# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nanhai Singh' _publ_contact_author_email 'NANHAI SINGH@YAHOO.COM' _publ_section_title ; Syntheses, crystal, photoluminescence and electrochemical investigation of some new phenylmercury(II) dithiocarbamate complexes involving ferrocene ; loop_ _publ_author_name 'Nanhai Singh' 'Abhinav Kumar' 'Mary Mahon' 'K Molloy' 'Rajendra Prasad' # Attachment 'cif.txt' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 710233' #TrackingRef 'cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 149 _chemical_formula_moiety 'C25 H23 Fe Hg N S2' _chemical_formula_sum 'C25 H23 Fe Hg N S2' _chemical_formula_weight 658.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _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 13.2728(14) _cell_length_b 10.1535(11) _cell_length_c 33.692(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4540.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7879 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 25.99 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 7.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.054 _exptl_absorpt_correction_T_max 0.684 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24163 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4460 _reflns_number_gt 3153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0783P)^2^+26.2111P] 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 ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4460 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 C22 C 0.9893(9) 0.4883(11) 0.5569(4) 0.083(3) Uani 1 1 d . . . H001 H 1.0527 0.5263 0.5596 0.100 Uiso 1 1 calc R . . C23 C 0.9083(12) 0.5454(11) 0.5749(4) 0.087(3) Uani 1 1 d . . . H007 H 0.9160 0.6235 0.5890 0.105 Uiso 1 1 calc R . . C10 C 1.1904(10) -0.2770(14) 0.2582(4) 0.091(4) Uani 1 1 d . . . H008 H 1.1679 -0.2903 0.2324 0.110 Uiso 1 1 calc R . . C24 C 0.8146(10) 0.4865(12) 0.5721(3) 0.086(4) Uani 1 1 d . . . H123 H 0.7594 0.5245 0.5847 0.104 Uiso 1 1 calc R . . Hg Hg 0.86351(3) 0.14243(4) 0.499202(10) 0.0657(2) Uani 1 1 d . . . Fe Fe 1.12006(8) -0.16840(10) 0.29999(4) 0.0436(3) Uani 1 1 d . . . S2 S 1.01655(16) 0.0514(2) 0.44127(7) 0.0555(5) Uani 1 1 d . . . S1 S 0.80760(17) -0.0378(3) 0.45937(7) 0.0600(6) Uani 1 1 d . . . N N 0.9218(5) -0.1471(6) 0.40510(18) 0.0413(14) Uani 