# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef 'compound 1-kw3-40b.CIF' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Xiao-Ying Huang' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. CHINA ; _publ_contact_author_email xyhuang@fjirsm.ac.cn _publ_contact_author_phone 86-59183793727 _publ_contact_author_fax 86-59183793727 loop_ _publ_author_name _publ_author_address 'Kai-Yao Wang' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 Graduate School of the Chinese Academy of Sciences Beijing, 10049 P. R. CHINA ; 'Liu-Jiang Zhou' ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 Graduate School of the Chinese Academy of Sciences Beijing, 10049 P. R. CHINA ; 'Xiao-Ying Huang' ; State Key Lab of Structural Chemistry Fujian Institute of Reseach on the Structure of Matter, Chinese Academy of Sciences Fuzhou 350002 P. R. CHINA ; _publ_section_title ; Novel Organic-Decorated Quaternary TM-Hg-Sb-Q Compounds (TM = Mn, Fe, Co; Q = S, Se): Assembly of Three Types of Metal Coordination Geometries ; data_compound-1-KW3-40B _database_code_depnum_ccdc_archive 'CCDC 862155' #TrackingRef 'compound 1-kw3-40b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Hg Mn2 N4 S6 Sb2' _chemical_formula_sum 'C24 H16 Hg Mn2 N4 S6 Sb2' _chemical_formula_weight 1106.74 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' Hg Hg -2.3894 9.2266 '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' 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' Sb Sb -0.5866 1.5461 '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 7.7501(8) _cell_length_b 8.6677(8) _cell_length_c 11.4926(12) _cell_angle_alpha 106.744(9) _cell_angle_beta 92.718(8) _cell_angle_gamma 102.944(8) _cell_volume 715.30(13) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1367 _cell_measurement_theta_min 2.5282 _cell_measurement_theta_max 29.1330 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 8.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60246 _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 6125 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.74 _reflns_number_total 3001 _reflns_number_gt 2103 _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^)+(0.0270P)^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 3001 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 1.0000 0.5000 0.5000 0.03822(18) Uani 1 2 d S . . Sb1 Sb 0.62176(8) 0.26035(7) 0.61894(5) 0.02990(18) Uani 1 1 d . . . Mn1 Mn 0.42849(18) 0.32596(15) 0.36805(11) 0.0291(3) Uani 1 1 d . . . S1 S 0.6629(3) 0.1703(3) 0.4094(2) 0.0373(6) Uani 1 1 d . . . S2 S 0.3743(3) 0.3825(3) 0.59444(19) 0.0285(5) Uani 1 1 d . . . S3 S 0.8519(3) 0.5307(3) 0.6773(2) 0.0313(6) Uani 1 1 d . . . N1 N 0.4271(9) 0.2527(8) 0.1601(6) 0.0229(16) Uani 1 1 d . . . N2 N 0.2176(9) 0.0886(7) 0.2899(6) 0.0223(16) Uani 1 1 d . . . C1 C 0.5222(12) 0.3378(10) 0.0978(7) 0.030(2) Uani 1 1 d . . . H1A H 0.5988 0.4401 0.1404 0.035 Uiso 1 1 calc R . . C2 C 0.5141(12) 0.2824(11) -0.0294(8) 0.036(2) Uani 1 1 d . . . H2A H 0.5851 0.3466 -0.0699 0.043 Uiso 1 1 calc R . . C3 C 0.4016(12) 0.1335(10) -0.0941(8) 0.034(2) Uani 1 1 d . . . H3A H 0.3933 0.0962 -0.1791 0.041 Uiso 1 1 calc R . . C4 C 0.2980(11) 0.0370(10) -0.0306(7) 0.029(2) Uani 1 1 d . . . C5 C 0.1747(11) -0.1179(11) -0.0885(8) 0.034(2) Uani 1 1 d . . . H5A H 0.1617 -0.1614 -0.1733 0.041 Uiso 1 1 calc R . . C6 C 0.0776(12) -0.2018(11) -0.0247(8) 0.037(2) Uani 1 1 d . . . H6A H 0.0011 -0.3049 -0.0656 0.044 Uiso 1 1 calc R . . C7 C 0.0870(11) -0.1386(10) 0.1057(8) 0.028(2) Uani 1 1 d . . . C8 C -0.0179(11) -0.2191(10) 0.1777(9) 0.035(2) Uani 1 1 d . . . H8A H -0.0955 -0.3233 0.1420 0.043 Uiso 1 1 calc R . . C9 C -0.0046(12) -0.1430(11) 0.2997(8) 0.038(2) Uani 1 1 d . . . H9A H -0.0745 -0.1941 0.3483 0.046 Uiso 1 1 calc R . . C10 C 0.1128(12) 0.0101(10) 0.3515(8) 0.036(2) Uani 1 1 d . . . H10A H 0.1177 0.0606 0.4353 0.043 Uiso 1 1 calc R . . C11 C 0.2036(10) 0.0154(9) 0.1668(7) 0.0197(18) Uani 1 1 d . . . C12 C 0.3139(11) 0.1052(10) 0.0991(7) 0.0235(19) Uani 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 Hg1 0.0387(4) 0.0458(3) 0.0328(3) 0.0131(3) 0.0129(3) 0.0126(3) Sb1 0.0313(4) 0.0328(4) 0.0213(3) 0.0067(3) 0.0019(3) 0.0018(3) Mn1 0.0323(8) 0.0274(7) 0.0171(7) -0.0001(5) 0.0019(6) -0.0044(6) S1 0.0398(15) 0.0435(14) 0.0227(12) -0.0012(10) 0.0063(11) 0.0130(12) S2 0.0241(12) 0.0315(12) 0.0219(11) 0.0033(9) 0.0032(10) -0.0031(10) S3 0.0282(13) 0.0340(12) 0.0222(11) 0.0005(9) 0.0007(10) 0.0000(11) N1 0.023(4) 0.026(4) 0.016(3) 0.003(3) 0.000(3) 0.005(3) N2 0.021(4) 0.023(4) 0.021(4) 0.005(3) 0.004(3) 0.003(3) C1 0.037(6) 0.027(5) 0.023(5) 0.009(4) 0.008(4) 0.003(4) C2 0.039(6) 0.041(6) 0.029(5) 0.013(4) 0.013(5) 0.010(5) C3 0.040(6) 0.039(5) 0.023(5) 0.002(4) 0.007(4) 0.021(5) C4 0.028(5) 0.032(5) 0.024(5) 0.002(4) 0.004(4) 0.016(4) C5 0.027(5) 0.041(5) 0.022(5) -0.007(4) -0.011(4) 0.009(4) C6 0.033(6) 0.033(5) 0.032(5) -0.003(4) -0.014(5) 0.005(5) C7 0.017(5) 0.027(5) 0.035(5) 0.003(4) -0.006(4) 0.007(4) C8 0.019(5) 0.026(5) 0.051(6) 0.011(4) -0.007(5) -0.011(4) C9 0.032(6) 0.047(6) 0.028(5) 0.012(4) 0.002(5) -0.003(5) C10 0.043(6) 0.033(5) 0.026(5) 