0.5836 0.6674 0.046 Uiso 1 1 calc R . . C7B C 0.3230(3) 0.3346(4) 1.1020(3) 0.0432(9) Uani 1 1 d . . . H7BA H 0.2612 0.3399 1.1422 0.065 Uiso 1 1 calc R . . H7BB H 0.3572 0.4081 1.1007 0.065 Uiso 1 1 calc R . . H7BC H 0.3707 0.2789 1.1329 0.065 Uiso 1 1 calc R . . C8A C 0.1693(2) 0.7904(3) 0.5233(2) 0.0260(6) Uani 1 1 d . . . H8AA H 0.1958 0.7726 0.4557 0.031 Uiso 1 1 calc R . . H8AB H 0.2265 0.7793 0.5750 0.031 Uiso 1 1 calc R . . C8B C 0.5766(3) 0.3886(3) 0.7667(3) 0.0429(9) Uani 1 1 d . . . H8BA H 0.5623 0.4703 0.7697 0.051 Uiso 1 1 calc R . . H8BB H 0.6481 0.3762 0.7947 0.051 Uiso 1 1 calc R . . C9A C 0.1347(3) 0.9106(3) 0.5248(3) 0.0431(9) Uani 1 1 d . . . H9AA H 0.1931 0.9598 0.5106 0.065 Uiso 1 1 calc R . . H9AB H 0.1095 0.9287 0.5921 0.065 Uiso 1 1 calc R . . H9AC H 0.0789 0.9220 0.4728 0.065 Uiso 1 1 calc R . . C9B C 0.5700(4) 0.3526(4) 0.6612(3) 0.0566(13) Uani 1 1 d . . . H9BA H 0.6213 0.3934 0.6229 0.085 Uiso 1 1 calc R . . H9BB H 0.5005 0.3685 0.6317 0.085 Uiso 1 1 calc R . . H9BC H 0.5836 0.2717 0.6575 0.085 Uiso 1 1 calc R . . 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 Hg 0.02002(5) 0.02008(5) 0.01776(5) 0.00277(3) -0.00203(3) -0.00053(3) Cl1 0.0312(4) 0.0245(3) 0.0354(4) 0.0084(3) -0.0096(3) -0.0099(2) Cl2 0.0265(3) 0.0288(3) 0.0192(3) -0.0055(2) 0.0052(2) -0.0044(2) S1A 0.0225(3) 0.0203(3) 0.0131(3) -0.0028(2) -0.0032(2) 0.0028(2) S1B 0.0216(3) 0.0163(3) 0.0252(3) 0.0006(2) -0.0069(2) -0.0013(2) N1A 0.0166(9) 0.0195(9) 0.0135(9) 0.0012(7) 0.0006(7) 0.0013(7) N1B 0.0193(10) 0.0194(10) 0.0170(10) 0.0030(7) 0.0010(8) 0.0020(7) N3A 0.0180(10) 0.0227(10) 0.0131(9) 0.0014(7) -0.0010(7) -0.0015(7) N3B 0.0273(12) 0.0253(12) 0.0282(12) -0.0005(9) 0.0112(10) -0.0006(9) C2A 0.0157(10) 0.0170(10) 0.0132(10) -0.0004(7) -0.0006(8) 0.0026(7) C2B 0.0165(11) 0.0199(11) 0.0185(11) 0.0013(8) -0.0016(8) -0.0004(8) C4A 0.0222(12) 0.0245(12) 0.0131(10) 0.0003(9) -0.0026(9) 0.0007(9) C4B 0.0307(15) 0.0270(14) 0.0356(17) -0.0010(11) 0.0095(12) 0.0079(11) C5A 0.0180(11) 0.0227(12) 0.0161(11) -0.0008(8) -0.0028(8) 0.0001(8) C5B 0.0315(14) 0.0196(12) 0.0225(13) 0.0032(9) 0.0019(11) 0.0063(10) C6B 0.0216(12) 0.0256(13) 0.0248(13) 0.0009(10) 0.0064(10) -0.0004(9) C6A 0.0216(12) 0.0258(12) 0.0189(12) 0.0056(9) 0.0037(9) 0.0001(9) C7A 0.0234(14) 0.0437(17) 0.0257(15) 0.0045(12) 0.0031(11) -0.0089(11) C7B 0.0372(19) 0.070(3) 0.0226(15) -0.0053(15) 0.0060(13) 0.0075(17) C8A 0.0245(13) 0.0358(15) 0.0178(12) 0.0043(10) 0.0003(10) -0.0111(11) C8B 0.042(2) 0.045(2) 0.044(2) -0.0032(16) 0.0221(16) -0.0134(15) C9A 0.067(3) 0.0275(16) 0.0362(18) -0.0018(13) 0.0158(17) -0.0168(16) C9B 0.077(3) 0.068(3) 0.0260(17) -0.0036(17) 0.0154(18) -0.041(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 Hg Cl1 2.4772(7) . ? Hg S1B 2.5092(7) . ? Hg S1A 2.5198(6) . ? Hg Cl2 2.5470(7) . ? S1A C2A 