# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound-1-KW3-9B _database_code_depnum_ccdc_archive 'CCDC 909671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Hg Sb2 Se5, C9 H30 N6 Ni' _chemical_formula_sum 'C9 H30 Hg N6 Ni Sb2 Se5' _chemical_formula_weight 1119.99 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2626(6) _cell_length_b 11.5370(6) _cell_length_c 12.1698(5) _cell_angle_alpha 105.999(4) _cell_angle_beta 97.174(4) _cell_angle_gamma 118.831(5) _cell_volume 1267.70(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2976 _cell_measurement_theta_min 2.2382 _cell_measurement_theta_max 29.0525 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 16.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63029 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis CCD; Oxford, 2006' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10641 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5231 _reflns_number_gt 4047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0171P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5231 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Hg1 Hg 0.69279(3) -0.06806(4) -0.14564(3) 0.03485(10) Uani 1 1 d . . . Sb1 Sb 0.67600(5) 0.13570(5) 0.15891(4) 0.02480(12) Uani 1 1 d . . . Sb2 Sb 0.95836(5) 0.06274(5) 0.14633(4) 0.02804(13) Uani 1 1 d . . . Se1 Se 0.52005(7) 0.10205(8) 0.30057(6) 0.02752(18) Uani 1 1 d . . . Se2 Se 0.58131(8) -0.12499(8) 0.03450(6) 0.02888(18) Uani 1 1 d . . . Se3 Se 0.89225(8) 0.18399(9) 0.31871(7) 0.0344(2) Uani 1 1 d . . . Se4 Se 1.22300(8) 0.22575(8) 0.26111(7) 0.03087(19) Uani 1 1 d . . . Se5 Se 0.92858(7) 0.18489(8) 0.00532(7) 0.03201(19) Uani 1 1 d . . . Ni1 Ni 0.67928(10) 0.35150(10) 0.72930(8) 0.0307(2) Uani 1 1 d . . . N1 N 0.6905(6) 0.1853(6) 0.6130(5) 0.0382(17) Uani 1 1 d . . . H1C H 0.6470 0.1069 0.6307 0.046 Uiso 1 1 calc R . . H1D H 0.6453 0.1620 0.5365 0.046 Uiso 1 1 calc R . . N2 N 0.8965(7) 0.4747(7) 0.7322(5) 0.0476(19) Uani 1 1 d . . . H2B H 0.9145 0.5544 0.7202 0.057 Uiso 1 1 calc R . . H2C H 0.9558 0.5011 0.8038 0.057 Uiso 1 1 calc R . . N3 N 0.6069(7) 0.3984(7) 0.5892(5) 0.0453(19) Uani 1 1 d . . . H3D H 0.6605 0.4932 0.6063 0.054 Uiso 1 1 calc R . . H3E H 0.6137 0.3517 0.5201 0.054 Uiso 1 1 calc R . . N4 N 0.4545(6) 0.2137(7) 0.6963(5) 0.0381(17) Uani 1 1 d . . . H4C H 0.4321 0.1247 0.6872 0.046 Uiso 1 1 calc R . . H4D H 0.4292 0.2471 0.7590 0.046 Uiso 1 1 calc R . . N5 N 0.7275(6) 0.3051(6) 0.8808(5) 0.0280(14) Uani 1 1 d . . . H5B H 0.6504 0.2256 0.8787 0.034 Uiso 1 1 calc R . . H5C H 0.7981 0.2890 0.8789 0.034 Uiso 1 1 calc R . . N6 N 0.6966(6) 0.5236(6) 0.8666(5) 0.0316(15) Uani 1 1 d . . . H6D H 0.7819 0.6043 0.8847 0.038 Uiso 1 1 calc R . . H6E H 0.6285 0.5383 0.8409 0.038 Uiso 1 1 calc R . . C1 C 0.8419(9) 0.2326(9) 0.6263(8) 0.055(3) Uani 1 1 d . . . H1A H 0.8829 0.2268 0.6980 0.065 Uiso 1 1 calc R . . H1B H 0.8488 0.1722 0.5573 0.065 Uiso 1 1 calc R . . C2 C 0.9181(9) 0.3836(10) 0.6352(8) 0.057(3) Uani 1 1 d . . . H2A H 0.8752 0.3826 0.5596 0.069 Uiso 1 1 calc R . . C3 C 1.0797(10) 0.4443(11) 0.6468(8) 0.075(3) Uani 1 1 d . . . H3A H 1.1226 0.5356 0.6396 0.112 Uiso 1 1 calc R . . H3B H 1.0874 0.3787 0.5843 0.112 Uiso 1 1 calc R . . H3C H 1.1278 0.4556 0.7236 0.112 Uiso 1 1 calc R . . C4 C 0.4568(9) 0.3524(9) 0.5766(7) 0.053(3) Uani 1 1 d . . . H4A H 0.4130 0.3463 0.4996 0.063 Uiso 1 1 calc R . . H4B H 0.4527 0.4224 0.6393 0.063 Uiso 1 1 calc R . . C5 C 0.3775(9) 0.2097(9) 0.5854(7) 0.052(2) Uani 1 1 d . . . H5A H 0.3772 0.1406 0.5170 0.062 Uiso 1 1 calc R . . C6 C 0.2210(9) 0.1580(10) 0.5758(8) 0.064(3) Uani 1 1 d . . . H6A H 0.1759 0.1555 0.5020 0.096 Uiso 1 1 calc R . . H6B H 0.2172 0.2228 0.6423 0.096 Uiso 1 1 calc R . . H6C H 0.1723 0.0637 0.5771 0.096 Uiso 1 1 calc R . . C7 C 0.7716(8) 0.4272(8) 0.9918(6) 0.0321(19) Uani 1 1 d . . . H7A H 0.8715 0.5001 1.0111 0.039 Uiso 1 1 calc R . . H7B H 0.7589 0.3956 1.0580 0.039 Uiso 1 1 calc R . . C8 C 0.6812(8) 0.4900(8) 0.9741(6) 0.0311(18) Uani 1 1 d . . . H8A H 0.5813 0.4157 0.9579 0.037 Uiso 1 1 calc R . . C9 C 0.7243(9) 0.6184(9) 1.0872(7) 0.048(2) Uani 1 1 d . . . H9A H 0.7082 0.5879 1.1527 0.072 Uiso 1 1 calc R . . H9B H 0.6683 0.6576 1.0730 0.072 Uiso 1 1 calc R . . H9C H 0.8233 0.6904 1.1068 0.072 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 0.02790(16) 0.0421(2) 0.03056(18) 0.00733(15) 0.00606(14) 0.02036(16) Sb1 0.0238(3) 0.0255(3) 0.0273(3) 0.0116(2) 0.0089(2) 0.0139(2) Sb2 0.0253(3) 0.0250(3) 0.0330(3) 0.0077(2) 0.0068(2) 0.0154(2) Se1 0.0267(4) 0.0362(5) 0.0225(4) 0.0117(3) 0.0083(3) 0.0187(4) Se2 0.0298(4) 0.0259(4) 0.0294(4) 0.0121(3) 0.0117(3) 0.0126(4) Se3 0.0344(4) 0.0487(5) 0.0253(4) 0.0126(4) 0.0090(4) 0.0271(4) Se4 0.0276(4) 0.0277(4) 0.0317(4) 0.0036(3) 0.0010(3) 0.0170(4) Se5 0.0253(4) 0.0300(4) 0.0285(4) 0.0093(3) 0.0032(3) 0.0086(4) Ni1 0.0408(6) 0.0230(5) 0.0234(5) 0.0092(4) 0.0056(5) 0.0147(5) N1 0.045(4) 0.027(4) 0.028(4) 0.006(3) 0.009(3) 0.011(3) N2 0.063(5) 0.032(4) 0.031(4) 0.007(3) 0.017(4) 0.016(4) N3 0.065(5) 0.033(4) 0.027(4) 0.011(3) 0.002(4) 0.022(4) N4 0.044(4) 0.035(4) 0.029(4) 0.014(3) 0.004(3) 0.018(3) N5 0.033(3) 0.022(3) 0.031(4) 0.012(3) 0.013(3) 0.014(3) N6 0.036(4) 0.030(4) 0.024(3) 0.011(3) 0.002(3) 0.015(3) C1 0.059(6) 0.032(5) 0.062(6) 0.007(5) 0.036(5) 0.019(5) C2 0.059(6) 0.050(6) 0.052(6) 0.009(5) 0.027(5) 0.025(5) C3 0.080(8) 0.075(8) 0.056(7) 0.010(6) 0.013(6) 0.041(7) C4 0.056(6) 0.045(6) 0.039(5) 0.019(4) -0.011(4) 0.019(5) C5 0.051(6) 0.042(6) 0.041(5) 0.014(4) -0.002(4) 0.015(5) C6 0.054(6) 0.066(7) 0.057(6) 0.026(5) -0.003(5) 0.026(6) C7 0.031(4) 0.033(5) 0.029(4) 0.015(4) 0.008(4) 0.013(4) C8 0.043(5) 0.027(4) 0.026(4) 0.013(3) 0.016(4) 0.018(4) C9 0.061(6) 0.049(6) 0.039(5) 0.015(4) 0.020(5) 0.033(5) _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 Se4 2.6023(8) 2_755 ? Hg1 Se1 2.6481(8) 2_655 ? Hg1 Se5 2.7010(8) . ? Hg1 Se2 2.7385(7) . ? Sb1 Se2 2.5432(9) . ? Sb1 Se1 2.5837(8) . ? Sb1 Se3 2.6335(9) . ? Sb2 Se4 2.5450(9) . ? Sb2 Se5 2.5863(10) . ? Sb2 Se3 2.5863(9) . ? Se1 Hg1 2.6481(8) 2_655 ? Se4 Hg1 2.6023(8) 2_755 ? Ni1 N3 2.110(6) . ? Ni1 N1 2.116(6) . ? Ni1 N6 2.118(6) . ? Ni1 N5 2.135(6) . ? Ni1 N2 2.146(6) . ? Ni1 N4 2.147(6) . ? N1 C1 1.489(9) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.480(9) . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 C4 1.479(10) . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 C5 1.487(9) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 C7 1.472(8) . ? N5 H5B 0.9000 . ? N5 H5C 0.9000 . ? N6 C8 1.471(8) . ? N6 H6D 0.9000 . ? N6 H6E 0.9000 . ? C1 C2 1.488(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.573(11) . ? C2 H2A 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.491(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.540(11) . ? C5 H5A 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.533(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.530(9) . ? C8 H8A 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 Se4 Hg1 Se1 107.99(3) 2_755 2_655 ? Se4 Hg1 Se5 107.19(3) 2_755 . ? Se1 Hg1 Se5 126.04(3) 2_655 . ? Se4 Hg1 Se2 119.53(3) 2_755 . ? Se1 Hg1 Se2 102.80(2) 2_655 . ? Se5 Hg1 Se2 93.76(2) . . ? Se2 Sb1 Se1 100.10(3) . . ? Se2 Sb1 Se3 97.16(3) . . ? Se1 Sb1 Se3 93.10(3) . . ? Se4 Sb2 Se5 102.49(3) . . ? Se4 Sb2 Se3 92.35(3) . . ? Se5 Sb2 Se3 97.49(3) . . ? Sb1 Se1 Hg1 93.51(3) . 2_655 ? Sb1 Se2 Hg1 94.66(3) . . ? Sb2 Se3 Sb1 89.38(3) . . ? Sb2 Se4 Hg1 98.54(3) . 2_755 ? Sb2 Se5 Hg1 89.60(3) . . ? N3 Ni1 N1 94.2(3) . . ? N3 Ni1 N6 93.9(2) . . ? N1 Ni1 N6 170.5(2) . . ? N3 Ni1 N5 171.3(2) . . ? N1 Ni1 N5 91.9(2) . . ? N6 Ni1 N5 80.7(2) . . ? N3 Ni1 N2 92.3(3) . . ? N1 Ni1 N2 80.9(2) . . ? N6 Ni1 N2 93.8(2) . . ? N5 Ni1 N2 94.9(2) . . ? N3 Ni1 N4 81.7(2) . . ? N1 Ni1 N4 92.8(2) . . ? N6 Ni1 N4 93.3(2) . . ? N5 Ni1 N4 91.8(2) . . ? N2 Ni1 N4 171.0(2) . . ? C1 N1 Ni1 110.1(5) . . ? C1 N1 H1C 109.6 . . ? Ni1 N1 H1C 109.6 . . ? C1 N1 H1D 109.6 . . ? Ni1 N1 H1D 109.6 . . ? H1C N1 H1D 108.2 . . ? C2 N2 Ni1 107.7(5) . . ? C2 N2 H2B 110.2 . . ? Ni1 N2 H2B 110.2 . . ? C2 N2 H2C 110.2 . . ? Ni1 N2 H2C 110.2 . . ? H2B N2 H2C 108.5 . . ? C4 N3 Ni1 108.4(5) . . ? C4 N3 H3D 110.0 . . ? Ni1 N3 H3D 110.0 . . ? C4 N3 H3E 110.0 . . ? Ni1 N3 H3E 110.0 . . ? H3D N3 H3E 108.4 . . ? C5 N4 Ni1 108.7(5) . . ? C5 N4 H4C 109.9 . . ? Ni1 N4 H4C 109.9 . . ? C5 N4 H4D 109.9 . . ? Ni1 N4 H4D 109.9 . . ? H4C N4 H4D 108.3 . . ? C7 N5 Ni1 109.4(4) . . ? C7 N5 H5B 109.8 . . ? Ni1 N5 H5B 109.8 . . ? C7 N5 H5C 109.8 . . ? Ni1 N5 H5C 109.8 . . ? H5B N5 H5C 108.2 . . ? C8 N6 Ni1 109.8(4) . . ? C8 N6 H6D 109.7 . . ? Ni1 N6 H6D 109.7 . . ? C8 N6 H6E 109.7 . . ? Ni1 N6 H6E 109.7 . . ? H6D N6 H6E 108.2 . . ? C2 C1 N1 106.8(7) . . ? C2 C1 H1A 110.4 . . ? N1 C1 H1A 110.4 . . ? C2 C1 H1B 110.4 . . ? N1 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? N2 C2 C1 111.3(7) . . ? N2 C2 C3 113.1(7) . . ? C1 C2 C3 111.3(8) . . ? N2 C2 H2A 106.9 . . ? C1 C2 H2A 106.9 . . ? C3 C2 H2A 106.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 109.9(7) . . ? N3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N4 C5 C4 109.8(6) . . ? N4 C5 C6 113.0(7) . . ? C4 C5 C6 112.0(8) . . ? N4 C5 H5A 107.2 . . ? C4 C5 H5A 107.2 . . ? C6 C5 H5A 107.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 C8 109.2(6) . . ? N5 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N5 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N6 C8 C9 114.1(6) . . ? N6 C8 C7 106.4(5) . . ? C9 C8 C7 111.1(6) . . ? N6 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? C7 C8 H8A 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C Se1 0.90 2.68 3.561(6) 166.5 2_656 N1 H1D Se1 0.90 2.77 3.668(6) 176.8 . N2 H2B Se3 0.90 2.96 3.772(7) 150.4 2_766 N3 H3D Se4 0.90 2.71 3.543(7) 155.1 2_766 N3 H3E Se1 0.90 2.94 3.780(6) 155.0 . N4 H4C Se1 0.90 2.95 3.799(7) 157.6 2_656 N5 H5B Se2 0.90 2.78 3.547(5) 144.3 2_656 N5 H5C Se5 0.90 2.85 3.560(6) 136.7 1_556 N6 H6D Se5 0.90 2.79 3.651(6) 159.8 2_766 C4 H4A Se4 0.97 2.88 3.805(8) 160.0 1_455 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.998 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.194 data_compound-2-KW3-9C _database_code_depnum_ccdc_archive 'CCDC 909672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Hg Sb2 Se5, C8 H26 Mn N6' _chemical_formula_sum 'C8 H26 Hg Mn N6 Sb2 Se5' _chemical_formula_weight 1100.18 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.1774(2) _cell_length_b 20.3003(5) _cell_length_c 20.8304(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4726.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3261 _cell_measurement_theta_min 2.2275 _cell_measurement_theta_max 29.1295 _exptl_crystal_description sheet _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3944 _exptl_absorpt_coefficient_mu 16.