0.004(4) 0.012(5) 0.004(5) C11 0.016(4) 0.021(4) 0.017(4) 0.001(3) -0.009(3) 0.005(4) C12 0.030(5) 0.025(4) 0.019(4) 0.004(3) 0.005(4) 0.018(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 Hg1 S3 2.364(2) 2_766 ? Hg1 S3 2.364(2) . ? Sb1 S1 2.369(2) . ? Sb1 S2 2.430(3) . ? Sb1 S3 2.496(2) . ? Mn1 N2 2.236(6) . ? Mn1 N1 2.288(6) . ? Mn1 S2 2.547(2) 2_666 ? Mn1 S2 2.578(2) . ? Mn1 S1 2.595(3) . ? Mn1 S3 2.831(3) 2_666 ? S2 Mn1 2.547(2) 2_666 ? S3 Mn1 2.831(3) 2_666 ? N1 C1 1.308(9) . ? N1 C12 1.349(9) . ? N2 C10 1.307(9) . ? N2 C11 1.361(9) . ? C1 C2 1.395(11) . ? C1 H1A 0.9300 . ? C2 C3 1.364(11) . ? C2 H2A 0.9300 . ? C3 C4 1.408(11) . ? C3 H3A 0.9300 . ? C4 C5 1.418(11) . ? C4 C12 1.424(10) . ? C5 C6 1.322(12) . ? C5 H5A 0.9300 . ? C6 C7 1.431(11) . ? C6 H6A 0.9300 . ? C7 C11 1.397(10) . ? C7 C8 1.405(12) . ? C8 C9 1.355(12) . ? C8 H8A 0.9300 . ? C9 C10 1.377(11) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.434(10) . ? 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 S3 Hg1 S3 180.0 2_766 . ? S1 Sb1 S2 97.13(8) . . ? S1 Sb1 S3 97.40(8) . . ? S2 Sb1 S3 94.49(8) . . ? N2 Mn1 N1 73.4(2) . . ? N2 Mn1 S2 163.0(2) . 2_666 ? N1 Mn1 S2 94.29(17) . 2_666 ? N2 Mn1 S2 98.17(17) . . ? N1 Mn1 S2 170.40(18) . . ? S2 Mn1 S2 93.03(7) 2_666 . ? N2 Mn1 S1 92.28(19) . . ? N1 Mn1 S1 96.57(18) . . ? S2 Mn1 S1 100.86(9) 2_666 . ? S2 Mn1 S1 88.14(8) . . ? N2 Mn1 S3 82.76(19) . 2_666 ? N1 Mn1 S3 83.90(18) . 2_666 ? S2 Mn1 S3 84.38(8) 2_666 2_666 ? S2 Mn1 S3 90.64(8) . 2_666 ? S1 Mn1 S3 174.67(9) . 2_666 ? Sb1 S1 Mn1 87.45(8) . . ? Sb1 S2 Mn1 94.45(8) . 2_666 ? Sb1 S2 Mn1 86.54(7) . . ? Mn1 S2 Mn1 86.97(7) 2_666 . ? Hg1 S3 Sb1 100.96(8) . . ? Hg1 S3 Mn1 104.75(9) . 2_666 ? Sb1 S3 Mn1 86.39(8) . 2_666 ? C1 N1 C12 118.9(7) . . ? C1 N1 Mn1 127.0(5) . . ? C12 N1 Mn1 114.1(5) . . ? C10 N2 C11 117.2(7) . . ? C10 N2 Mn1 126.4(5) . . ? C11 N2 Mn1 116.4(5) . . ? N1 C1 C2 123.1(8) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 119.6(8) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 119.1(8) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 123.9(8) . . ? C3 C4 C12 117.1(8) . . ? C5 C4 C12 119.0(8) . . ? C6 C5 C4 121.5(8) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 121.9(8) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C11 C7 C8 116.8(8) . . ? C11 C7 C6 118.8(8) . . ? C8 C7 C6 124.3(8) . . ? C9 C8 C7 119.1(8) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.8(8) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? N2 C10 C9 123.8(8) . . ? N2 C10 H10A 118.1 . . ? C9 C10 H10A 118.1 . . ? N2 C11 C7 123.2(7) . . ? N2 C11 C12 116.9(6) . . ? C7 C11 C12 119.9(7) . . ? N1 C12 C4 122.1(7) . . ? N1 C12 C11 118.9(7) . . ? C4 C12 C11 118.9(7) . . ? 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 C3 H3A S1 0.93 2.91 3.749(9) 151.3 2_655 C9 H9A S2 0.93 2.75 3.622(9) 156.5 2_556 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.039 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.197 data_compound-2-KW3-43A _database_code_depnum_ccdc_archive 'CCDC 862156' #TrackingRef 'compound 2-kw3-43a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Hg Mn N4 Sb2 Se5' _chemical_formula_sum 'C6 H18 Hg Mn N4 Sb2 Se5' _chemical_formula_weight 1040.07 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' Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 '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 7.5404(4) _cell_length_b 10.8268(6) _cell_length_c 12.5959(9) _cell_angle_alpha 69.403(6) _cell_angle_beta 78.061(5) _cell_angle_gamma 86.215(5) _cell_volume 941.73(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2784 _cell_measurement_theta_min 2.7555 _cell_measurement_theta_max 29.0130 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 21.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49477 _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 7963 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.75 _reflns_number_total 3974 _reflns_number_gt 3269 _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^)+(0.0377P)^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 3974 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.084 _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 0.33167(5) 0.15597(4) 0.28579(4) 0.03032(13) Uani 1 1 d . . . Sb1 Sb 0.07097(9) 0.32463(6) 0.47141(6) 0.02124(16) Uani 1 1 d . . . Sb2 Sb 0.20338(8) -0.07671(6) 0.62557(6) 0.01825(16) Uani 1 1 d . . . Se1 Se 0.36179(12) 0.15009(9) 0.50678(9) 0.0185(2) Uani 1 1 d . . . Se2 Se 0.25705(13) 0.49648(9) 0.49904(9) 0.0220(2) Uani 1 1 d . . . Se3 Se 0.65869(13) 0.11588(9) 0.19460(9) 0.0216(2) Uani 1 1 d . . . Se4 Se 0.09566(13) -0.01846(10) 0.30451(11) 0.0301(3) Uani 1 1 d . . . Se5 Se 0.15857(15) 0.39192(10) 0.25178(10) 0.0296(3) Uani 1 1 d . . . Mn1 Mn 0.2969(2) 0.37267(14) 0.71037(14) 0.0218(3) Uani 1 1 d . . . N1 N 0.3599(13) 0.5452(8) 0.7488(8) 0.035(2) Uani 1 1 d . . . H1A H 0.2965 0.6138 0.7095 0.041 Uiso 1 1 d R . . H1D H 0.4787 0.5666 0.7244 0.041 Uiso 1 1 d R . . N2 N 0.4987(11) 0.2193(8) 0.7253(8) 0.030(2) Uani 1 1 d . . . H2A H 0.5873 0.2575 0.6646 0.036 Uiso 1 1 d R . . H2D H 0.4587 0.1459 0.7169 0.036 Uiso 1 1 