1 1 d . . . C20 C 0.8833(8) 0.3133(9) 0.5317(2) 0.058(2) Uani 1 1 d . . . C11 C 1.0150(6) -0.1781(8) 0.3830(2) 0.0476(18) Uani 1 1 d . . . H00A H 1.0227 -0.2730 0.3816 0.057 Uiso 1 1 calc R . . H00B H 1.0722 -0.1432 0.3974 0.057 Uiso 1 1 calc R . . C13 C 0.7505(6) -0.1699(7) 0.3737(2) 0.0433(17) Uani 1 1 d . . . C12 C 0.8346(6) -0.2321(8) 0.3973(2) 0.0481(19) Uani 1 1 d . . . H00C H 0.8074 -0.2612 0.4225 0.058 Uiso 1 1 calc R . . H00D H 0.8577 -0.3096 0.3832 0.058 Uiso 1 1 calc R . . C5 C 1.0664(6) -0.0070(8) 0.3294(3) 0.052(2) Uani 1 1 d . . . H006 H 1.1027 0.0498 0.3457 0.063 Uiso 1 1 calc R . . C19 C 0.9180(6) -0.0527(8) 0.4320(2) 0.0438(18) Uani 1 1 d . . . C1 C 1.0161(5) -0.1234(7) 0.3416(2) 0.0409(17) Uani 1 1 d . . . C2 C 0.9690(5) -0.1796(9) 0.3077(2) 0.0472(19) Uani 1 1 d . . . H011 H 0.9302 -0.2558 0.3073 0.057 Uiso 1 1 calc R . . C18 C 0.6571(7) -0.2280(10) 0.3746(3) 0.061(2) Uani 1 1 d . . . H013 H 0.6464 -0.3012 0.3906 0.073 Uiso 1 1 calc R . . C14 C 0.7652(6) -0.0607(8) 0.3497(2) 0.0479(18) Uani 1 1 d . . . H014 H 0.8283 -0.0212 0.3486 0.057 Uiso 1 1 calc R . . C3 C 0.9920(6) -0.0983(11) 0.2747(3) 0.066(3) Uani 1 1 d . . . H015 H 0.9712 -0.1121 0.2487 0.079 Uiso 1 1 calc R . . C15 C 0.6872(7) -0.0105(10) 0.3275(3) 0.062(2) Uani 1 1 d . . . H016 H 0.6978 0.0636 0.3118 0.075 Uiso 1 1 calc R . . C17 C 0.5786(7) -0.1781(11) 0.3518(3) 0.074(3) Uani 1 1 d . . . H020 H 0.5158 -0.2187 0.3524 0.089 Uiso 1 1 calc R . . C7 C 1.2695(6) -0.1892(10) 0.3109(3) 0.064(2) Uani 1 1 d . . . H022 H 1.3091 -0.1331 0.3262 0.077 Uiso 1 1 calc R . . C6 C 1.2521(7) -0.1792(11) 0.2701(3) 0.070(3) Uani 1 1 d . . . H024 H 1.2791 -0.1148 0.2536 0.084 Uiso 1 1 calc R . . C16 C 0.5936(8) -0.0686(12) 0.3283(3) 0.073(3) Uani 1 1 d . . . H027 H 0.5411 -0.0344 0.3132 0.088 Uiso 1 1 calc R . . C9 C 1.1658(9) -0.3548(10) 0.2908(6) 0.101(5) Uani 1 1 d . . . H029 H 1.1244 -0.4288 0.2907 0.121 Uiso 1 1 calc R . . C21 C 0.9778(9) 0.3710(11) 0.5341(3) 0.076(3) Uani 1 1 d . . . H033 H 1.0327 0.3339 0.5210 0.092 Uiso 1 1 calc R . . C8 C 1.2163(8) -0.2994(11) 0.3245(4) 0.085(4) Uani 1 1 d . . . H034 H 1.2141 -0.3306 0.3505 0.102 Uiso 1 1 calc R . . C4 C 1.0517(7) 0.0069(9) 0.2883(3) 0.059(2) Uani 1 1 d . . . H036 H 1.0773 0.0745 0.2726 0.070 Uiso 1 1 calc R . . C25 C 0.8026(8) 0.3704(10) 0.5505(3) 0.070(3) Uani 1 1 