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69262 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis CCD; Oxford, 2006' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13723 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5104 _reflns_number_gt 3830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0489P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5104 _refine_ls_number_parameters 244 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 0.997 _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 Hg1 Hg 0.43224(3) 0.62042(2) 0.826793(18) 0.03692(12) Uani 1 1 d . . . Sb1 Sb 0.59910(5) 0.62473(3) 0.66506(3) 0.02994(15) Uani 1 1 d . . . Sb2 Sb 0.27017(4) 0.60715(3) 0.66846(3) 0.02450(14) Uani 1 1 d . . . Se1 Se 0.10860(6) 0.65906(4) 0.59816(4) 0.0296(2) Uani 1 1 d . . . Se2 Se 0.33681(7) 0.70300(4) 0.73833(4) 0.0357(2) Uani 1 1 d . . . Se3 Se 0.43348(7) 0.60961(5) 0.57739(4) 0.0313(2) Uani 1 1 d . . . Se4 Se 0.76227(7) 0.56094(5) 0.60716(5) 0.0409(3) Uani 1 1 d . . . Se5 Se 0.53060(7) 0.53469(4) 0.74186(4) 0.0328(2) Uani 1 1 d . . . Mn1 Mn 0.21154(11) 0.89096(7) 0.60680(7) 0.0347(3) Uani 1 1 d . . . N1 N 0.2201(5) 0.9299(3) 0.7090(3) 0.0297(16) Uani 1 1 d . A . H1A H 0.2933 0.9465 0.7172 0.036 Uiso 1 1 calc R . . H1B H 0.1658 0.9622 0.7146 0.036 Uiso 1 1 calc R . . N2 N 0.0855(5) 0.8226(4) 0.6628(3) 0.0341(17) Uani 1 1 d . A . H2A H 0.1143 0.7808 0.6603 0.041 Uiso 1 1 calc R . . N3 N 0.0300(6) 0.9298(4) 0.5803(4) 0.045(2) Uani 1 1 d . A . H3A H 0.0266 0.9731 0.5896 0.054 Uiso 1 1 d R . . H3B H 0.0193 0.9253 0.5377 0.054 Uiso 1 1 d R . . N4 N 0.2175(7) 0.8148(4) 0.5265(4) 0.053(2) Uani 1 1 d . A . H4A H 0.1740 0.7794 0.5379 0.063 Uiso 1 1 d R . . H4B H 0.1849 0.8320 0.4907 0.063 Uiso 1 1 d R . . C1 C 0.1948(8) 0.8752(5) 0.7519(4) 0.041(2) Uani 1 1 d . . . H1C H 0.1873 0.8912 0.7956 0.049 Uiso 1 1 calc R A . H1D H 0.2600 0.8437 0.7505 0.049 Uiso 1 1 calc R . . C2 C 0.0789(7) 0.8420(5) 0.7313(4) 0.040(2) Uani 1 1 d . A . H2B H 0.0652 0.8032 0.7576 0.048 Uiso 1 1 calc R . . H2C H 0.0124 0.8720 0.7377 0.048 Uiso 1 1 calc R . . C3 C -0.0294(7) 0.8254(5) 0.6294(5) 0.044(2) Uani 1 1 d . . . H3C H -0.0900 0.8045 0.6558 0.053 Uiso 1 1 calc R A . H3D H -0.0235 0.8007 0.5896 0.053 Uiso 1 1 calc R . . C4 C -0.0676(8) 0.8949(5) 0.6146(5) 0.050(3) Uani 1 1 d . A . H4C H -0.1390 0.8943 0.5882 0.060 Uiso 1 1 calc R . . H4D H -0.0862 0.9179 0.6542 0.060 Uiso 1 1 calc R . . C5 C 0.3416(10) 0.7944(6) 0.5133(5) 0.069(3) Uani 1 1 d . . . H5A H 0.3413 0.7517 0.4925 0.083 Uiso 1 1 calc R A . H5B H 0.3783 0.8257 0.4841 0.083 Uiso 1 1 calc R . . C6 C 0.4121(10) 0.7909(6) 0.5723(7) 0.071(4) Uani 1 1 d . A . H6A H 0.4952 0.7834 0.5609 0.086 Uiso 1 1 d R . . H6B H 0.3857 0.7534 0.5975 0.086 Uiso 1 1 d R . . N5A N 0.391(2) 0.8435(15) 0.6145(19) 0.049(4) Uani 0.50 1 d PU A 1 H5C H 0.3960 0.8265 0.6548 0.058 Uiso 0.50 1 calc PR A 1 N6A N 0.3402(19) 0.9690(18) 0.5586(19) 0.040(4) Uani 0.50 1 d PU A 1 H6C H 0.3150 0.9781 0.5185 0.048 Uiso 0.50 1 calc PR A 1 H6D H 0.3396 1.0067 0.5814 0.048 Uiso 0.50 1 calc PR A 1 C7A C 0.483(2) 0.8989(13) 0.6114(11) 0.049(4) Uani 0.50 1 d PU A 1 H7A H 0.4784 0.9246 0.6505 0.058 Uiso 0.50 1 calc PR A 1 H7B H 0.5623 0.8803 0.6083 0.058 Uiso 0.50 1 calc PR A 1 C8A C 0.4617(18) 0.9418(12) 0.5567(11) 0.046(4) Uani 0.50 1 d PU A 1 H8A H 0.4725 0.9170 0.5173 0.056 Uiso 0.50 1 calc PR A 1 H8B H 0.5194 0.9774 0.5571 0.056 Uiso 0.50 1 calc PR A 1 N5B N 0.416(2) 0.8552(16) 0.6103(19) 0.050(4) Uani 0.50 1 d PU A 2 H5D H 0.4402 0.8483 0.6514 0.059 Uiso 0.50 1 calc PR A 2 N6B N 0.3074(18) 0.9698(19) 0.5597(19) 0.042(4) Uani 0.50 1 d PU A 2 H6E H 0.3034 0.9645 0.5169 0.051 Uiso 0.50 1 calc PR A 2 H6F H 0.2734 1.0087 0.5696 0.051 Uiso 0.50 1 calc PR A 2 C7B C 0.489(2) 0.9052(13) 0.5787(12) 0.051(4) Uani 0.50 1 d PU A 2 H7C H 0.5674 0.9064 0.5991 0.061 Uiso 0.50 1 calc PR A 2 H7D H 0.5012 0.8927 0.5342 0.061 Uiso 0.50 1 calc PR A 2 C8B C 0.4376(18) 0.9700(11) 0.5809(11) 0.051(4) Uani 0.50 1 d PU A 2 H8C H 0.4829 0.9992 0.5532 0.061 Uiso 0.50 1 calc PR A 2 H8D H 0.4428 0.9869 0.6244 0.061 Uiso 0.50 1 calc PR A 2 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 0.0252(2) 0.0550(3) 0.0305(2) -0.00443(18) -0.00089(14) 0.00447(15) Sb1 0.0209(3) 0.0354(3) 0.0334(3) -0.0079(3) -0.0009(2) 0.0000(2) Sb2 0.0218(3) 0.0245(3) 0.0272(3) 0.0028(2) 0.0001(2) 0.0017(2) Se1 0.0230(4) 0.0361(5) 0.0298(5) 0.0069(4) -0.0023(4) -0.0002(3) Se2 0.0449(5) 0.0316(5) 0.0305(5) -0.0043(4) -0.0063(4) 0.0097(4) Se3 0.0269(4) 0.0423(5) 0.0248(5) -0.0007(4) 0.0008(3) 0.0029(3) Se4 0.0232(4) 0.0593(6) 0.0402(6) -0.0160(5) 0.0063(4) -0.0017(4) Se5 0.0345(4) 0.0367(5) 0.0273(5) -0.0034(4) -0.0015(4) 0.0106(4) Mn1 0.0406(8) 0.0310(7) 0.0326(8) -0.0013(6) 0.0053(6) -0.0037(6) N1 0.031(4) 0.022(4) 0.036(4) -0.004(3) -0.006(3) -0.001(3) N2 0.035(4) 0.027(4) 0.040(5) -0.001(4) 0.002(3) -0.005(3) N3 0.058(5) 0.037(5) 0.041(5) 0.004(4) -0.011(4) -0.001(4) N4 0.074(5) 0.039(5) 0.046(5) -0.009(4) 0.017(4) -0.015(4) C1 0.056(6) 0.042(6) 0.026(5) 0.009(5) -0.006(5) 0.005(4) C2 0.046(5) 0.037(5) 0.037(6) 0.001(5) 0.008(4) -0.009(4) C3 0.039(5) 0.043(6) 0.049(6) 0.001(5) 0.002(5) -0.012(4) C4 0.043(6) 0.052(7) 0.054(7) -0.016(6) -0.005(5) 0.000(5) C5 0.107(9) 0.053(7) 0.048(7) -0.005(6) 0.032(7) 0.017(7) C6 0.083(8) 0.038(7) 0.093(10) 0.007(7) 0.025(8) 0.010(6) N5A 0.045(8) 0.051(8) 0.050(7) 0.008(7) 0.018(7) -0.008(7) N6A 0.041(9) 0.039(6) 0.039(6) -0.002(6) 0.018(8) -0.012(8) C7A 0.040(7) 0.062(8) 0.044(7) 0.003(7) 0.016(8) -0.007(6) C8A 0.043(7) 0.049(8) 0.047(8) -0.001(7) 0.016(7) -0.008(7) N5B 0.045(9) 0.057(8) 0.046(7) 0.003(7) 0.012(8) -0.006(7) N6B 0.044(9) 0.043(7) 0.040(6) -0.009(6) 0.017(8) -0.006(8) C7B 0.047(7) 0.060(8) 0.045(8) 0.000(8) 0.020(8) -0.007(7) C8B 0.047(7) 0.060(8) 0.046(7) -0.001(7) 0.016(7) -0.013(7) _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 Se1 2.6354(9) 6_657 ? Hg1 Se4 2.6382(9) 6_557 ? Hg1 Se2 2.7098(10) . ? Hg1 Se5 2.7142(9) . ? Sb1 Se4 2.5412(10) . ? Sb1 Se5 2.5469(11) . ? Sb1 