d R . . N3 N 0.0249(11) 0.2802(9) 0.7836(8) 0.029(2) Uani 1 1 d . . . H3A H 0.0007 0.2384 0.7369 0.035 Uiso 1 1 d R . . H3D H -0.0590 0.3436 0.7837 0.035 Uiso 1 1 d R . . N4 N 0.2905(10) 0.2875(7) 0.9114(7) 0.0195(18) Uani 1 1 d . . . C1 C 0.3055(17) 0.5250(11) 0.8743(11) 0.039(3) Uani 1 1 d . . . H1B H 0.3618 0.5920 0.8914 0.047 Uiso 1 1 calc R . . H1C H 0.1750 0.5329 0.8948 0.047 Uiso 1 1 calc R . . C2 C 0.3627(14) 0.3926(10) 0.9425(11) 0.034(3) Uani 1 1 d . . . H2B H 0.3194 0.3770 1.0243 0.040 Uiso 1 1 calc R . . H2C H 0.4941 0.3889 0.9284 0.040 Uiso 1 1 calc R . . C3 C 0.5648(14) 0.1924(11) 0.8336(10) 0.032(3) Uani 1 1 d . . . H3B H 0.6369 0.2666 0.8272 0.038 Uiso 1 1 calc R . . H3C H 0.6412 0.1149 0.8470 0.038 Uiso 1 1 calc R . . C4 C 0.4072(14) 0.1702(11) 0.9329(10) 0.031(3) Uani 1 1 d . . . H4A H 0.3382 0.0936 0.9415 0.037 Uiso 1 1 calc R . . H4B H 0.4507 0.1538 1.0039 0.037 Uiso 1 1 calc R . . C5 C 0.0094(14) 0.1903(11) 0.9047(10) 0.034(3) Uani 1 1 d . . . H5A H 0.0661 0.1068 0.9058 0.041 Uiso 1 1 calc R . . H5B H -0.1176 0.1732 0.9405 0.041 Uiso 1 1 calc R . . C6 C 0.0988(13) 0.2486(11) 0.9729(10) 0.033(3) Uani 1 1 d . . . H6A H 0.0320 0.3254 0.9813 0.039 Uiso 1 1 calc R . . H6B H 0.0980 0.1844 1.0495 0.039 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 0.0189(2) 0.0377(3) 0.0372(3) -0.0167(2) -0.00530(19) 0.00049(17) Sb1 0.0209(3) 0.0231(3) 0.0193(4) -0.0062(3) -0.0052(3) 0.0003(3) Sb2 0.0141(3) 0.0187(3) 0.0243(4) -0.0099(3) -0.0052(3) 0.0024(2) Se1 0.0158(5) 0.0212(5) 0.0176(6) -0.0055(4) -0.0045(4) 0.0036(4) Se2 0.0234(5) 0.0211(5) 0.0220(6) -0.0051(4) -0.0103(4) 0.0013(4) Se3 0.0185(5) 0.0261(5) 0.0183(6) -0.0062(4) -0.0028(4) 0.0021(4) Se4 0.0125(5) 0.0273(5) 0.0541(8) -0.0225(5) 0.0003(5) 0.0003(4) Se5 0.0413(7) 0.0294(6) 0.0207(6) -0.0102(5) -0.0130(5) 0.0136(5) Mn1 0.0235(8) 0.0227(8) 0.0208(9) -0.0062(7) -0.0096(7) -0.0004(6) N1 0.047(6) 0.027(5) 0.025(6) -0.001(4) -0.012(5) -0.005(4) N2 0.024(5) 0.033(5) 0.032(6) -0.017(4) 0.003(4) 0.004(4) N3 0.022(5) 0.036(5) 0.031(6) -0.013(4) -0.010(4) 0.000(4) N4 0.020(4) 0.023(4) 0.017(5) -0.010(4) -0.003(4) 0.001(3) C1 0.055(8) 0.027(6) 0.042(8) -0.022(6) -0.007(6) -0.006(5) C2 0.024(6) 0.042(7) 0.051(9) -0.033(6) -0.012(5) 0.001(5) C3 0.026(6) 0.041(7) 0.039(8) -0.020(6) -0.022(5) 0.010(5) C4 0.030(6) 0.041(6) 0.022(7) -0.009(5) -0.010(5) 0.002(5) C5 0.023(6) 0.049(7) 0.030(7) -0.013(6) -0.002(5) -0.014(5) C6 0.025(6) 0.042(7) 0.026(7) -0.008(5) 0.002(5) -0.004(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 2.5740(10) . ? Hg1 Se4 2.5973(11) . ? Hg1 Se5 2.7266(11) . ? Hg1 Se1 2.8175(11) . ? Sb1 Se5 2.5515(13) . ? Sb1 Se2 2.5601(11) . ? Sb1 Se1 2.8006(11) . ? Sb2 Se4 2.5361(11) 2_556 ? Sb2 Se3 2.5754(12) 2_656 ? Sb2 Se1 2.5996(12) . ? Se2 Mn1 2.5960(19) . ? Se3 Sb2 2.5754(12) 2_656 ? Se4 Sb2 2.5361(11) 2_556 ? Mn1 N2 2.162(8) . ? Mn1 N1 2.191(8) . ? Mn1 N3 2.213(9) . ? Mn1 N4 2.362(8) . ? N1 C1 1.488(14) . ? N1 H1A 0.9048 . ? N1 H1D 0.9023 . ? N2 C3 1.475(13) . ? N2 H2A 0.8973 . ? N2 H2D 0.9150 . ? N3 C5 1.478(14) . ? N3 H3A 0.9095 . ? N3 H3D 0.9020 . ? N4 C4 1.473(12) . ? N4 C2 1.493(11) . ? N4 C6 1.502(12) . ? C1 C2 1.478(15) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.499(15) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.505(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 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 Se4 115.00(3) . . ? Se3 Hg1 Se5 127.34(4) . . ? Se4 Hg1 Se5 107.67(4) . . ? Se3 Hg1 Se1 103.23(3) . . ? Se4 Hg1 Se1 110.12(4) . . ? Se5 Hg1 Se1 89.02(3) . . ? Se5 Sb1 Se2 98.89(4) . . ? Se5 Sb1 Se1 93.03(4) . . ? Se2 Sb1 Se1 88.74(3) . . ? Se4 Sb2 Se3 97.31(4) 2_556 2_656 ? Se4 Sb2 Se1 95.49(4) 2_556 . ? Se3 Sb2 Se1 95.45(4) 2_656 . ? Sb2 Se1 Sb1 103.26(4) . . ? Sb2 Se1 Hg1 97.55(3) . . ? Sb1 Se1 Hg1 80.93(3) . . ? Sb1 Se2 Mn1 99.87(5) . . ? Hg1 Se3 Sb2 96.77(4) . 2_656 ? Sb2 Se4 Hg1 103.17(4) 2_556 . ? Sb1 Se5 Hg1 87.32(4) . . ? N2 Mn1 N1 116.9(3) . . ? N2 Mn1 N3 109.0(3) . . ? N1 Mn1 N3 119.1(3) . . ? N2 Mn1 N4 77.5(3) . . ? N1 Mn1 N4 76.6(3) . . ? N3 Mn1 N4 76.6(3) . . ? N2 Mn1 Se2 113.3(3) . . ? N1 Mn1 Se2 97.4(2) . . ? N3 Mn1 Se2 99.0(2) . . ? N4 Mn1 Se2 169.14(19) . . ? C1 N1 Mn1 112.0(6) . . ? C1 N1 H1A 108.4 . . ? Mn1 N1 H1A 107.3 . . ? C1 N1 H1D 109.7 . . ? Mn1 N1 H1D 111.5 . . ? H1A N1 H1D 107.8 . . ? C3 N2 Mn1 109.2(6) . . ? C3 N2 H2A 109.5 . . ? Mn1 N2 H2A 102.3 . . ? C3 N2 H2D 114.1 . . ? Mn1 N2 H2D 112.5 . . ? H2A N2 H2D 108.6 . . ? C5 N3 Mn1 112.2(6) . . ? C5 N3 H3A 112.0 . . ? Mn1 N3 H3A 108.3 . . ? C5 N3 H3D 106.9 . . ? Mn1 N3 H3D 109.4 . . ? H3A N3 H3D 107.8 . . ? C4 N4 C2 111.5(7) . . ? C4 N4 C6 110.0(8) . . ? C2 N4 C6 112.7(8) . . ? C4 N4 Mn1 106.8(6) . . ? C2 N4 Mn1 107.3(6) . . ? C6 N4 Mn1 108.3(6) . . ? C2 C1 N1 109.4(9) . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1C 109.8 . . ? H1B C1 H1C 108.2 . . ? C1 C2 N4 111.3(9) . . ? C1 C2 H2B 109.4 . . ? N4 C2 H2B 109.4 . . ? C1 C2 H2C 109.4 . . ? N4 C2 H2C 109.4 . . ? H2B C2 H2C 108.0 . . ? N2 C3 C4 109.8(8) . . ? N2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? N2 C3 H3C 109.7 . . ? C4 C3 H3C 109.7 . . ? H3B C3 H3C 108.2 . . ? N4 C4 C3 109.5(9) . . ? N4 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N4 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 111.2(9) . . ? N3 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N4 C6 C5 109.6(9) . . ? N4 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N4 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se4 Sb2 Se1 Sb1 -20.21(5) 2_556 . . . ? Se3 Sb2 Se1 Sb1 -118.12(4) 2_656 . . . ? Se4 Sb2 Se1 Hg1 -102.62(4) 2_556 . . . ? Se3 Sb2 Se1 Hg1 159.47(3) 2_656 . . . ? Se5 Sb1 Se1 Sb2 -119.15(4) . . . . ? Se2 Sb1 Se1 Sb2 142.02(4) . . . . ? Se5 Sb1 Se1 Hg1 -23.46(4) . . . . ? Se2 Sb1 Se1 Hg1 -122.29(4) . . . . ? Se3 Hg1 Se1 Sb2 -107.59(4) . . . . ? Se4 Hg1 Se1 Sb2 15.67(4) . . . . ? Se5 Hg1 Se1 Sb2 124.15(4) . . . . ? Se3 Hg1 Se1 Sb1 150.10(3) . . . . ? Se4 Hg1 Se1 Sb1 -86.64(3) . . . . ? Se5 Hg1 Se1 Sb1 21.84(3) . . . . ? Se5 Sb1 Se2 Mn1 -154.76(5) . . . . ? Se1 Sb1 Se2 Mn1 -61.89(5) . . . . ? Se4 Hg1 Se3 Sb2 -115.44(4) . . . 2_656 ? Se5 Hg1 Se3 Sb2 103.58(5) . . . 2_656 ? Se1 Hg1 Se3 Sb2 4.53(4) . . . 2_656 ? Se3 Hg1 Se4 Sb2 -173.50(4) . . . 2_556 ? Se5 Hg1 Se4 Sb2 -25.19(6) . . . 2_556 ? Se1 Hg1 Se4 Sb2 70.41(5) . . . 2_556 ? Se2 Sb1 Se5 Hg1 113.19(3) . . . . ? Se1 Sb1 Se5 Hg1 24.00(4) . . . . ? Se3 Hg1 Se5 Sb1 -129.76(4) . . . . ? Se4 Hg1 Se5 Sb1 87.02(4) . . . . ? Se1 Hg1 Se5 Sb1 -23.81(4) . . . . ? Sb1 Se2 Mn1 N2 76.8(3) . . . . ? Sb1 Se2 Mn1 N1 -159.7(3) . . . . ? Sb1 Se2 Mn1 N3 -38.5(2) . . . . ? Sb1 Se2 Mn1 N4 -103.7(10) . . . . ? N2 Mn1 N1 C1 -86.8(8) . . . . ? N3 Mn1 N1 C1 47.6(8) . . . . ? N4 Mn1 N1 C1 -18.5(7) . . . . ? Se2 Mn1 N1 C1 152.3(7) . . . . ? N1 Mn1 N2 C3 45.2(8) . . . . ? N3 Mn1 N2 C3 -93.5(7) . . . . ? N4 Mn1 N2 C3 -22.6(7) . . . . ? Se2 Mn1 N2 C3 157.4(6) . . . . ? N2 Mn1 N3 C5 56.2(7) . . . . ? N1 Mn1 N3 C5 -81.4(7) . . . . ? N4 Mn1 N3 C5 -15.3(6) . . . . ? Se2 Mn1 N3 C5 174.8(6) . . . . ? N2 Mn1 N4 C4 -7.1(6) . . . . ? N1 Mn1 N4 C4 -129.0(6) . . . . ? N3 Mn1 N4 C4 106.1(6) . . . . ? Se2 Mn1 N4 C4 173.3(8) . . . . ? N2 Mn1 N4 C2 112.4(6) . . . . ? N1 Mn1 N4 C2 -9.5(6) . . . . ? N3 Mn1 N4 C2 -134.3(6) . . . . ? Se2 Mn1 N4 C2 -67.1(13) . . . . ? N2 Mn1 N4 C6 -125.6(6) . . . . ? N1 Mn1 N4 C6 112.5(6) . . . . ? N3 Mn1 N4 C6 -12.3(6) . . . . ? Se2 Mn1 N4 C6 54.8(13) . . . . ? Mn1 N1 C1 C2 45.0(11) . . . . ? N1 C1 C2 N4 -54.9(12) . . . . ? C4 N4 C2 C1 153.1(9) . . . . ? C6 N4 C2 C1 -82.5(11) . . . . ? Mn1 N4 C2 C1 36.6(10) . . . . ? Mn1 N2 C3 C4 50.6(10) . . . . ? C2 N4 C4 C3 -81.5(10) . . . . ? C6 N4 C4 C3 152.7(8) . . . . ? Mn1 N4 C4 C3 35.3(9) . . . . ? N2 C3 C4 N4 -58.6(11) . . . . ? Mn1 N3 C5 C6 41.9(10) . . . . ? C4 N4 C6 C5 -78.8(11) . . . . ? C2 N4 C6 C5 156.1(9) . . . . ? Mn1 N4 C6 C5 37.6(9) . . . . ? N3 C5 C6 N4 -53.6(11) . . . . ? 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 H1D Se5 0.90 2.89 3.736(9) 156.2 2_666 N2 H2A Se2 0.90 2.88 3.651(9) 145.5 2_666 N2 H2D Se1 0.92 2.87 3.455(9) 122.7 . N2 H2D Se3 0.92 2.79 3.618(9) 151.9 2_656 N3 H3A Se4 0.91 2.78 3.614(8) 153.0 2_556 N3 H3D Se5 0.90 2.81 3.634(8) 151.8 2_566 C1 H1B Se3 0.97 2.97 3.689(10) 132.3 2_666 C2 H2B Se5 0.97 2.93 3.878(12) 166.8 1_556 C3 H3C Se4 0.97 2.87 3.599(10) 132.8 2_656 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.051 _refine_diff_density_min -2.878 _refine_diff_density_rms 0.325 data_compound-3-KW3-36I _database_code_depnum_ccdc_archive 'CCDC 862157' #TrackingRef 'compound 3-kw3-36i.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Fe Hg N4 Sb2 Se5' _chemical_formula_sum 'C6 H18 Fe Hg N4 Sb2 Se5' _chemical_formula_weight 1040.98 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' Fe Fe 0.3463 0.8444 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 '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 7.5282(4) _cell_length_b 10.7335(6) _cell_length_c 12.5982(8) _cell_angle_alpha 69.494(5) _cell_angle_beta 78.655(5) _cell_angle_gamma 86.608(4) _cell_volume 934.80(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2872 _cell_measurement_theta_min 2.7542 _cell_measurement_theta_max 29.0142 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 21.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34673 _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 8015 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.75 _reflns_number_total 3943 _reflns_number_gt 3139 _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^)+(0.0206P)^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 3943 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.33269(5) 0.15696(4) 0.28589(3) 0.03037(11) Uani 1 1 d . . . Sb1 Sb 0.07027(8) 0.32529(6) 0.47069(5) 0.02252(15) Uani 1 1 d . . . Sb2 Sb 0.20302(7) -0.07715(5) 0.62589(5) 0.01964(14) Uani 1 1 d . . . Se1 Se 0.36260(11) 0.15006(8) 0.50618(7) 0.0199(2) Uani 1 1 d . . . Se2 Se 0.25148(12) 0.49229(9) 0.51166(8) 0.0237(2) Uani 1 1 d . . . Se3 Se 0.65726(11) 0.11376(9) 0.19480(8) 0.0231(2) Uani 1 1 d . . . Se4 Se 0.09506(11) -0.01923(9) 0.30549(10) 0.0312(3) Uani 1 1 d . . . Se5 Se 0.17048(13) 0.39776(9) 0.25147(8) 0.0311(2) Uani 1 1 d . . . Fe1 Fe 0.28316(16) 0.37068(12) 0.71963(11) 0.0209(3) Uani 1 1 d . . . N1 N 0.3402(11) 