d . . . H042 H 0.7394 0.3313 0.5489 0.084 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 C22 0.089(8) 0.089(8) 0.072(8) 0.025(6) -0.009(6) -0.013(7) C23 0.127(11) 0.066(6) 0.069(7) -0.005(6) -0.021(8) -0.002(7) C10 0.080(8) 0.099(9) 0.095(9) -0.044(8) 0.010(7) 0.017(7) C24 0.102(9) 0.093(8) 0.065(7) -0.017(6) -0.015(6) 0.037(7) Hg 0.0796(3) 0.0766(3) 0.0410(3) -0.00733(17) -0.00745(17) 0.01277(19) Fe 0.0365(6) 0.0441(6) 0.0503(7) 0.0031(5) 0.0063(5) 0.0025(5) S2 0.0473(12) 0.0665(13) 0.0526(13) -0.0022(11) -0.0078(10) -0.0051(10) S1 0.0493(12) 0.0899(16) 0.0407(12) -0.0110(11) 0.0067(10) -0.0053(11) N 0.039(3) 0.053(4) 0.032(3) 0.003(3) -0.002(3) 0.002(3) C20 0.081(7) 0.060(5) 0.032(4) 0.001(4) -0.019(4) 0.017(5) C11 0.043(4) 0.053(4) 0.046(5) 0.003(4) 0.004(4) 0.009(4) C13 0.047(4) 0.047(4) 0.036(4) -0.008(3) -0.003(3) -0.002(3) C12 0.052(5) 0.051(4) 0.041(5) 0.003(4) 0.001(4) -0.003(4) C5 0.047(5) 0.047(4) 0.064(6) 0.003(4) 0.007(4) 0.006(4) C19 0.043(4) 0.056(4) 0.033(4) 0.004(4) -0.001(3) 0.004(4) C1 0.036(4) 0.047(4) 0.039(4) 0.003(3) 0.003(3) 0.004(3) C2 0.034(4) 0.072(5) 0.035(4) 0.004(4) 0.005(3) -0.008(4) C18 0.051(5) 0.065(6) 0.068(6) -0.011(5) 0.007(4) -0.007(4) C14 0.047(4) 0.053(4) 0.044(4) 0.000(4) 0.001(4) 0.003(4) C3 0.039(4) 0.111(8) 0.047(5) 0.018(5) 0.001(4) 0.014(5) C15 0.067(6) 0.069(6) 0.050(5) -0.004(4) -0.002(5) 0.021(5) C17 0.044(5) 0.090(7) 0.090(8) -0.030(7) -0.002(5) -0.012(5) C7 0.041(5) 0.077(6) 0.075(7) 0.002(5) -0.003(4) 0.015(4) C6 0.047(5) 0.082(7) 0.082(7) 0.003(6) 0.028(5) 0.010(5) C16 0.059(6) 0.097(8) 0.063(6) -0.025(6) -0.019(5) 0.017(6) C9 0.060(7) 0.046(6) 0.197(17) -0.016(8) 0.011(9) 0.006(5) C21 0.080(7) 0.090(8) 0.059(7) 0.032(6) -0.005(5) 0.012(6) C8 0.069(7) 0.080(7) 0.105(9) 0.047(7) 0.024(7) 0.042(6) C4 0.053(5) 0.055(5) 0.067(6) 0.022(4) 0.021(4) 0.015(4) C25 0.071(7) 0.080(7) 0.059(6) -0.001(5) -0.020(5) 0.013(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 C22 C23 1.363(16) . ? C22 C21 1.427(15) . ? C22 H001 0.9300 . ? C23 C24 1.383(17) . ? C23 H007 0.9300 . ? C10 C6 1.348(15) . ? C10 C9 1.391(19) . ? C10 Fe 2.017(10) . ? C10 H008 0.9300 . ? C24 C25 1.394(15) . ? C24 H123 0.9300 . ? Hg C20 2.068(9) . ? Hg S1 2.388(2) . ? Hg S2 2.965(2) . ? Fe C9 2.012(10) . ? Fe C1 2.019(7) . ? Fe C6 2.024(9) . ? Fe C8 2.021(9) . ? Fe C2 