1.721(2) . ? S1B C2B 1.722(3) . ? N1A C2A 1.345(3) . ? N1A C5A 1.382(3) . ? N1A C6A 1.469(3) . ? N1B C2B 1.349(3) . ? N1B C5B 1.385(3) . ? N1B C6B 1.457(3) . ? N3A C2A 1.348(3) . ? N3A C4A 1.381(3) . ? N3A C8A 1.459(3) . ? N3B C2B 1.353(3) . ? N3B C4B 1.383(4) . ? N3B C8B 1.469(4) . ? C4A C5A 1.357(4) . ? C4B C5B 1.348(4) . ? C6B C7B 1.505(5) . ? C6A C7A 1.506(4) . ? C8A C9A 1.499(5) . ? C8B C9B 1.450(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 Cl1 Hg S1B 111.25(2) . . ? Cl1 Hg S1A 115.65(3) . . ? S1B Hg S1A 112.99(2) . . ? Cl1 Hg Cl2 104.90(3) . . ? S1B Hg Cl2 110.28(3) . . ? S1A Hg Cl2 100.85(2) . . ? C2A S1A Hg 98.77(8) . . ? C2B S1B Hg 100.12(9) . . ? C2A N1A C5A 109.4(2) . . ? C2A N1A C6A 123.6(2) . . ? C5A N1A C6A 127.0(2) . . ? C2B N1B C5B 109.3(2) . . ? C2B N1B C6B 126.3(2) . . ? C5B N1B C6B 124.4(2) . . ? C2A N3A C4A 109.3(2) . . ? C2A N3A C8A 125.5(2) . . ? C4A N3A C8A 125.1(2) . . ? C2B N3B C4B 109.6(2) . . ? C2B N3B C8B 126.9(3) . . ? C4B N3B C8B 123.5(3) . . ? N1A C2A N3A 107.2(2) . . ? N1A C2A S1A 126.57(19) . . ? N3A C2A S1A 126.19(19) . . ? N1B C2B N3B 106.6(2) . . ? N1B C2B S1B 126.9(2) . . ? N3B C2B S1B 126.3(2) . . ? C5A C4A N3A 107.1(2) . . ? C5B C4B N3B 106.9(3) . . ? C4A C5A N1A 107.0(2) . . ? C4B C5B N1B 107.5(3) . . ? N1B C6B C7B 112.4(3) . . ? N1A C6A C7A 112.4(2) . . ? N3A C8A C9A 111.3(3) . . ? C9B C8B N3B 113.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.669 _refine_diff_density_min -1.615 _refine_diff_density_rms 0.166 data_global #END data_Hg(NTf2)2(C2C2ImT)2 #TrackingRef 'WLU Hg extraction combined cif 04-10-13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 F12 Hg N6 O8 S6' _chemical_formula_weight 1073.38 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 8.4298(5) _cell_length_b 17.8332(10) _cell_length_c 11.8196(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.958(2) _cell_angle_gamma 90.00 _cell_volume 1750.08(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8205 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.49 _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method none _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 4.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4959 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'Bruker AXScale' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27092 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4028 _reflns_number_gt 3307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+1.0601P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4028 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.5000 0.0000 0.5000 0.01712(5) Uani 1 2 d S . . S1 S 0.67293(8) 0.09561(4) 0.58436(6) 0.02013(14) Uani 1 1 d . . . S2 S 0.29978(7) -0.04980(4) 0.78209(6) 0.01890(14) Uani 1 1 d . . . S3 S 0.51393(8) -0.16423(4) 0.74583(6) 0.02201(15) Uani 1 1 d . . . F1 