0.5429(7) 0.7530(7) 0.036(2) Uani 1 1 d . . . H1A H 0.2767 0.6115 0.7137 0.043 Uiso 1 1 d R . . H1D H 0.4590 0.5643 0.7286 0.043 Uiso 1 1 d R . . N2 N 0.4931(9) 0.2319(7) 0.7208(6) 0.0277(18) Uani 1 1 d . . . H2A H 0.5817 0.2701 0.6601 0.033 Uiso 1 1 d R . . H2D H 0.4531 0.1585 0.7124 0.033 Uiso 1 1 d R . . N3 N 0.0219(9) 0.2784(7) 0.7877(6) 0.0253(18) Uani 1 1 d . . . H3A H -0.0023 0.2365 0.7410 0.030 Uiso 1 1 d R . . H3D H -0.0620 0.3418 0.7879 0.030 Uiso 1 1 d R . . N4 N 0.2865(9) 0.2853(6) 0.9124(6) 0.0200(16) Uani 1 1 d . . . C1 C 0.2918(14) 0.5243(9) 0.8770(9) 0.039(3) Uani 1 1 d . . . H1B H 0.1615 0.5289 0.8996 0.046 Uiso 1 1 calc R . . H1C H 0.3474 0.5939 0.8923 0.046 Uiso 1 1 calc R . . C2 C 0.3579(12) 0.3907(8) 0.9446(8) 0.031(2) Uani 1 1 d . . . H2B H 0.3175 0.3734 1.0265 0.037 Uiso 1 1 calc R . . H2C H 0.4893 0.3902 0.9286 0.037 Uiso 1 1 calc R . . C3 C 0.5637(12) 0.1965(10) 0.8297(8) 0.032(2) Uani 1 1 d . . . H3B H 0.6376 0.2690 0.8270 0.039 Uiso 1 1 calc R . . H3C H 0.6386 0.1181 0.8393 0.039 Uiso 1 1 calc R . . C4 C 0.4080(12) 0.1701(9) 0.9288(8) 0.030(2) Uani 1 1 d . . . H4A H 0.3410 0.0924 0.9354 0.036 Uiso 1 1 calc R . . H4B H 0.4531 0.1516 0.9997 0.036 Uiso 1 1 calc R . . C5 C 0.0074(12) 0.1859(9) 0.9073(8) 0.033(2) Uani 1 1 d . . . H5A H 0.0636 0.1023 0.9071 0.039 Uiso 1 1 calc R . . H5B H -0.1194 0.1683 0.9428 0.039 Uiso 1 1 calc R . . C6 C 0.0983(11) 0.2432(9) 0.9763(8) 0.029(2) Uani 1 1 d . . . H6A H 0.0310 0.3191 0.9873 0.035 Uiso 1 1 calc R . . H6B H 0.1019 0.1770 1.0516 0.035 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 0.02180(19) 0.0371(2) 0.0339(2) -0.01556(19) -0.00340(18) 0.00110(16) Sb1 0.0239(3) 0.0233(3) 0.0188(3) -0.0059(3) -0.0031(3) 0.0005(2) Sb2 0.0177(3) 0.0190(3) 0.0237(3) -0.0095(3) -0.0039(3) 0.0025(2) Se1 0.0196(4) 0.0214(5) 0.0170(5) -0.0051(4) -0.0036(4) 0.0036(3) Se2 0.0256(5) 0.0233(5) 0.0219(5) -0.0057(4) -0.0085(4) 0.0019(4) Se3 0.0218(4) 0.0278(5) 0.0167(5) -0.0056(4) -0.0012(4) 0.0023(4) Se4 0.0162(4) 0.0287(5) 0.0514(7) -0.0219(5) 0.0024(5) 0.0002(4) Se5 0.0442(6) 0.0298(5) 0.0183(5) -0.0080(4) -0.0084(5) 0.0137(4) Fe1 0.0214(6) 0.0205(7) 0.0200(7) -0.0043(6) -0.0061(6) -0.0016(5) N1 0.053(5) 0.017(4) 0.041(6) -0.007(4) -0.022(5) -0.005(4) N2 0.030(4) 0.035(5) 0.019(4) -0.010(4) -0.003(4) -0.001(3) N3 0.018(4) 0.033(4) 0.022(5) -0.006(4) -0.002(3) -0.004(3) N4 0.018(4) 0.020(4) 0.023(4) -0.012(3) 0.003(3) -0.001(3) C1 0.061(7) 0.025(5) 0.041(7) -0.023(5) -0.017(6) 0.005(5) C2 0.037(5) 0.029(5) 0.033(6) -0.015(5) -0.009(5) 0.000(4) C3 0.026(5) 0.043(6) 0.034(6) -0.019(5) -0.010(5) 0.009(4) C4 0.038(6) 0.037(6) 0.016(5) -0.011(4) -0.004(5) 0.001(4) C5 0.031(5) 0.045(6) 0.018(5) -0.004(5) -0.001(5) -0.017(5) C6 0.025(5) 0.043(6) 0.017(5) -0.008(4) -0.005(4) -0.003(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 Hg1 Se3 2.5765(9) . ? Hg1 Se4 2.5956(10) . ? Hg1 Se5 2.7219(10) . ? Hg1 Se1 2.8032(10) . ? Sb1 Se5 2.5586(11) . ? Sb1 Se2 2.5602(11) . ? Sb1 Se1 2.8087(10) . ? Sb1 Se2 3.0467(10) 2_566 ? Sb2 Se4 2.5380(10) 2_556 ? Sb2 Se3 2.5745(11) 2_656 ? Sb2 Se1 2.5927(10) . ? Se2 Fe1 2.5374(15) . ? Se2 Sb1 3.0467(10) 2_566 ? Se3 Sb2 2.5745(11) 2_656 ? Se4 Sb2 2.5380(10) 2_556 ? Fe1 N2 2.105(7) . ? Fe1 N3 2.135(7) . ? Fe1 N1 2.118(7) . ? Fe1 N4 2.280(7) . ? N1 C1 1.475(12) . ? N1 H1A 0.9012 . ? N1 H1D 0.9022 . ? N2 C3 1.486(11) . ? N2 H2A 0.9002 . ? N2 H2D 0.9062 . ? N3 C5 1.472(11) . ? N3 H3A 0.9043 . ? N3 H3D 0.9004 . ? N4 C4 1.474(10) . ? N4 C6 1.494(10) . ? N4 C2 1.488(10) . ? C1 C2 1.502(12) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.492(12) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.504(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 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 Se4 114.37(3) . . ? Se3 Hg1 Se5 126.58(3) . . ? Se4 Hg1 Se5 109.37(3) . . ? Se3 Hg1 Se1 104.06(3) . . ? Se4 Hg1 Se1 109.31(3) . . ? Se5 Hg1 Se1 88.44(3) . . ? Se5 Sb1 Se2 99.82(4) . . ? Se5 Sb1 Se1 91.66(3) . . ? Se2 Sb1 Se1 88.19(3) . . ? Se5 Sb1 Se2 100.55(3) . 2_566 ? Se2 Sb1 Se2 86.11(3) . 2_566 ? Se1 Sb1 Se2 167.24(3) . 2_566 ? Se4 Sb2 Se3 97.18(4) 2_556 2_656 ? Se4 Sb2 Se1 95.80(3) 2_556 . ? Se3 Sb2 Se1 95.32(3) 2_656 . ? Sb2 Se1 Hg1 98.46(3) . . ? Sb2 Se1 Sb1 102.73(3) . . ? Hg1 Se1 Sb1 81.07(3) . . ? Fe1 Se2 Sb1 102.40(4) . . ? Fe1 Se2 Sb1 104.06(4) . 2_566 ? Sb1 Se2 Sb1 93.89(3) . 2_566 ? Sb2 Se3 Hg1 96.18(3) 2_656 . ? Sb2 Se4 Hg1 103.31(3) 2_556 . ? Sb1 Se5 Hg1 87.31(3) . . ? N2 Fe1 N3 112.7(3) . . ? N2 Fe1 N1 116.8(3) . . ? N3 Fe1 N1 119.6(3) . . ? N2 Fe1 N4 80.0(3) . . ? N3 Fe1 N4 78.2(3) . . ? N1 Fe1 N4 78.5(3) . . ? N2 Fe1 Se2 108.1(2) . . ? N3 Fe1 Se2 99.9(2) . . ? N1 Fe1 Se2 95.7(2) . . ? N4 Fe1 Se2 171.69(17) . . ? C1 N1 Fe1 112.0(6) . . ? C1 N1 H1A 108.9 . . ? Fe1 N1 H1A 109.0 . . ? C1 N1 H1D 108.5 . . ? Fe1 N1 H1D 110.4 . . ? H1A N1 H1D 107.9 . . ? C3 N2 Fe1 109.7(5) . . ? C3 N2 H2A 109.8 . . ? Fe1 N2 H2A 107.7 . . ? C3 N2 H2D 110.9 . . ? Fe1 N2 H2D 110.4 . . ? H2A N2 H2D 108.2 . . ? C5 N3 Fe1 112.2(5) . . ? C5 N3 H3A 111.1 . . ? Fe1 N3 H3A 109.0 . . ? C5 N3 H3D 107.5 . . ? Fe1 N3 H3D 109.0 . . ? H3A N3 H3D 107.9 . . ? C4 N4 C6 110.9(7) . . ? C4 N4 C2 111.4(7) . . ? C6 N4 C2 111.9(7) . . ? C4 N4 Fe1 106.0(5) . . ? C6 N4 Fe1 108.8(5) . . ? C2 N4 Fe1 107.6(5) . . ? N1 C1 C2 108.6(7) . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? N1 C1 H1C 110.0 . . ? C2 C1 H1C 110.0 . . ? H1B C1 H1C 108.3 . . ? C1 C2 N4 109.8(7) . . ? C1 C2 H2B 109.7 . . ? N4 C2 H2B 109.7 . . ? C1 C2 H2C 109.7 . . ? N4 C2 H2C 109.7 . . ? H2B C2 H2C 108.2 . . ? N2 C3 C4 109.1(7) . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? N2 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? H3B C3 H3C 108.3 . . ? N4 C4 C3 110.7(7) . . ? N4 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 110.8(7) . . ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N4 C6 C5 108.5(7) . . ? N4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se4 Sb2 Se1 Hg1 -102.63(4) 2_556 . . . ? Se3 Sb2 Se1 Hg1 159.58(3) 2_656 . . . ? Se4 Sb2 Se1 Sb1 -19.95(4) 2_556 . . . ? Se3 Sb2 Se1 Sb1 -117.74(3) 2_656 . . . ? Se3 Hg1 Se1 Sb2 -107.10(3) . . . . ? Se4 Hg1 Se1 Sb2 15.48(4) . . . . ? Se5 Hg1 Se1 Sb2 125.48(3) . . . . ? Se3 Hg1 Se1 Sb1 151.24(3) . . . . ? Se4 Hg1 Se1 Sb1 -86.19(3) . . . . ? Se5 Hg1 Se1 Sb1 23.81(3) . . . . ? Se5 Sb1 Se1 Sb2 -122.17(4) . . . . ? Se2 Sb1 Se1 Sb2 138.06(4) . . . . ? Se2 Sb1 Se1 Sb2 74.60(16) 2_566 . . . ? Se5 Sb1 Se1 Hg1 -25.44(3) . . . . ? Se2 Sb1 Se1 Hg1 -125.21(3) . . . . ? Se2 Sb1 Se1 Hg1 171.33(15) 2_566 . . . ? Se5 Sb1 Se2 Fe1 -154.63(4) . . . . ? Se1 Sb1 Se2 Fe1 -63.25(4) . . . . ? Se2 Sb1 Se2 Fe1 105.33(4) 2_566 . . . ? Se5 Sb1 Se2 Sb1 100.05(3) . . . 2_566 ? Se1 Sb1 Se2 Sb1 -168.58(3) . . . 2_566 ? Se2 Sb1 Se2 Sb1 0.0 2_566 . . 2_566 ? Se4 Hg1 Se3 Sb2 -115.81(4) . . . 2_656 ? Se5 Hg1 Se3 Sb2 102.06(4) . . . 2_656 ? Se1 Hg1 Se3 Sb2 3.38(4) . . . 2_656 ? Se3 Hg1 Se4 Sb2 -173.29(4) . . . 2_556 ? Se5 Hg1 Se4 Sb2 -24.79(5) . . . 2_556 ? Se1 Hg1 Se4 Sb2 70.52(4) . . . 2_556 ? Se2 Sb1 Se5 Hg1 114.39(3) . . . . ? Se1 Sb1 Se5 Hg1 25.94(3) . . . . ? Se2 Sb1 Se5 Hg1 -157.77(3) 2_566 . . . ? Se3 Hg1 Se5 Sb1 -132.41(4) . . . . ? Se4 Hg1 Se5 Sb1 83.94(4) . . . . ? Se1 Hg1 Se5 Sb1 -26.00(3) . . . . ? Sb1 Se2 Fe1 N2 79.5(2) . . . . ? Sb1 Se2 Fe1 N2 176.7(2) 2_566 . . . ? Sb1 Se2 Fe1 N3 -38.5(2) . . . . ? Sb1 Se2 Fe1 N3 58.8(2) 2_566 . . . ? Sb1 Se2 Fe1 N1 -159.9(2) . . . . ? Sb1 Se2 Fe1 N1 -62.6(2) 2_566 . . . ? Sb1 Se2 Fe1 N4 -114.9(12) . . . . ? Sb1 Se2 Fe1 N4 -17.7(12) 2_566 . . . ? N2 Fe1 N1 C1 -91.1(7) . . . . ? N3 Fe1 N1 C1 50.6(7) . . . . ? N4 Fe1 N1 C1 -18.6(6) . . . . ? Se2 Fe1 N1 C1 155.4(6) . . . . ? N3 Fe1 N2 C3 -92.1(6) . . . . ? N1 Fe1 N2 C3 52.2(7) . . . . ? N4 Fe1 N2 C3 -19.4(6) . . . . ? Se2 Fe1 N2 C3 158.5(5) . . . . ? N2 Fe1 N3 C5 58.7(6) . . . . ? N1 Fe1 N3 C5 -84.4(6) . . . . ? N4 Fe1 N3 C5 -15.0(6) . . . . ? Se2 Fe1 N3 C5 173.2(5) . . . . ? N2 Fe1 N4 C4 -9.1(5) . . . . ? N3 Fe1 N4 C4 106.7(5) . . . . ? N1 Fe1 N4 C4 -129.4(6) . . . . ? Se2 Fe1 N4 C4 -175.2(10) . . . . ? N2 Fe1 N4 C6 -128.4(6) . . . . ? N3 Fe1 N4 C6 -12.6(5) . . . . ? N1 Fe1 N4 C6 111.3(6) . . . . ? Se2 Fe1 N4 C6 65.5(15) . . . . ? N2 Fe1 N4 C2 110.2(5) . . . . ? N3 Fe1 N4 C2 -133.9(5) . . . . ? N1 Fe1 N4 C2 -10.0(5) . . . . ? Se2 Fe1 N4 C2 -55.9(15) . . . . ? Fe1 N1 C1 C2 44.7(9) . . . . ? N1 C1 C2 N4 -54.2(10) . . . . ? C4 N4 C2 C1 152.4(8) . . . . ? C6 N4 C2 C1 -82.8(9) . . . . ? Fe1 N4 C2 C1 36.6(8) . . . . ? Fe1 N2 C3 C4 45.8(9) . . . . ? C6 N4 C4 C3 154.4(8) . . . . ? C2 N4 C4 C3 -80.3(9) . . . . ? Fe1 N4 C4 C3 36.5(8) . . . . ? N2 C3 C4 N4 -56.1(10) . . . . ? Fe1 N3 C5 C6 41.2(9) . . . . ? C4 N4 C6 C5 -79.1(9) . . . . ? C2 N4 C6 C5 155.8(7) . . . . ? Fe1 N4 C6 C5 37.1(8) . . . . ? N3 C5 C6 N4 -52.1(10) . . . . ? 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 H1D Se5 0.90 2.91 3.762(8) 157.1 2_666 N2 H2A Se2 0.90 2.86 3.664(7) 148.7 2_666 N2 H2D Se1 0.91 2.84 3.443(7) 124.9 . N2 H2D Se3 0.91 2.85 3.665(8) 150.8 2_656 N3 H3A Se4 0.90 2.75 3.589(8) 154.0 2_556 N3 H3D Se5 0.90 2.77 3.592(7) 153.3 2_566 C1 H1C Se3 0.97 2.94 3.693(9) 135.4 2_666 C2 H2B Se5 0.97 2.93 3.872(10) 164.4 1_556 C3 H3C Se4 0.97 2.85 3.619(8) 136.5 2_656 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.446 _refine_diff_density_min -2.152 _refine_diff_density_rms 0.257 data_compound-4-KW3-36H _database_code_depnum_ccdc_archive 'CCDC 862158' #TrackingRef 'compound 4-kw3-36h.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Co Hg N4 Sb2 Se5' _chemical_formula_sum 'C6 H18 Co Hg N4 Sb2 Se5' _chemical_formula_weight 1044.06 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' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 '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 7.5076(4) _cell_length_b 10.6782(6) _cell_length_c 12.5866(9) _cell_angle_alpha 69.630(6) _cell_angle_beta 78.974(5) _cell_angle_gamma 86.992(4) _cell_volume 928.37(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3199 _cell_measurement_theta_min 2.7589 _cell_measurement_theta_max 29.1865 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 922 _exptl_absorpt_coefficient_mu 21.