Se3 2.6185(10) . ? Sb2 Se2 2.5414(10) . ? Sb2 Se1 2.5526(9) . ? Sb2 Se3 2.6332(10) . ? Se1 Hg1 2.6354(9) 6_557 ? Se4 Hg1 2.6382(9) 6_657 ? Mn1 N6B 2.16(3) . ? Mn1 N5A 2.23(3) . ? Mn1 N3 2.246(7) . ? Mn1 N1 2.274(7) . ? Mn1 N4 2.279(8) . ? Mn1 N2 2.295(7) . ? Mn1 N6A 2.36(3) . ? Mn1 N5B 2.40(3) . ? N1 C1 1.453(10) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.462(10) . ? N2 C2 1.483(10) . ? N2 H2A 0.9100 . ? N3 C4 1.485(11) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5 1.473(12) . ? N4 H4A 0.9001 . ? N4 H4B 0.9000 . ? C1 C2 1.522(11) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.507(13) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.463(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N5A 1.40(4) . ? C6 N5B 1.53(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N5A C7A 1.52(3) . ? N5A H5C 0.9100 . ? N6A C8A 1.47(3) . ? N6A H6C 0.9000 . ? N6A H6D 0.9000 . ? C7A C8A 1.45(3) . ? C7A H7A 0.9700 . ? C7A H7B 0.9700 . ? C8A H8A 0.9700 . ? C8A H8B 0.9700 . ? N5B C7B 1.46(3) . ? N5B H5D 0.9100 . ? N6B C8B 1.52(3) . ? N6B H6E 0.9000 . ? N6B H6F 0.9000 . ? C7B C8B 1.44(3) . ? C7B H7C 0.9700 . ? C7B H7D 0.9700 . ? C8B H8C 0.9700 . ? C8B H8D 0.9700 . ? 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 Se1 Hg1 Se4 111.44(3) 6_657 6_557 ? Se1 Hg1 Se2 120.90(3) 6_657 . ? Se4 Hg1 Se2 110.75(3) 6_557 . ? Se1 Hg1 Se5 105.93(3) 6_657 . ? Se4 Hg1 Se5 109.76(3) 6_557 . ? Se2 Hg1 Se5 96.48(3) . . ? Se4 Sb1 Se5 98.52(4) . . ? Se4 Sb1 Se3 96.70(3) . . ? Se5 Sb1 Se3 98.13(3) . . ? Se2 Sb2 Se1 102.70(3) . . ? Se2 Sb2 Se3 101.24(3) . . ? Se1 Sb2 Se3 93.97(3) . . ? Sb2 Se1 Hg1 93.78(3) . 6_557 ? Sb2 Se2 Hg1 91.79(3) . . ? Sb1 Se3 Sb2 89.42(3) . . ? Sb1 Se4 Hg1 92.07(3) . 6_657 ? Sb1 Se5 Hg1 94.08(3) . . ? N6B Mn1 N5A 84.6(9) . . ? N6B Mn1 N3 94.4(7) . . ? N5A Mn1 N3 169.0(11) . . ? N6B Mn1 N1 98.4(10) . . ? N5A Mn1 N1 92.6(11) . . ? N3 Mn1 N1 98.4(3) . . ? N6B Mn1 N4 98.9(10) . . ? N5A Mn1 N4 74.6(10) . . ? N3 Mn1 N4 94.8(3) . . ? N1 Mn1 N4 157.3(3) . . ? N6B Mn1 N2 169.2(9) . . ? N5A Mn1 N2 104.8(7) . . ? N3 Mn1 N2 77.5(3) . . ? N1 Mn1 N2 76.1(2) . . ? N4 Mn1 N2 88.9(3) . . ? N6B Mn1 N6A 7.8(14) . . ? N5A Mn1 N6A 76.9(11) . . ? N3 Mn1 N6A 102.1(7) . . ? N1 Mn1 N6A 98.0(10) . . ? N4 Mn1 N6A 97.2(10) . . ? N2 Mn1 N6A 173.9(9) . . ? N6B Mn1 N5B 76.4(11) . . ? N5A Mn1 N5B 8.3(12) . . ? N3 Mn1 N5B 167.0(9) . . ? N1 Mn1 N5B 92.1(10) . . ? N4 Mn1 N5B 77.8(9) . . ? N2 Mn1 N5B 112.7(7) . . ? N6A Mn1 N5B 68.7(9) . . ? C1 N1 Mn1 107.5(5) . . ? C1 N1 H1A 110.2 . . ? Mn1 N1 H1A 110.2 . . ? C1 N1 H1B 110.2 . . ? Mn1 N1 H1B 110.2 . . ? H1A N1 H1B 108.5 . . ? C3 N2 C2 113.8(7) . . ? C3 N2 Mn1 105.9(5) . . ? C2 N2 Mn1 111.1(5) . . ? C3 N2 H2A 108.6 . . ? C2 N2 H2A 108.6 . . ? Mn1 N2 H2A 108.6 . . ? C4 N3 Mn1 112.2(6) . . ? C4 N3 H3A 109.3 . . ? Mn1 N3 H3A 109.2 . . ? C4 N3 H3B 109.1 . . ? Mn1 N3 H3B 109.1 . . ? H3A N3 H3B 107.9 . . ? C5 N4 Mn1 110.8(6) . . ? C5 N4 H4A 109.5 . . ? Mn1 N4 H4A 109.4 . . ? C5 N4 H4B 109.6 . . ? Mn1 N4 H4B 109.5 . . ? H4A N4 H4B 108.0 . . ? N1 C1 C2 109.3(7) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.3 . . ? N2 C2 C1 110.3(7) . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? N2 C2 H2C 109.6 . . ? C1 C2 H2C 109.6 . . ? H2B C2 H2C 108.1 . . ? N2 C3 C4 112.4(7) . . ? N2 C3 H3C 109.1 . . ? C4 C3 H3C 109.1 . . ? N2 C3 H3D 109.1 . . ? C4 C3 H3D 109.1 . . ? H3C C3 H3D 107.8 . . ? N3 C4 C3 109.7(7) . . ? N3 C4 H4C 109.7 . . ? C3 C4 H4C 109.7 . . ? N3 C4 H4D 109.7 . . ? C3 C4 H4D 109.7 . . ? H4C C4 H4D 108.2 . . ? C6 C5 N4 111.4(9) . . ? C6 C5 H5A 109.4 . . ? N4 C5 H5A 109.4 . . ? C6 C5 H5B 109.4 . . ? N4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N5A C6 C5 113.5(18) . . ? N5A C6 N5B 13.7(18) . . ? C5 C6 N5B 114.0(17) . . ? N5A C6 H6A 115.5 . . ? C5 C6 H6A 108.6 . . ? N5B C6 H6A 103.6 . . ? N5A C6 H6B 101.9 . . ? C5 C6 H6B 109.3 . . ? N5B C6 H6B 113.4 . . ? H6A C6 H6B 107.5 . . ? C6 N5A C7A 115(2) . . ? C6 N5A Mn1 116(2) . . ? C7A N5A Mn1 106.3(19) . . ? C6 N5A H5C 106.3 . . ? C7A N5A H5C 106.3 . . ? Mn1 N5A H5C 106.3 . . ? C8A N6A Mn1 109(2) . . ? C8A N6A H6C 109.9 . . ? Mn1 N6A H6C 109.9 . . ? C8A N6A H6D 109.9 . . ? Mn1 N6A H6D 109.9 . . ? H6C N6A H6D 108.3 . . ? C8A C7A N5A 112(2) . . ? C8A C7A H7A 109.3 . . ? N5A C7A H7A 109.3 . . ? C8A C7A H7B 109.3 . . ? N5A C7A H7B 109.3 . . ? H7A C7A H7B 107.9 . . ? C7A C8A N6A 110.7(19) . . ? C7A C8A H8A 109.5 . . ? N6A C8A H8A 109.5 . . ? C7A C8A H8B 109.5 . . ? N6A C8A H8B 109.5 . . ? H8A C8A H8B 108.1 . . ? C7B N5B C6 112(3) . . ? C7B N5B Mn1 108(2) . . ? C6 N5B Mn1 102.6(15) . . ? C7B N5B H5D 111.2 . . ? C6 N5B H5D 111.2 . . ? Mn1 N5B H5D 111.2 . . ? C8B N6B Mn1 110(2) . . ? C8B N6B H6E 109.6 . . ? Mn1 N6B H6E 109.6 . . ? C8B N6B H6F 109.6 . . ? Mn1 N6B H6F 109.6 . . ? H6E N6B H6F 108.1 . . ? C8B C7B N5B 113(2) . . ? C8B C7B H7C 109.0 . . ? N5B C7B H7C 109.0 . . ? C8B C7B H7D 109.0 . . ? N5B C7B H7D 109.0 . . ? H7C C7B H7D 107.8 . . ? C7B C8B N6B 112(2) . . ? C7B C8B H8C 109.2 . . ? N6B C8B H8C 109.2 . . ? C7B C8B H8D 109.2 . . ? N6B C8B H8D 109.2 . . ? H8C C8B H8D 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Se5 0.90 2.79 3.651(6) 159.5 3_656 N1 H1B Se5 0.90 2.70 3.584(6) 166.1 8_665 N2 H2A Se1 0.91 2.79 3.592(7) 147.7 . N3 H3A Se3 0.90 2.82 3.673(8) 158.9 8_665 N3 H3B Se3 0.90 2.68 3.548(8) 163.3 4_466 N4 H4A Se1 0.90 2.84 3.702(8) 160.5 . N6A H6C Se4 0.90 2.80 3.61(4) 151.2 4_466 N6B H6E Se4 0.90 2.68 3.57(4) 171.7 4_466 C8B H8D Se5 0.97 2.97 3.93(2) 177.2 3_656 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.697 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.212 data_compound-3-KW3-11D _database_code_depnum_ccdc_archive 'CCDC 909673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(Hg Sb Se3), C6 H24 N6 Ni' _chemical_formula_sum 'C6 H24 Hg2 N6 Ni Sb2 Se6' _chemical_formula_weight 1357.46 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.4656(7) _cell_length_b 7.9377(2) _cell_length_c 15.2026(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.515(3) _cell_angle_gamma 90.00 _cell_volume 2367.77(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1431 _cell_measurement_theta_min 2.7625 _cell_measurement_theta_max 28.9411 _exptl_crystal_description sheet _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 25.