2.025(7) . ? Fe C7 2.029(9) . ? Fe C3 2.030(8) . ? Fe C4 2.036(8) . ? Fe C5 2.043(8) . ? S2 C19 1.711(8) . ? S1 C19 1.738(8) . ? N C19 1.320(10) . ? N C12 1.468(10) . ? N C11 1.478(9) . ? C20 C25 1.373(14) . ? C20 C21 1.387(14) . ? C11 C1 1.501(10) . ? C11 H00A 0.9700 . ? C11 H00B 0.9700 . ? C13 C18 1.372(11) . ? C13 C14 1.386(11) . ? C13 C12 1.509(11) . ? C12 H00C 0.9700 . ? C12 H00D 0.9700 . ? C5 C4 1.406(12) . ? C5 C1 1.418(11) . ? C5 H006 0.9300 . ? C1 C2 1.420(11) . ? C2 C3 1.418(12) . ? C2 H011 0.9300 . ? C18 C17 1.390(14) . ? C18 H013 0.9300 . ? C14 C15 1.375(11) . ? C14 H014 0.9300 . ? C3 C4 1.407(14) . ? C3 H015 0.9300 . ? C15 C16 1.375(14) . ? C15 H016 0.9300 . ? C17 C16 1.381(15) . ? C17 H020 0.9300 . ? C7 C6 1.399(13) . ? C7 C8 1.400(14) . ? C7 H022 0.9300 . ? C6 H024 0.9300 . ? C16 H027 0.9300 . ? C9 C8 1.435(18) . ? C9 H029 0.9300 . ? C21 H033 0.9300 . ? C8 H034 0.9300 . ? C4 H036 0.9300 . ? C25 H042 0.9300 . ? 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 C23 C22 C21 120.7(11) . . ? C23 C22 H001 119.6 . . ? C21 C22 H001 119.6 . . ? C22 C23 C24 119.7(11) . . ? C22 C23 H007 120.2 . . ? C24 C23 H007 120.2 . . ? C6 C10 C9 109.1(12) . . ? C6 C10 Fe 70.8(6) . . ? C9 C10 Fe 69.6(7) . . ? C6 C10 H008 125.5 . . ? C9 C10 H008 125.5 . . ? Fe C10 H008 125.7 . . ? C23 C24 C25 120.3(11) . . ? C23 C24 H123 119.9 . . ? C25 C24 H123 119.9 . . ? C20 Hg S1 168.5(3) . . ? C20 Hg S2 121.5(3) . . ? S1 Hg S2 66.67(7) . . ? C9 Fe C10 40.4(5) . . ? C9 Fe C1 121.8(5) . . ? C10 Fe C1 157.6(5) . . ? C9 Fe C6 67.1(5) . . ? C10 Fe C6 39.0(5) . . ? C1 Fe C6 161.7(4) . . ? C9 Fe C8 41.7(5) . . ? C10 Fe C8 68.5(6) . . ? C1 Fe C8 107.3(4) . . ? C6 Fe C8 67.7(4) . . ? C9 Fe C2 105.4(4) . . ? C10 Fe C2 121.2(5) . . ? C1 Fe C2 41.1(3) . . ? C6 Fe C2 156.7(4) . . ? C8 Fe C2 122.4(4) . . ? C9 Fe C7 68.6(5) . . ? C10 Fe C7 67.5(5) . . ? C1 Fe C7 124.4(4) . . ? C6 Fe C7 40.4(4) . . ? C8 Fe C7 40.4(4) . . ? C2 Fe C7 159.9(4) . . ? C9 Fe C3 121.2(6) . . ? C10 Fe C3 106.7(5) . . ? C1 Fe C3 68.9(3) . . ? C6 Fe C3 122.4(4) . . ? C8 Fe C3 158.7(5) . . ? C2 Fe C3 40.9(3) . . ? C7 Fe C3 158.7(4) . . ? C9 Fe C4 157.9(6) . . ? C10 Fe C4 123.3(5) . . ? C1 Fe C4 68.4(3) . . ? C6 Fe C4 109.7(4) . . ? C8 Fe C4 159.4(5) . . ? C2 Fe C4 68.5(4) . . ? C7 Fe C4 124.2(4) . . ? C3 Fe C4 40.5(4) . . ? C9 Fe C5 159.2(6) . . ? C10 Fe