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.24965 _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 7816 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.74 _reflns_number_total 3905 _reflns_number_gt 3296 _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^)+(0.0193P)^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 SHELXL _refine_ls_extinction_coef 0.00389(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3905 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.33460(4) 0.15792(3) 0.28603(3) 0.02568(11) Uani 1 1 d . . . Sb1 Sb 0.07079(7) 0.32509(5) 0.47085(5) 0.01981(14) Uani 1 1 d . . . Sb2 Sb 0.20243(6) -0.07699(5) 0.62574(5) 0.01759(14) Uani 1 1 d . . . Se1 Se 0.36461(10) 0.15048(7) 0.50670(7) 0.01720(18) Uani 1 1 d . . . Se2 Se 0.24843(10) 0.49152(7) 0.51796(7) 0.02039(19) Uani 1 1 d . . . Se3 Se 0.65828(10) 0.11309(7) 0.19467(7) 0.01997(19) Uani 1 1 d . . . Se4 Se 0.09484(10) -0.02018(8) 0.30668(9) 0.0281(2) Uani 1 1 d . . . Se5 Se 0.17652(12) 0.40109(8) 0.25226(7) 0.0276(2) Uani 1 1 d . . . Co1 Co 0.27718(13) 0.37085(10) 0.72321(9) 0.0179(2) Uani 1 1 d . . . N1 N 0.3334(10) 0.5417(6) 0.7568(6) 0.037(2) Uani 1 1 d . . . H1A H 0.2700 0.6103 0.7175 0.044 Uiso 1 1 d R . . H1D H 0.4522 0.5631 0.7324 0.044 Uiso 1 1 d R . . N2 N 0.4868(8) 0.2400(6) 0.7225(6) 0.0261(16) Uani 1 1 d . . . H2A H 0.5755 0.2783 0.6618 0.031 Uiso 1 1 d R . . H2D H 0.4469 0.1667 0.7141 0.031 Uiso 1 1 d R . . N3 N 0.0234(8) 0.2781(6) 0.7883(6) 0.0226(16) Uani 1 1 d . . . H3A H -0.0008 0.2362 0.7416 0.027 Uiso 1 1 d R . . H3D H -0.0605 0.3414 0.7884 0.027 Uiso 1 1 d R . . N4 N 0.2852(7) 0.2843(6) 0.9133(5) 0.0159(14) Uani 1 1 d . . . C1 C 0.2865(13) 0.5223(8) 0.8792(8) 0.037(2) Uani 1 1 d . . . H1B H 0.1559 0.5253 0.9020 0.044 Uiso 1 1 calc R . . H1C H 0.3409 0.5930 0.8947 0.044 Uiso 1 1 calc R . . C2 C 0.3540(11) 0.3907(7) 0.9464(7) 0.026(2) Uani 1 1 d . . . H2B H 0.4856 0.3917 0.9311 0.031 Uiso 1 1 calc R . . H2C H 0.3127 0.3729 1.0282 0.031 Uiso 1 1 calc R . . C3 C 0.5638(10) 0.2002(8) 0.8280(7) 0.027(2) Uani 1 1 d . . . H3B H 0.6393 0.2718 0.8267 0.032 Uiso 1 1 calc R . . H3C H 0.6380 0.1218 0.8337 0.032 Uiso 1 1 calc R . . C4 C 0.4076(10) 0.1695(7) 0.9299(7) 0.0212(18) Uani 1 1 d . . . H4A H 0.3416 0.0906 0.9365 0.025 Uiso 1 1 calc R . . H4B H 0.4541 0.1518 1.0004 0.025 Uiso 1 1 calc R . . C5 C 0.0077(11) 0.1817(8) 0.9074(8) 0.032(2) Uani 1 1 d . . . H5A H 0.0654 0.0985 0.9065 0.039 Uiso 1 1 calc R . . H5B H -0.1191 0.1628 0.9428 0.039 Uiso 1 1 calc R . . C6 C 0.0991(10) 0.2420(9) 0.9750(8) 0.030(2) Uani 1 1 d . . . H6A H 0.0312 0.3184 0.9847 0.036 Uiso 1 1 calc R . . H6B H 0.1022 0.1768 1.0509 0.036 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 0.01903(17) 0.0324(2) 0.0273(2) -0.01381(16) -0.00156(14) 0.00074(13) Sb1 0.0237(3) 0.0193(3) 0.0139(3) -0.0034(2) -0.0018(2) 0.0002(2) Sb2 0.0176(3) 0.0162(3) 0.0199(3) -0.0079(2) -0.0029(2) 0.0018(2) Se1 0.0191(4) 0.0183(4) 0.0126(4) -0.0039(3) -0.0027(3) 0.0029(3) Se2 0.0231(4) 0.0198(4) 0.0164(5) -0.0025(4) -0.0067(3) 0.0016(3) Se3 0.0196(4) 0.0238(4) 0.0134(4) -0.0049(4) 0.0005(3) 0.0032(3) Se4 0.0155(4) 0.0247(4) 0.0464(6) -0.0190(4) 0.0020(4) 0.0001(3) Se5 0.0428(5) 0.0244(4) 0.0143(5) -0.0058(4) -0.0067(4) 0.0125(4) Co1 0.0202(5) 0.0167(5) 0.0152(6) -0.0021(5) -0.0052(5) -0.0022(4) N1 0.060(5) 0.016(4) 0.030(5) 0.002(4) -0.017(4) -0.005(3) N2 0.024(3) 0.037(4) 0.018(4) -0.013(3) 0.001(3) -0.002(3) N3 0.018(3) 0.035(4) 0.018(4) -0.013(3) -0.006(3) 0.001(3) N4 0.017(3) 0.020(3) 0.011(3) -0.006(3) -0.002(3) -0.002(3) C1 0.062(6) 0.018(4) 0.032(6) -0.010(4) -0.011(5) 0.002(4) C2 0.037(5) 0.027(4) 0.024(5) -0.019(4) -0.010(4) 0.000(4) C3 0.026(4) 0.034(5) 0.027(5) -0.018(4) -0.012(4) 0.012(4) C4 0.026(4) 0.019(4) 0.015(4) -0.002(4) -0.003(4) 0.004(3) C5 0.030(4) 0.033(5) 0.026(5) 0.000(4) -0.001(4) -0.013(4) C6 0.026(4) 0.042(5) 0.023(5) -0.014(4) -0.003(4) 0.001(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 Hg1 Se3 2.5786(8) . ? Hg1 Se4 2.6001(8) . ? Hg1 Se5 2.7263(9) . ? Hg1 Se1 2.8028(9) . ? Sb1 Se5 2.5566(10) . ? Sb1 Se2 2.5639(9) . ? Sb1 Se1 2.8124(9) . ? Sb1 Se2 3.0279(9) 2_566 ? Sb2 Se4 2.5350(9) 2_556 ? Sb2 Se3 2.5703(10) 2_656 ? Sb2 Se1 2.5896(9) . ? Se2 Co1 2.4996(13) . ? Se2 Sb1 3.0279(9) 2_566 ? Se3 Sb2 2.5703(10) 2_656 ? Se4 Sb2 2.5350(9) 2_556 ? Co1 N2 2.050(6) . ? Co1 N3 2.078(6) . ? Co1 N1 2.090(7) . ? Co1 N4 2.256(6) . ? N1 C1 1.456(11) . ? N1 H1A 0.9000 . ? N1 H1D 0.9000 . ? N2 C3 1.466(10) . ? N2 H2A 0.9001 . ? N2 H2D 0.8999 . ? N3 C5 1.481(10) . ? N3 H3A 0.9001 . ? N3 H3D 0.8999 . ? N4 C4 1.473(9) . ? N4 C6 1.473(9) . ? N4 C2 1.484(9) . ? C1 C2 1.486(11) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.516(10) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.503(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 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 Se4 113.98(3) . . ? Se3 Hg1 Se5 126.51(3) . . ? Se4 Hg1 Se5 110.10(3) . . ? Se3 Hg1 Se1 104.53(3) . . ? Se4 Hg1 Se1 108.72(3) . . ? Se5 Hg1 Se1 88.09(3) . . ? Se5 Sb1 Se2 100.07(3) . . ? Se5 Sb1 Se1 91.33(3) . . ? Se2 Sb1 Se1 88.17(3) . . ? Se5 Sb1 Se2 99.48(3) . 2_566 ? Se2 Sb1 Se2 86.04(3) . 2_566 ? Se1 Sb1 Se2 168.48(3) . 