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36690 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis CCD; Oxford, 2006' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4988 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2528 _reflns_number_gt 1980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0280P)^2^+2.0000P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00033(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2528 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Hg1 Hg 0.74776(2) 0.61108(5) 0.59678(3) 0.03437(16) Uani 1 1 d . . . Sb1 Sb 0.73384(3) 0.12900(7) 0.63753(4) 0.02164(18) Uani 1 1 d . . . Se1 Se 0.82343(4) 0.61118(11) 0.47057(7) 0.0233(2) Uani 1 1 d . . . Se2 Se 0.66124(5) 0.36347(11) 0.54497(8) 0.0334(3) Uani 1 1 d . . . Se3 Se 0.83761(5) 0.58389(18) 0.75152(8) 0.0509(4) Uani 1 1 d . . . Ni1 Ni 0.5000 0.36941(19) 0.2500 0.0209(4) Uani 1 2 d S . . N1 N 0.5557(3) 0.1889(9) 0.3437(5) 0.0224(17) Uani 1 1 d . . . H1C H 0.5652 0.0995 0.3131 0.027 Uiso 1 1 calc R . . H1D H 0.5953 0.2338 0.3774 0.027 Uiso 1 1 calc R . . N2 N 0.4346(4) 0.3559(10) 0.3369(6) 0.031(2) Uani 1 1 d . . . H2C H 0.4198 0.4593 0.3462 0.038 Uiso 1 1 calc R . . H2D H 0.3983 0.2904 0.3114 0.038 Uiso 1 1 calc R . . N3 N 0.5584(4) 0.5708(9) 0.3256(6) 0.039(2) Uani 1 1 d . . . H3C H 0.5681 0.5509 0.3863 0.047 Uiso 1 1 calc R . . H3D H 0.5977 0.5827 0.3109 0.047 Uiso 1 1 calc R . . C1 C 0.5142(5) 0.1353(12) 0.4041(7) 0.033(3) Uani 1 1 d . . . H1B H 0.5436 0.0897 0.4608 0.039 Uiso 1 1 calc R . . H1A H 0.4825 0.0478 0.3742 0.039 Uiso 1 1 calc R . . C2 C 0.4758(4) 0.2824(13) 0.4245(7) 0.032(2) Uani 1 1 d . . . H2A H 0.4464 0.2469 0.4609 0.038 Uiso 1 1 calc R . . H2B H 0.5074 0.3660 0.4591 0.038 Uiso 1 1 calc R . . C3 C 0.5161(5) 0.7246(11) 0.3008(8) 0.045(3) Uani 1 1 d . . . H3A H 0.5442 0.8241 0.3188 0.054 Uiso 1 1 calc R . . H3B H 0.4811 0.7258 0.3325 0.054 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 0.0434(3) 0.0333(2) 0.0236(2) 0.00343(17) 0.00488(19) -0.00906(19) Sb1 0.0164(3) 0.0272(3) 0.0203(3) 0.0011(3) 0.0037(2) 0.0005(3) Se1 0.0241(5) 0.0202(5) 0.0275(5) -0.0024(4) 0.0102(4) 0.0008(4) Se2 0.0291(5) 0.0213(5) 0.0398(7) 0.0024(4) -0.0067(5) -0.0022(4) Se3 0.0301(6) 0.1048(11) 0.0192(6) 0.0013(6) 0.0093(5) 0.0166(7) Ni1 0.0196(8) 0.0173(8) 0.0261(10) 0.000 0.0070(7) 0.000 N1 0.020(4) 0.025(4) 0.025(5) -0.002(3) 0.009(3) -0.002(3) N2 0.024(4) 0.031(5) 0.038(6) 0.001(4) 0.008(4) 0.004(4) N3 0.046(5) 0.027(4) 0.047(6) -0.009(4) 0.016(5) -0.014(4) C1 0.031(5) 0.033(6) 0.031(6) 0.007(5) 0.005(5) -0.008(5) C2 0.018(5) 0.049(6) 0.033(6) -0.002(5) 0.014(4) -0.003(5) C3 0.041(7) 0.016(5) 0.085(10) -0.012(5) 0.029(7) -0.008(5) _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 Se3 2.5499(11) . ? Hg1 Se2 2.6127(10) . ? Hg1 Se1 2.6802(10) 7_666 ? Hg1 Se1 2.7872(11) . ? Sb1 Se2 2.5422(10) . ? Sb1 Se3 2.5523(13) 4_646 ? Sb1 Se1 2.5718(11) 7_656 ? Se1 Sb1 2.5718(10) 7_656 ? Se1 Hg1 2.6802(10) 7_666 ? Se3 Sb1 2.5523(13) 4_656 ? Ni1 N1 2.111(7) 2_655 ? Ni1 N1 2.111(7) . ? Ni1 N3 2.127(7) . ? Ni1 N3 2.127(7) 2_655 ? Ni1 N2 2.134(8) 2_655 ? Ni1 N2 2.134(8) . ? N1 C1 1.481(12) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.478(11) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 C3 1.482(11) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? C1 C2 1.488(12) . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C3 1.50(2) 2_655 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? 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 Se3 Hg1 Se2 117.62(4) . . ? Se3 Hg1 Se1 126.39(4) . 7_666 ? Se2 Hg1 Se1 104.79(3) . 7_666 ? Se3 Hg1 Se1 103.83(4) . . ? Se2 Hg1 Se1 104.73(4) . . ? Se1 Hg1 Se1 94.87(3) 7_666 . ? Se2 Sb1 Se3 96.54(5) . 4_646 ? Se2 Sb1 Se1 95.77(4) . 7_656 ? Se3 Sb1 Se1 94.34(4) 4_646 7_656 ? Sb1 Se1 Hg1 105.43(4) 7_656 7_666 ? Sb1 Se1 Hg1 101.43(3) 7_656 . ? Hg1 Se1 Hg1 85.13(3) 7_666 . ? Sb1 Se2 Hg1 98.31(3) . . ? Hg1 Se3 Sb1 101.51(4) . 4_656 ? N1 Ni1 N1 94.5(4) 2_655 . ? N1 Ni1 N3 170.9(3) 2_655 . ? N1 Ni1 N3 91.9(3) . . ? N1 Ni1 N3 91.9(3) 2_655 2_655 ? N1 Ni1 N3 170.9(3) . 2_655 ? N3 Ni1 N3 82.5(5) . 2_655 ? N1 Ni1 N2 82.0(3) 2_655 2_655 ? N1 Ni1 N2 94.0(3) . 2_655 ? N3 Ni1 N2 91.0(3) . 2_655 ? N3 Ni1 N2 93.3(3) 2_655 2_655 ? N1 Ni1 N2 94.0(3) 2_655 . ? N1 Ni1 N2 82.0(3) . . ? N3 Ni1 N2 93.3(3) . . ? N3 Ni1 N2 91.0(3) 2_655 . ? N2 Ni1 N2 174.2(4) 2_655 . ? C1 N1 Ni1 108.6(5) . . ? C1 N1 H1C 110.0 . . ? Ni1 N1 H1C 110.0 . . ? C1 N1 H1D 110.0 . . ? Ni1 N1 H1D 110.0 . . ? H1C N1 H1D 108.4 . . ? C2 N2 Ni1 106.2(5) . . ? C2 N2 H2C 110.5 . . ? Ni1 N2 H2C 110.5 . . ? C2 N2 H2D 110.5 . . ? Ni1 N2 H2D 110.5 . . ? H2C N2 H2D 108.7 . . ? C3 N3 Ni1 106.5(6) . . ? C3 N3 H3C 110.4 . . ? Ni1 N3 H3C 110.4 . . ? C3 N3 H3D 110.4 . . ? Ni1 N3 H3D 110.4 . . ? H3C N3 H3D 108.6 . . ? N1 C1 C2 109.4(7) . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? H1B C1 H1A 108.2 . . ? N2 C2 C1 108.8(8) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N3 C3 C3 108.4(8) . 