C5 159.8(5) . . ? C1 Fe C5 40.8(3) . . ? C6 Fe C5 125.9(4) . . ? C8 Fe C5 123.3(5) . . ? C2 Fe C5 68.7(3) . . ? C7 Fe C5 109.6(4) . . ? C3 Fe C5 68.3(4) . . ? C4 Fe C5 40.3(4) . . ? C19 S2 Hg 77.8(3) . . ? C19 S1 Hg 95.9(3) . . ? C19 N C12 121.3(7) . . ? C19 N C11 122.3(7) . . ? C12 N C11 116.4(6) . . ? C25 C20 C21 120.0(10) . . ? C25 C20 Hg 120.0(8) . . ? C21 C20 Hg 120.0(8) . . ? N C11 C1 113.5(6) . . ? N C11 H00A 108.9 . . ? C1 C11 H00A 108.9 . . ? N C11 H00B 108.9 . . ? C1 C11 H00B 108.9 . . ? H00A C11 H00B 107.7 . . ? C18 C13 C14 119.0(8) . . ? C18 C13 C12 118.4(8) . . ? C14 C13 C12 122.5(7) . . ? N C12 C13 115.6(6) . . ? N C12 H00C 108.4 . . ? C13 C12 H00C 108.4 . . ? N C12 H00D 108.4 . . ? C13 C12 H00D 108.4 . . ? H00C C12 H00D 107.4 . . ? C4 C5 C1 107.7(8) . . ? C4 C5 Fe 69.6(5) . . ? C1 C5 Fe 68.7(4) . . ? C4 C5 H006 126.2 . . ? C1 C5 H006 126.2 . . ? Fe C5 H006 127.1 . . ? N C19 S2 123.0(6) . . ? N C19 S1 117.4(6) . . ? S2 C19 S1 119.6(5) . . ? C5 C1 C2 108.0(7) . . ? C5 C1 C11 125.6(7) . . ? C2 C1 C11 126.4(7) . . ? C5 C1 Fe 70.5(4) . . ? C2 C1 Fe 69.7(4) . . ? C11 C1 Fe 124.6(5) . . ? C3 C2 C1 107.6(8) . . ? C3 C2 Fe 69.8(4) . . ? C1 C2 Fe 69.2(4) . . ? C3 C2 H011 126.2 . . ? C1 C2 H011 126.2 . . ? Fe C2 H011 126.4 . . ? C13 C18 C17 120.5(9) . . ? C13 C18 H013 119.7 . . ? C17 C18 H013 119.7 . . ? C15 C14 C13 120.5(8) . . ? C15 C14 H014 119.8 . . ? C13 C14 H014 119.8 . . ? C2 C3 C4 108.0(8) . . ? C2 C3 Fe 69.3(5) . . ? C4 C3 Fe 70.0(5) . . ? C2 C3 H015 126.0 . . ? C4 C3 H015 126.0 . . ? Fe C3 H015 126.2 . . ? C14 C15 C16 120.7(9) . . ? C14 C15 H016 119.7 . . ? C16 C15 H016 119.7 . . ? C16 C17 C18 120.1(9) . . ? C16 C17 H020 119.9 . . ? C18 C17 H020 119.9 . . ? C6 C7 C8 107.2(10) . . ? C6 C7 Fe 69.6(5) . . ? C8 C7 Fe 69.5(5) . . ? C6 C7 H022 126.4 . . ? C8 C7 H022 126.4 . . ? Fe C7 H022 126.1 . . ? C10 C6 C7 109.8(11) . . ? C10 C6 Fe 70.2(6) . . ? C7 C6 Fe 70.0(5) . . ? C10 C6 H024 125.1 . . ? C7 C6 H024 125.1 . . ? Fe C6 H024 126.3 . . ? C17 C16 C15 119.2(9) . . ? C17 C16 H027 120.4 . . ? C15 C16 H027 120.4 . . ? C10 C9 C8 107.0(10) . . ? C10 C9 Fe 70.0(6) . . ? C8 C9 Fe 69.5(6) . . ? C10 C9 H029 126.5 . . ? C8 C9 H029 126.5 . . ? Fe C9 H029 125.6 . . ? C20 C21 C22 118.7(11) . . ? C20 C21 H033 120.7 . . ? C22 C21 H033 120.7 . . ? C7 C8 C9 106.8(11) . . ? C7 C8 Fe 70.1(5) . . ? C9 C8 Fe 68.8(6) . . ? C7 C8 H034 126.6 . . ? C9 C8 H034 126.6 . . ? Fe C8 H034 126.1 . . ? C5 C4 C3 108.8(8) . . ? C5 C4 Fe 70.1(5) . . ? C3 C4 Fe 69.5(5) . . ? C5 C4 H036 125.6 . . ? C3 C4 H036 125.6 . . ? Fe C4 H036 126.3 . . ? C20 C25 C24 120.6(11) . . ? C20 C25 H042 119.7 . . ? C24 C25 H042 119.7 . . ? 