2_566 ? Se4 Sb2 Se3 97.07(4) 2_556 2_656 ? Se4 Sb2 Se1 95.90(3) 2_556 . ? Se3 Sb2 Se1 95.19(3) 2_656 . ? Sb2 Se1 Hg1 98.59(3) . . ? Sb2 Se1 Sb1 102.13(3) . . ? Hg1 Se1 Sb1 80.92(2) . . ? Co1 Se2 Sb1 103.31(4) . . ? Co1 Se2 Sb1 105.11(4) . 2_566 ? Sb1 Se2 Sb1 93.96(3) . 2_566 ? Sb2 Se3 Hg1 95.62(3) 2_656 . ? Sb2 Se4 Hg1 103.31(3) 2_556 . ? Sb1 Se5 Hg1 87.16(3) . . ? N2 Co1 N3 113.7(3) . . ? N2 Co1 N1 115.6(3) . . ? N3 Co1 N1 120.2(3) . . ? N2 Co1 N4 79.5(2) . . ? N3 Co1 N4 79.0(2) . . ? N1 Co1 N4 78.8(2) . . ? N2 Co1 Se2 107.25(19) . . ? N3 Co1 Se2 100.35(18) . . ? N1 Co1 Se2 95.5(2) . . ? N4 Co1 Se2 172.70(16) . . ? C1 N1 Co1 111.8(5) . . ? C1 N1 H1A 109.3 . . ? Co1 N1 H1A 109.0 . . ? C1 N1 H1D 108.7 . . ? Co1 N1 H1D 109.9 . . ? H1A N1 H1D 108.0 . . ? C3 N2 Co1 112.9(5) . . ? C3 N2 H2A 108.5 . . ? Co1 N2 H2A 109.2 . . ? C3 N2 H2D 109.1 . . ? Co1 N2 H2D 109.1 . . ? H2A N2 H2D 107.9 . . ? C5 N3 Co1 113.1(5) . . ? C5 N3 H3A 109.7 . . ? Co1 N3 H3A 109.4 . . ? C5 N3 H3D 108.3 . . ? Co1 N3 H3D 108.4 . . ? H3A N3 H3D 107.9 . . ? C4 N4 C6 111.2(6) . . ? C4 N4 C2 111.8(6) . . ? C6 N4 C2 111.4(6) . . ? C4 N4 Co1 107.0(4) . . ? C6 N4 Co1 107.6(5) . . ? C2 N4 Co1 107.6(4) . . ? N1 C1 C2 109.3(7) . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? H1B C1 H1C 108.3 . . ? N4 C2 C1 109.5(7) . . ? N4 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? N4 C2 H2C 109.8 . . ? C1 C2 H2C 109.8 . . ? H2B C2 H2C 108.2 . . ? N2 C3 C4 107.9(6) . . ? N2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? N2 C3 H3C 110.1 . . ? C4 C3 H3C 110.1 . . ? H3B C3 H3C 108.4 . . ? N4 C4 C3 109.4(6) . . ? N4 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N4 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 108.3(6) . . ? N3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C5 109.4(7) . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se4 Sb2 Se1 Hg1 -102.57(3) 2_556 . . . ? Se3 Sb2 Se1 Hg1 159.76(3) 2_656 . . . ? Se4 Sb2 Se1 Sb1 -20.08(4) 2_556 . . . ? Se3 Sb2 Se1 Sb1 -117.75(3) 2_656 . . . ? Se3 Hg1 Se1 Sb2 -106.93(3) . . . . ? Se4 Hg1 Se1 Sb2 15.16(3) . . . . ? Se5 Hg1 Se1 Sb2 125.75(3) . . . . ? Se3 Hg1 Se1 Sb1 152.06(2) . . . . ? Se4 Hg1 Se1 Sb1 -85.85(3) . . . . ? Se5 Hg1 Se1 Sb1 24.74(2) . . . . ? Se5 Sb1 Se1 Sb2 -123.41(3) . . . . ? Se2 Sb1 Se1 Sb2 136.56(3) . . . . ? Se2 Sb1 Se1 Sb2 76.78(14) 2_566 . . . ? Se5 Sb1 Se1 Hg1 -26.49(3) . . . . ? Se2 Sb1 Se1 Hg1 -126.52(3) . . . . ? Se2 Sb1 Se1 Hg1 173.70(13) 2_566 . . . ? Se5 Sb1 Se2 Co1 -154.51(4) . . . . ? Se1 Sb1 Se2 Co1 -63.49(4) . . . . ? Se2 Sb1 Se2 Co1 106.55(4) 2_566 . . . ? Se5 Sb1 Se2 Sb1 98.93(3) . . . 2_566 ? Se1 Sb1 Se2 Sb1 -170.04(3) . . . 2_566 ? Se2 Sb1 Se2 Sb1 0.0 2_566 . . 2_566 ? Se4 Hg1 Se3 Sb2 -115.55(3) . . . 2_656 ? Se5 Hg1 Se3 Sb2 101.59(4) . . . 2_656 ? Se1 Hg1 Se3 Sb2 3.02(3) . . . 2_656 ? Se3 Hg1 Se4 Sb2 -173.05(3) . . . 2_556 ? Se5 Hg1 Se4 Sb2 -24.16(5) . . . 2_556 ? Se1 Hg1 Se4 Sb2 70.80(4) . . . 2_556 ? Se2 Sb1 Se5 Hg1 115.34(3) . . . . ? Se1 Sb1 Se5 Hg1 26.96(3) . . . . ? Se2 Sb1 Se5 Hg1 -157.04(3) 2_566 . . . ? Se3 Hg1 Se5 Sb1 -133.79(3) . . . . ? Se4 Hg1 Se5 Sb1 82.18(4) . . . . ? Se1 Hg1 Se5 Sb1 -27.07(3) . . . . ? Sb1 Se2 Co1 N2 80.39(19) . . . . ? Sb1 Se2 Co1 N2 178.29(19) 2_566 . . . ? Sb1 Se2 Co1 N3 -38.56(19) . . . . ? Sb1 Se2 Co1 N3 59.34(19) 2_566 . . . ? Sb1 Se2 Co1 N1 -160.6(2) . . . . ? Sb1 Se2 Co1 N1 -62.7(2) 2_566 . . . ? Sb1 Se2 Co1 N4 -122.5(11) . . . . ? Sb1 Se2 Co1 N4 -24.6(11) 2_566 . . . ? N2 Co1 N1 C1 -91.7(6) . . . . ? N3 Co1 N1 C1 50.8(7) . . . . ? N4 Co1 N1 C1 -19.3(6) . . . . ? Se2 Co1 N1 C1 156.2(6) . . . . ? N3 Co1 N2 C3 -91.7(5) . . . . ? N1 Co1 N2 C3 53.3(6) . . . . ? N4 Co1 N2 C3 -18.8(5) . . . . ? Se2 Co1 N2 C3 158.4(5) . . . . ? N2 Co1 N3 C5 57.7(6) . . . . ? N1 Co1 N3 C5 -85.5(6) . . . . ? N4 Co1 N3 C5 -15.5(6) . . . . ? Se2 Co1 N3 C5 171.9(5) . . . . ? N2 Co1 N4 C4 -10.4(4) . . . . ? N3 Co1 N4 C4 106.5(4) . . . . ? N1 Co1 N4 C4 -129.4(5) . . . . ? Se2 Co1 N4 C4 -168.2(9) . . . . ? N2 Co1 N4 C6 -130.0(5) . . . . ? N3 Co1 N4 C6 -13.1(5) . . . . ? N1 Co1 N4 C6 111.0(5) . . . . ? Se2 Co1 N4 C6 72.2(13) . . . . ? N2 Co1 N4 C2 109.9(5) . . . . ? N3 Co1 N4 C2 -133.2(5) . . . . ? N1 Co1 N4 C2 -9.1(5) . . . . ? Se2 Co1 N4 C2 -47.9(14) . . . . ? Co1 N1 C1 C2 45.3(8) . . . . ? C4 N4 C2 C1 152.5(7) . . . . ? C6 N4 C2 C1 -82.4(8) . . . . ? Co1 N4 C2 C1 35.3(7) . . . . ? N1 C1 C2 N4 -53.7(9) . . . . ? Co1 N2 C3 C4 44.4(7) . . . . ? C6 N4 C4 C3 153.7(7) . . . . ? C2 N4 C4 C3 -81.1(8) . . . . ? Co1 N4 C4 C3 36.5(7) . . . . ? N2 C3 C4 N4 -53.6(8) . . . . ? Co1 N3 C5 C6 41.5(8) . . . . ? C4 N4 C6 C5 -78.1(8) . . . . ? C2 N4 C6 C5 156.4(7) . . . . ? Co1 N4 C6 C5 38.8(8) . . . . ? N3 C5 C6 N4 -53.2(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 H1D Se5 0.90 2.88 3.735(7) 158.1 2_666 N2 H2A Se2 0.90 2.87 3.686(6) 151.5 2_666 N2 H2D Se1 0.90 2.86 3.462(7) 125.8 . N2 H2D Se3 0.90 2.89 3.709(6) 151.2 2_656 N3 H3A Se4 0.90 2.74 3.571(7) 154.3 2_556 N3 H3D Se5 0.90 2.74 3.576(6) 154.6 2_566 C1 H1C Se3 0.97 2.94 3.701(8) 136.0 2_666 C2 H2C Se5 0.97 2.92 3.864(9) 163.8 1_556 C3 H3C Se4 0.97 2.84 3.636(8) 139.8 2_656 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.014 _refine_diff_density_min -1.841 _refine_diff_density_rms 0.264