2_655 ? N3 C3 H3A 110.0 . . ? C3 C3 H3A 110.0 2_655 . ? N3 C3 H3B 110.0 . . ? C3 C3 H3B 110.0 2_655 . ? H3A C3 H3B 108.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C Se3 0.90 2.85 3.653(7) 148.7 7_656 N1 H1D Se2 0.90 2.72 3.492(7) 144.1 . C2 H2A Se1 0.97 2.78 3.648(9) 149.6 3_445 N2 H2C Se2 0.90 3.00 3.747(8) 141.0 5_666 N3 H3C Se2 0.90 3.01 3.777(9) 144.5 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.675 _refine_diff_density_min -2.150 _refine_diff_density_rms 0.264 data_compound-4-KW3-11E _database_code_depnum_ccdc_archive 'CCDC 909674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Hg2 Sb2 Se6, C8 H26 N6 Ni' _chemical_formula_sum 'C8 H26 Hg2 N6 Ni Sb2 Se6' _chemical_formula_weight 1383.50 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.1754(5) _cell_length_b 7.9178(3) _cell_length_c 20.6589(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2482.29(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1333 _cell_measurement_theta_min 2.3803 _cell_measurement_theta_max 29.1995 _exptl_crystal_description sheet _exptl_crystal_colour brown _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 24.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74846 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis CCD; Oxford, 2006' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6605 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3939 _reflns_number_gt 2880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0150P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(13) _refine_ls_number_reflns 3939 _refine_ls_number_parameters 226 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 0.995 _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 0.40106(6) 0.17549(12) 0.33538(7) 0.0363(3) Uani 1 1 d . . . Hg2 Hg 0.20424(6) 0.88813(11) 0.34008(6) 0.0347(3) Uani 1 1 d . . . Sb1 Sb 0.44059(10) 0.6703(2) 0.32473(9) 0.0238(4) Uani 1 1 d . . . Sb2 Sb 0.16111(9) 0.40317(19) 0.35646(8) 0.0210(4) Uani 1 1 d . . . Se1 Se 0.51936(18) 0.1427(5) 0.42194(17) 0.0540(10) Uani 1 1 d . . . Se2 Se 0.36256(16) 0.4330(3) 0.26244(14) 0.0267(6) Uani 1 1 d . . . Se3 Se 0.24472(16) 0.1539(3) 0.40987(13) 0.0230(6) Uani 1 1 d . . . Se4 Se 0.08484(14) 0.7889(3) 0.26092(14) 0.0276(6) Uani 1 1 d . . . Se5 Se 0.22462(17) 0.6373(3) 0.42678(15) 0.0308(7) Uani 1 1 d . . . Se6 Se 0.35871(15) 0.9012(3) 0.26234(14) 0.0232(6) Uani 1 1 d . . . Ni1 Ni 0.4576(2) 0.6035(4) 0.57384(17) 0.0201(8) Uani 1 1 d . . . N1 N 0.3802(12) 0.434(2) 0.5209(11) 0.033(6) Uani 1 1 d U . . H1C H 0.3597 0.4856 0.4852 0.040 Uiso 1 1 calc R . . H1D H 0.4136 0.3460 0.5084 0.040 Uiso 1 1 calc R . . N2 N 0.3517(12) 0.578(2) 0.6381(10) 0.022(5) Uani 1 1 d U . . H2C H 0.3670 0.4953 0.6665 0.027 Uiso 1 1 calc R . . N3 N 0.4933(13) 0.795(2) 0.6422(10) 0.031(6) Uani 1 1 d U . . H3C H 0.5478 0.7710 0.6580 0.037 Uiso 1 1 calc R . . N4 N 0.4085(13) 0.818(2) 0.5223(11) 0.038(6) Uani 1 1 d U . . H4C H 0.4382 0.8297 0.4848 0.045 Uiso 1 1 calc R . . H4D H 0.3512 0.8025 0.5129 0.045 Uiso 1 1 calc R . . N5 N 0.5332(13) 0.417(2) 0.6239(10) 0.027(5) Uani 1 1 d U . . H5C H 0.5465 0.4544 0.6639 0.032 Uiso 1 1 calc R . . H5D H 0.5015 0.3216 0.6279 0.032 Uiso 1 1 calc R . . N6 N 0.5744(12) 0.598(2) 0.5149(10) 0.030(5) Uani 1 1 d U . . H6C H 0.5670 0.5278 0.4811 0.036 Uiso 1 1 calc R . . H6D H 0.5866 0.7020 0.4996 0.036 Uiso 1 1 calc R . . C1 C 0.3060(14) 0.373(3) 0.5596(12) 0.025(6) Uani 1 1 d U . . H1A H 0.3240 0.2766 0.5856 0.030 Uiso 1 1 calc R . . H1B H 0.2581 0.3377 0.5316 0.030 Uiso 1 1 calc R . . C2 C 0.2766(16) 0.516(3) 0.6028(14) 0.033(7) Uani 1 1 d U . . H2A H 0.2514 0.6059 0.5768 0.040 Uiso 1 1 calc R . . H2B H 0.2319 0.4764 0.6327 0.040 Uiso 1 1 calc R . . C3 C 0.3408(15) 0.736(3) 0.6775(14) 0.033(7) Uani 1 1 d U . . H3A H 0.3107 0.8215 0.6523 0.040 Uiso 1 1 calc R . . H3B H 0.3058 0.7122 0.7157 0.040 Uiso 1 1 calc R . . C4 C 0.4302(14) 0.798(3) 0.6970(13) 0.033(7) Uani 1 1 d U . . H4A H 0.4251 0.9128 0.7133 0.039 Uiso 1 1 calc R . . H4B H 0.4527 0.7282 0.7318 0.039 Uiso 1 1 calc R . . C5 C 0.499(2) 0.951(4) 0.6052(17) 0.052(9) Uani 1 1 d U . . H5A H 0.5521 0.9498 0.5790 0.063 Uiso 1 1 calc R . . H5B H 0.5026 1.0464 0.6346 0.063 Uiso 1 1 calc R . . C6 C 0.4193(17) 0.970(3) 0.5619(16) 0.048(8) Uani 1 1 d U . . H6A H 0.3671 0.9879 0.5881 0.058 Uiso 1 1 calc R . . H6B H 0.4267 1.0680 0.5341 0.058 Uiso 1 1 calc R . . C7 C 0.6147(15) 0.382(3) 0.5881(15) 0.036(7) Uani 1 1 d U . . H7A H 0.6038 0.2956 0.5556 0.043 Uiso 1 1 calc R . . H7B H 0.6595 0.3400 0.6175 0.043 Uiso 1 1 calc R . . C8 C 0.6458(16) 0.539(3) 0.5564(15) 0.039(7) Uani 1 1 d U . . H8A H 0.6600 0.6233 0.5887 0.046 Uiso 1 1 calc R . . H8B H 0.6981 0.5162 0.5308 0.046 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 0.0261(5) 0.0252(6) 0.0576(9) 0.0052(6) -0.0016(7) -0.0009(4) Hg2 0.0323(5) 0.0266(6) 0.0454(8) 0.0031(6) -0.0090(6) -0.0091(5) Sb1 0.0256(8) 0.0235(9) 0.0222(11) -0.0004(8) 0.0002(9) 0.0024(7) Sb2 0.0213(7) 0.0191(9) 0.0227(11) -0.0018(8) -0.0033(8) 0.0001(7) Se1 0.0220(14) 0.101(3) 0.039(2) -0.012(2) 0.0047(15) 0.0009(17) Se2 0.0310(13) 0.0181(14) 0.0309(17) 0.0027(13) 0.0030(14) -0.0052(11) Se3 0.0238(12) 0.0160(14) 0.0292(17) -0.0008(11) 0.0024(13) 0.0009(11) Se4 0.0187(12) 0.0329(16) 0.0312(17) 0.0012(13) -0.0039(14) 0.0013(12) Se5 0.0414(15) 0.0155(14) 0.0355(18) -0.0006(12) -0.0121(14) -0.0007(12) Se6 0.0226(12) 0.0183(14) 0.0288(17) -0.0012(13) 0.0021(13) 0.0035(11) Ni1 0.0242(16) 0.0116(17) 0.025(2) -0.0011(14) -0.0001(15) -0.0016(15) N1 0.032(8) 0.030(9) 0.039(10) -0.003(8) -0.006(8) 