F 0.7858(2) -0.22727(10) 0.82429(17) 0.0351(4) Uani 1 1 d . . . F2 F 0.6133(2) -0.23650(10) 0.93862(16) 0.0334(4) Uani 1 1 d . . . F3 F 0.7343(2) -0.13216(11) 0.92389(17) 0.0364(4) Uani 1 1 d . . . F4 F 0.0303(2) -0.12356(13) 0.7789(2) 0.0502(6) Uani 1 1 d . . . F5 F 0.1247(2) -0.12812(12) 0.62176(19) 0.0447(5) Uani 1 1 d . . . F6 F 0.0106(2) -0.02768(12) 0.66921(19) 0.0434(5) Uani 1 1 d . . . O1 O 0.3548(2) -0.00509(11) 0.69604(17) 0.0248(4) Uani 1 1 d . . . O2 O 0.2665(3) -0.01411(12) 0.88308(19) 0.0319(5) Uani 1 1 d . . . O3 O 0.5958(2) -0.11673(13) 0.67710(19) 0.0309(5) Uani 1 1 d . . . O4 O 0.4489(3) -0.23308(14) 0.6983(2) 0.0436(6) Uani 1 1 d . . . N1 N 0.6280(2) 0.09928(13) 0.80824(19) 0.0181(5) Uani 1 1 d . . . N1A N 0.3959(3) -0.12359(15) 0.8164(2) 0.0259(6) Uani 1 1 d . . . N3 N 0.4526(3) 0.16582(13) 0.6963(2) 0.0188(5) Uani 1 1 d . . . C1A C 0.6701(3) -0.19132(16) 0.8658(3) 0.0228(6) Uani 1 1 d . . . C2 C 0.5792(3) 0.11974(15) 0.6989(2) 0.0176(5) Uani 1 1 d . . . C2A C 0.1046(3) -0.08421(19) 0.7092(3) 0.0285(7) Uani 1 1 d . . . C4 C 0.4217(3) 0.17381(16) 0.8060(3) 0.0234(6) Uani 1 1 d . . . H4A H 0.3380 0.2030 0.8284 0.028 Uiso 1 1 calc R . . C5 C 0.5311(3) 0.13290(16) 0.8760(3) 0.0231(6) Uani 1 1 d . . . H5A H 0.5400 0.1281 0.9569 0.028 Uiso 1 1 calc R . . C6 C 0.7651(3) 0.04957(16) 0.8508(2) 0.0227(6) Uani 1 1 d . . . H6A H 0.7828 0.0150 0.7886 0.027 Uiso 1 1 calc R . . H6B H 0.7395 0.0190 0.9151 0.027 Uiso 1 1 calc R . . C7 C 0.9169(4) 0.0939(2) 0.8911(3) 0.0376(8) Uani 1 1 d . . . H7A H 1.0055 0.0594 0.9190 0.056 Uiso 1 1 calc R . . H7B H 0.9000 0.1276 0.9534 0.056 Uiso 1 1 calc R . . H7C H 0.9436 0.1234 0.8271 0.056 Uiso 1 1 calc R . . C8 C 0.3603(3) 0.20128(17) 0.5936(3) 0.0255(6) Uani 1 1 d . . . H8A H 0.4281 0.2041 0.5331 0.031 Uiso 1 1 calc R . . H8B H 0.3322 0.2531 0.6125 0.031 Uiso 1 1 calc R . . C9 C 0.2069(3) 0.15835(19) 0.5476(3) 0.0317(7) Uani 1 1 d . . . H9A H 0.1479 0.1843 0.4801 0.048 Uiso 1 1 calc R . . H9B H 0.1393 0.1555 0.6072 0.048 Uiso 1 1 calc R . . H9C H 0.2344 0.1076 0.5260 0.048 Uiso 1 1 calc R . . 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 Hg 0.02110(7) 0.01486(7) 0.01548(7) -0.00269(7) 0.00336(5) -0.00047(6) S1 0.0230(3) 0.0194(3) 0.0188(3) -0.0028(3) 0.0058(3) -0.0046(3) S2 0.0181(3) 0.0201(3) 0.0188(3) 0.0013(3) 0.0041(2) 0.0013(2) S3 0.0199(3) 0.0237(4) 0.0219(4) -0.0015(3) 0.0023(3) 0.0036(3) F1 0.0268(8) 0.0314(10) 0.0504(12) 0.0124(9) 0.0163(8) 0.0144(7) F2 0.0329(9) 0.0305(10) 0.0394(11) 0.0169(8) 0.0130(8) 0.0075(8) F3 0.0337(9) 0.0312(11) 0.0386(11) -0.0018(8) -0.0101(8) -0.0029(8) F4 0.0259(9) 0.0553(14) 0.0719(16) 0.0192(12) 0.0157(10) -0.0096(9) F5 0.0284(9) 0.0517(13) 0.0503(13) -0.0215(10) -0.0030(9) -0.0041(9) F6 0.0274(9) 0.0497(12) 0.0494(13) 0.0105(10) -0.0040(8) 0.0165(8) O1 0.0289(9) 0.0190(10) 0.0292(11) 