0.003(7) N2 0.024(8) 0.020(8) 0.023(9) 0.006(7) -0.004(7) 0.002(7) N3 0.035(8) 0.026(9) 0.031(9) -0.002(7) 0.001(8) -0.004(7) N4 0.043(9) 0.034(9) 0.037(10) 0.009(8) -0.004(8) 0.002(8) N5 0.024(8) 0.029(9) 0.026(9) 0.006(7) 0.003(7) 0.003(7) N6 0.045(9) 0.026(8) 0.018(9) 0.002(7) 0.004(8) 0.004(8) C1 0.033(9) 0.024(9) 0.019(9) -0.003(8) -0.004(8) -0.001(8) C2 0.030(9) 0.030(10) 0.040(10) -0.006(8) 0.001(8) 0.000(8) C3 0.034(9) 0.034(10) 0.032(10) 0.003(8) 0.002(8) 0.007(8) C4 0.036(9) 0.033(10) 0.029(10) -0.005(8) 0.012(8) 0.001(8) C5 0.059(11) 0.047(12) 0.051(12) -0.001(9) 0.005(9) -0.008(9) C6 0.057(11) 0.036(11) 0.051(12) 0.003(9) 0.005(9) 0.005(9) C7 0.030(9) 0.038(10) 0.039(11) 0.004(8) 0.007(8) 0.004(8) C8 0.036(10) 0.037(10) 0.043(11) 0.000(9) 0.002(9) -0.004(8) _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 Se1 2.547(3) . ? Hg1 Se2 2.602(3) . ? Hg1 Se6 2.721(3) 1_545 ? Hg1 Se3 2.833(3) . ? Hg2 Se4 2.564(3) . ? Hg2 Se3 2.623(3) 1_565 ? Hg2 Se5 2.692(3) . ? Hg2 Se6 2.843(3) . ? Sb1 Se6 2.559(3) . ? Sb1 Se2 2.567(3) . ? Sb1 Se4 2.576(3) 3_565 ? Sb2 Se5 2.545(3) . ? Sb2 Se1 2.567(3) 3_455 ? Sb2 Se3 2.593(3) . ? Se1 Sb2 2.567(3) 3 ? Se3 Hg2 2.623(3) 1_545 ? Se4 Sb1 2.576(3) 3_465 ? Se6 Hg1 2.721(3) 1_565 ? Ni1 N1 2.09(2) . ? Ni1 N2 2.09(2) . ? Ni1 N5 2.137(18) . ? Ni1 N4 2.14(2) . ? Ni1 N3 2.14(2) . ? Ni1 N6 2.151(19) . ? N1 C1 1.46(3) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.44(3) . ? N2 C3 1.50(3) . ? N2 H2C 0.9100 . ? N3 C5 1.45(3) . ? N3 C4 1.48(3) . ? N3 H3C 0.9100 . ? N4 C6 1.47(3) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 C7 1.47(3) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 C8 1.46(3) . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? C1 C2 1.51(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.50(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.51(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.48(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 Se1 Hg1 Se2 130.14(11) . . ? Se1 Hg1 Se6 118.32(10) . 1_545 ? Se2 Hg1 Se6 104.55(10) . 1_545 ? Se1 Hg1 Se3 101.70(10) . . ? Se2 Hg1 Se3 100.02(8) . . ? Se6 Hg1 Se3 93.16(8) 1_545 . ? Se4 Hg2 Se3 139.61(9) . 1_565 ? Se4 Hg2 Se5 106.23(9) . . ? Se3 Hg2 Se5 101.48(9) 1_565 . ? Se4 Hg2 Se6 103.50(9) . . ? Se3 Hg2 Se6 95.06(8) 1_565 . ? Se5 Hg2 Se6 107.93(8) . . ? Se6 Sb1 Se2 92.66(10) . . ? Se6 Sb1 Se4 93.75(10) . 3_565 ? Se2 Sb1 Se4 103.14(10) . 3_565 ? Se5 Sb2 Se1 96.88(12) . 3_455 ? Se5 Sb2 Se3 97.26(10) . . ? Se1 Sb2 Se3 94.47(11) 3_455 . ? Hg1 Se1 Sb2 103.59(13) . 3 ? Sb1 Se2 Hg1 100.35(10) . . ? Sb2 Se3 Hg2 105.20(10) . 1_545 ? Sb2 Se3 Hg1 97.62(9) . . ? Hg2 Se3 Hg1 86.91(8) 1_545 . ? Hg2 Se4 Sb1 103.63(11) . 3_465 ? Sb2 Se5 Hg2 96.55(10) . . ? Sb1 Se6 Hg1 100.15(10) . 1_565 ? Sb1 Se6 Hg2 95.15(9) . . ? Hg1 Se6 Hg2 84.87(8) 1_565 . ? N1 Ni1 N2 80.8(8) . . ? N1 Ni1 N5 96.4(8) . . ? N2 Ni1 N5 92.2(7) . . ? N1 Ni1 N4 93.0(8) . . ? N2 Ni1 N4 97.1(8) . . ? N5 Ni1 N4 167.7(8) . . ? N1 Ni1 N3 160.2(8) . . ? N2 Ni1 N3 81.0(8) . . ? N5 Ni1 N3 92.0(8) . . ? N4 Ni1 N3 81.6(8) . . ? N1 Ni1 N6 98.9(8) . . ? N2 Ni1 N6 171.7(8) . . ? N5 Ni1 N6 79.5(7) . . ? N4 Ni1 N6 91.2(8) . . ? N3 Ni1 N6 100.3(8) . . ? C1 N1 Ni1 111.1(16) . . ? C1 N1 H1C 109.4 . . ? Ni1 N1 H1C 109.4 . . ? C1 N1 H1D 109.4 . . ? Ni1 N1 H1D 109.4 . . ? H1C N1 H1D 108.0 . . ? C2 N2 C3 118.3(18) . . ? C2 N2 Ni1 108.6(15) . . ? C3 N2 Ni1 110.5(14) . . ? C2 N2 H2C 106.3 . . ? C3 N2 H2C 106.3 . . ? Ni1 N2 H2C 106.3 . . ? C5 N3 C4 115(2) . . ? C5 N3 Ni1 105.7(17) . . ? C4 N3 Ni1 110.5(15) . . ? C5 N3 H3C 108.4 . . ? C4 N3 H3C 108.4 . . ? Ni1 N3 H3C 108.4 . . ? C6 N4 Ni1 109.6(18) . . ? C6 N4 H4C 109.7 . . ? Ni1 N4 H4C 109.7 . . ? C6 N4 H4D 109.7 . . ? Ni1 N4 H4D 109.7 . . ? H4C N4 H4D 108.2 . . ? C7 N5 Ni1 109.8(15) . . ? C7 N5 H5C 109.7 . . ? Ni1 N5 H5C 109.7 . . ? C7 N5 H5D 109.7 . . ? Ni1 N5 H5D 109.7 . . ? H5C N5 H5D 108.2 . . ? C8 N6 Ni1 106.5(16) . . ? C8 N6 H6C 110.4 . . ? Ni1 N6 H6C 110.4 . . ? C8 N6 H6D 110.4 . . ? Ni1 N6 H6D 110.4 . . ? H6C N6 H6D 108.6 . . ? N1 C1 C2 107.5(19) . . ? N1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? N1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? N2 C2 C1 108.9(19) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 N2 108.7(19) . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? N2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 112(2) . . ? N3 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 110(2) . . ? N3 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C5 110(2) . . ? N4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N5 C7 C8 109(2) . . ? N5 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N5 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N6 C8 C7 107(2) . . ? N6 C8 H8A 110.3 . . ? C7 C8 H8A 110.3 . . ? N6 C8 H8B 110.3 . . ? C7 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C Se5 0.90 2.66 3.46(2) 147.4 . N1 H1D Se1 0.90 2.89 3.74(2) 157.2 . N2 H2C Se4 0.91 2.65 3.551(19) 171.8 4_545 N3 H3C Se2 0.91 3.02 3.77(2) 141.3 2_665 N4 H4D Se5 0.90 2.93 3.70(2) 145.6 . N4 H4C Se1 0.90 3.06 3.71(2) 130.7 1_565 N5 H5C Se2 0.90 2.62 3.48(2) 160.8 2_665 N5 H5D Se4 0.90 3.06 3.50(2) 112.5 4_545 N6 H6D Se5 0.90 2.88 3.591(19) 137.4 3_565 C1 H1B Se3 0.97 2.91 3.67(2) 135.3 . C6 H6B Se1 0.97 2.77 3.54(3) 136.4 1_565 C8 H8B Se3 0.97 2.93 3.71(3) 138.3 3 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.256 _refine_diff_density_min -2.190 _refine_diff_density_rms 0.356 data_compound-5-KW4-18D _database_code_depnum_ccdc_archive 'CCDC 909675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Hg3 Sb3 Se8, C2 H8 N' _chemical_formula_sum 'C2 H8 Hg3 N Sb3 Se8' _chemical_formula_weight 1644.79 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 orthorhombic _symmetry_space_group_name_H-M 'A b m 2' _symmetry_space_group_name_Hall 'A 2 -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, z' '-x, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x, -y+1, z+1/2' '-x, y+1, z+1/2' _cell_length_a 11.3895(5) _cell_length_b 15.5501(7) _cell_length_c 11.2968(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2000.75(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1177 _cell_measurement_theta_min 2.6144 _cell_measurement_theta_max 28.8876 _exptl_crystal_description sheet _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 41.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.04698 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlis CCD; Oxford, 2006' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2416 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.75 _reflns_number_total 1481 _reflns_number_gt 1290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND. Version 3.0. Crystal Impact' _computing_publication_material 'Windows Word 2003' _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^)+(0.0980P)^2^+3.8000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 1481 _refine_ls_number_parameters 86 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1705 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.084 _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 0.81984(14) 0.37568(8) 0.18454(13) 0.0329(4) Uani 1 1 d . . . Hg2 Hg 1.0000 0.5000 -0.06698(17) 0.0307(5) Uani 1 2 d S . . Sb1 Sb 1.0170(3) 0.2500 -0.0592(3) 0.0219(7) Uani 1 2 d S . . Sb2 Sb 0.66569(19) 0.48271(14) -0.0901(3) 0.0251(6) Uani 1 1 d . . . Se1 Se 0.8168(3) 0.5271(2) 0.0696(3) 0.0227(7) Uani 1 1 d . . . Se2 Se 0.6408(4) 0.3681(2) 0.3242(3) 0.0356(10) Uani 1 1 d . . . Se3 Se 1.0311(3) 0.36703(17) 0.2877(3) 0.0231(8) Uani 1 1 d . . . Se4 Se 0.8068(5) 0.2500 0.0220(4) 0.0254(11) Uani 1 2 d S . . Se5 Se 0.5000 0.5000 0.0633(4) 0.0296(12) Uani 1 2 d S . . N1 N 0.623(6) 0.2500 0.575(4) 0.076(18) Uani 1 2 d SDU . . H1A H 0.6511 0.2034 0.5369 0.092 Uiso 0.50 1 d PR . . H1B H 0.6511 0.2966 0.5369 0.092 Uiso 0.50 1 d PR . . C1 C 0.672(4) 0.2500 0.693(4) 0.025(10) Uani 1 2 d SDU . . H1C H 0.7567 0.2500 0.6907 0.037 Uiso 1 2 d SR . . H1D H 0.6456 0.3004 0.7343 0.037 Uiso 1 1 d R . . C2 C 0.499(5) 0.2500 0.567(5) 0.038(13) Uani 1 2 d SU . . H2A H 0.4787 0.2500 0.4850 0.057 Uiso 1 2 d SR . . H2B H 0.4676 0.1996 0.6046 0.057 Uiso 0.50 1 d PR . . H2C H 0.4676 0.3004 0.6046 0.057 Uiso 0.50 1 d PR . . 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 0.0399(9) 0.0338(8) 0.0250(8) 0.0000(7) 0.0016(8) 0.0053(5) Hg2 0.0283(10) 0.0243(9) 0.0394(13) 0.000 0.000 0.0024(8) Sb1 0.0292(19) 0.0187(13) 0.0177(16) 0.000 -0.0011(14) 0.000 Sb2 0.0250(12) 0.0256(13) 0.0247(13) -0.0053(10) -0.0004(10) 0.0009(9) Se1 0.0211(18) 0.0218(15) 0.025(2) -0.0019(14) -0.0015(15) 0.0013(12) Se2 0.042(2) 0.039(2) 0.026(2) -0.0108(16) 0.0074(18) -0.0160(17) Se3 0.029(2) 0.0202(15) 0.0198(18) 0.0035(13) -0.0003(16) 0.0069(12) Se4 0.033(3) 0.023(2) 0.020(3) 0.000 0.003(2) 0.000 Se5 0.026(3) 0.043(3) 0.020(3) 0.000 0.000 -0.002(2) N1 0.07(2) 0.08(2) 0.08(2) 0.000 0.000(10) 0.000 C1 0.016(13) 0.029(13) 0.029(13) 0.000 0.002(9) 0.000 C2 0.037(16) 0.039(15) 0.039(16) 0.000 -0.002(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 Se2 2.581(5) . ? Hg1 Se3 2.676(4) . ? Hg1 Se4 2.685(4) . ? Hg1 Se1 2.690(4) . ? Hg2 Se1 2.629(4) 2_765 ? Hg2 Se1 2.629(4) . ? Hg2 Se3 2.664(3) 8_744 ? Hg2 Se3 2.664(3) 7_554 ? Sb1 Se4 2.564(6) . ? Sb1 Se3 2.569(4) 6_754 ? Sb1 Se3 2.569(4) 8_744 ? Sb2 Se2 2.530(4) 7_554 ? Sb2 Se5 2.576(4) . ? Sb2 Se1 2.587(4) . ? Se2 Sb2 2.530(4) 7 ? Se3 Sb1 2.569(4) 6_755 ? Se3 Hg2 2.664(3) 7 ? Se4 Hg1 2.685(4) 3 ? Se5 Sb2 2.576(4) 2_665 ? N1 C2 1.42(8) . ? N1 C1 1.448(10) . ? N1 H1A 0.9001 . ? N1 H1B 0.9001 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 H2A 0.9601 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? 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 Se2 Hg1 Se3 116.20(14) . . ? Se2 Hg1 Se4 109.94(15) . . ? Se3 Hg1 Se4 108.10(14) . . ? Se2 Hg1 Se1 108.98(13) . . ? Se3 Hg1 Se1 105.42(11) . . ? Se4 Hg1 Se1 107.84(13) . . ? Se1 Hg2 Se1 108.15(18) 2_765 . ? Se1 Hg2 Se3 110.02(10) 2_765 8_744 ? Se1 Hg2 Se3 112.38(10) . 8_744 ? Se1 Hg2 Se3 112.38(10) 2_765 7_554 ? Se1 Hg2 Se3 110.02(10) . 7_554 ? Se3 Hg2 Se3 103.91(15) 8_744 7_554 ? Se4 Sb1 Se3 92.41(15) . 6_754 ? Se4 Sb1 Se3 92.41(15) . 8_744 ? Se3 Sb1 Se3 90.20(17) 6_754 8_744 ? Se2 Sb2 Se5 94.57(12) 7_554 . ? Se2 Sb2 Se1 95.53(15) 7_554 . ? Se5 Sb2 Se1 89.46(13) . . ? Sb2 Se1 Hg2 94.37(13) . . ? Sb2 Se1 Hg1 96.40(12) . . ? Hg2 Se1 Hg1 97.62(11) . . ? Sb2 Se2 Hg1 95.94(14) 7 . ? Sb1 Se3 Hg2 96.13(13) 6_755 7 ? Sb1 Se3 Hg1 97.88(14) 6_755 . ? Hg2 Se3 Hg1 96.32(11) 7 . ? Sb1 Se4 Hg1 101.14(16) . . ? Sb1 Se4 Hg1 101.14(16) . 3 ? Hg1 Se4 Hg1 93.40(17) . 3 ? Sb2 Se5 Sb2 95.5(2) 2_665 . ? C2 N1 C1 116(5) . . ? C2 N1 H1A 108.7 . . ? C1 N1 H1A 107.8 . . ? C2 N1 H1B 108.7 . . ? C1 N1 H1B 107.8 . . ? H1A N1 H1B 107.1 . . ? N1 C1 H1C 110.9 . . ? N1 C1 H1D 108.8 . . ? H1C C1 H1D 109.5 . . ? N1 C2 H2A 107.7 . . ? N1 C2 H2B 110.4 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 110.4 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B Se2 0.90 2.65 3.38(4) 139.1 . N1 H1A Se2 0.90 2.65 3.38(4) 139.1 3 C2 H2C Se2 0.96 2.96 3.79(5) 144.4 8_645 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.502 _refine_diff_density_min -3.823 _refine_diff_density_rms 0.772