0.0032(9) 0.0124(8) -0.0013(9) O2 0.0371(11) 0.0364(14) 0.0239(11) -0.0038(9) 0.0103(9) 0.0080(9) O3 0.0311(11) 0.0386(13) 0.0251(12) 0.0087(10) 0.0112(9) 0.0128(9) O4 0.0367(12) 0.0381(14) 0.0523(16) -0.0204(12) -0.0022(11) -0.0038(10) N1 0.0205(10) 0.0159(12) 0.0177(12) -0.0029(9) 0.0033(9) -0.0003(9) N1A 0.0227(11) 0.0297(14) 0.0264(14) 0.0090(11) 0.0072(10) 0.0102(10) N3 0.0212(10) 0.0161(12) 0.0179(12) -0.0013(9) -0.0001(9) 0.0004(9) C1A 0.0195(12) 0.0191(15) 0.0303(16) 0.0048(12) 0.0059(11) 0.0057(10) C2 0.0188(12) 0.0147(13) 0.0187(14) -0.0021(11) 0.0021(10) -0.0035(10) C2A 0.0177(12) 0.0344(18) 0.0329(17) 0.0031(14) 0.0033(12) 0.0023(12) C4 0.0243(13) 0.0214(15) 0.0249(15) -0.0059(12) 0.0054(11) -0.0007(11) C5 0.0278(14) 0.0222(15) 0.0203(15) -0.0043(12) 0.0074(11) -0.0003(11) C6 0.0269(13) 0.0192(14) 0.0210(15) 0.0006(11) 0.0012(11) 0.0073(11) C7 0.0243(14) 0.0351(19) 0.049(2) -0.0010(16) -0.0071(14) 0.0045(13) C8 0.0261(13) 0.0228(15) 0.0247(16) -0.0002(12) -0.0038(11) 0.0034(11) C9 0.0231(13) 0.0338(18) 0.0340(18) -0.0049(14) -0.0071(12) 0.0023(13) _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 Hg S1 2.3503(7) 3_656 ? Hg S1 2.3503(7) . ? S1 C2 1.736(3) . ? S2 O2 1.423(2) . ? S2 O1 1.431(2) . ? S2 N1A 1.561(2) . ? S2 C2A 1.826(3) . ? S3 O4 1.420(2) . ? S3 O3 1.431(2) . ? S3 N1A 1.581(2) . ? S3 C1A 1.825(3) . ? F1 C1A 1.330(3) . ? F2 C1A 1.327(3) . ? F3 C1A 1.322(3) . ? F4 C2A 1.320(4) . ? F5 C2A 1.330(4) . ? F6 C2A 1.318(4) . ? N1 C2 1.337(4) . ? N1 C5 1.376(3) . ? N1 C6 1.474(3) . ? N3 C2 1.343(3) . ? N3 C4 1.374(4) . ? N3 C8 1.467(4) . ? C4 C5 1.343(4) . ? C6 C7 1.509(4) . ? C8 C9 1.520(4) . ? 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 S1 Hg S1 180.00(2) 3_656 . ? C2 S1 Hg 100.27(9) . . ? O2 S2 O1 118.82(13) . . ? O2 S2 N1A 109.15(14) . . ? O1 S2 N1A 115.90(12) . . ? O2 S2 C2A 104.71(14) . . ? O1 S2 C2A 103.16(13) . . ? N1A S2 C2A 102.94(14) . . ? O4 S3 O3 118.58(16) . . ? O4 S3 N1A 111.72(14) . . ? O3 S3 N1A 115.94(13) . . ? O4 S3 C1A 104.80(15) . . ? O3 S3 C1A 104.14(13) . . ? N1A S3 C1A 98.43(13) . . ? C2 N1 C5 109.2(2) . . ? C2 N1 C6 125.8(2) . . ? C5 N1 C6 124.9(2) . . ? S2 N1A S3 126.53(16) . . ? C2 N3 C4 108.7(2) . . ? C2 N3 C8 126.1(2) . . ? C4 N3 C8 125.2(2) . . ? F3 C1A F2 108.0(2) . . ? F3 C1A F1 108.4(2) . . ? F2 C1A F1 108.5(2) . . ? F3 C1A S3 111.56(19) . . ? F2 C1A S3 111.84(19) . . ? F1 C1A S3 108.5(2) . . ? N1 C2 N3 107.4(2) . . ? N1 C2 S1 125.5(2) . . ? N3 C2 S1 126.9(2) . . ? F6 C2A F4 108.0(2) . . ? F6 C2A F5 108.8(3) . . ? F4 C2A F5 108.1(3) . . ? F6 C2A S2 110.4(2) . . ? F4 C2A S2 111.7(2) . . ? F5 C2A S2 109.83(18) . . ? C5 C4 N3 107.6(2) . . ? C4 C5 N1 107.0(3) . . ? N1 C6 C7 111.4(2) . . ? N3 C8 C9 112.0(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.106 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.090 #END