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 C21 C22 C23 C24 2.2(17) . . . . ? C22 C23 C24 C25 -0.9(17) . . . . ? C6 C10 Fe C9 -119.9(12) . . . . ? C6 C10 Fe C1 -163.9(9) . . . . ? C9 C10 Fe C1 -44.0(16) . . . . ? C9 C10 Fe C6 119.9(12) . . . . ? C6 C10 Fe C8 -80.7(8) . . . . ? C9 C10 Fe C8 39.2(8) . . . . ? C6 C10 Fe C2 163.5(6) . . . . ? C9 C10 Fe C2 -76.6(9) . . . . ? C6 C10 Fe C7 -37.0(7) . . . . ? C9 C10 Fe C7 83.0(8) . . . . ? C6 C10 Fe C3 121.3(8) . . . . ? C9 C10 Fe C3 -118.8(8) . . . . ? C6 C10 Fe C4 80.1(9) . . . . ? C9 C10 Fe C4 -159.9(8) . . . . ? C6 C10 Fe C5 48.9(17) . . . . ? C9 C10 Fe C5 168.8(11) . . . . ? C20 Hg S2 C19 -170.8(4) . . . . ? S1 Hg S2 C19 0.1(3) . . . . ? C20 Hg S1 C19 137.4(13) . . . . ? S2 Hg S1 C19 -0.1(3) . . . . ? S1 Hg C20 C25 30.6(18) . . . . ? S2 Hg C20 C25 163.8(6) . . . . ? S1 Hg C20 C21 -148.8(10) . . . . ? S2 Hg C20 C21 -15.6(8) . . . . ? C19 N C11 C1 -101.7(8) . . . . ? C12 N C11 C1 81.7(8) . . . . ? C19 N C12 C13 75.4(9) . . . . ? C11 N C12 C13 -108.0(8) . . . . ? C18 C13 C12 N -162.1(7) . . . . ? C14 C13 C12 N 21.1(11) . . . . ? C9 Fe C5 C4 -158.6(12) . . . . ? C10 Fe C5 C4 42.0(15) . . . . ? C1 Fe C5 C4 -119.5(7) . . . . ? C6 Fe C5 C4 77.9(7) . . . . ? C8 Fe C5 C4 163.0(6) . . . . ? C2 Fe C5 C4 -81.3(6) . . . . ? C7 Fe C5 C4 120.1(6) . . . . ? C3 Fe C5 C4 -37.2(5) . . . . ? C9 Fe C5 C1 -39.1(14) . . . . ? C10 Fe C5 C1 161.6(13) . . . . ? C6 Fe C5 C1 -162.6(5) . . . . ? C8 Fe C5 C1 -77.5(6) . . . . ? C2 Fe C5 C1 38.2(4) . . . . ? C7 Fe C5 C1 -120.4(5) . . . . ? C3 Fe C5 C1 82.3(5) . . . . ? C4 Fe C5 C1 119.5(7) . . . . ? C12 N C19 S2 -178.3(5) . . . . ? C11 N C19 S2 5.3(10) . . . . ? C12 N C19 S1 2.9(9) . . . . ? C11 N C19 S1 -173.6(5) . . . . ? Hg S2 C19 N -178.9(7) . . . . ? Hg S2 C19 S1 -0.1(4) . . . . ? Hg S1 C19 N 179.0(5) . . . . ? Hg S1 C19 S2 0.1(5) . . . . ? C4 C5 C1 C2 -0.9(9) . . . . ? Fe C5 C1 C2 -59.8(5) . . . . ? C4 C5 C1 C11 178.0(7) . . . . ? Fe C5 C1 C11 119.2(7) . . . . ? C4 C5 C1 Fe 58.8(5) . . . . ? N C11 C1 C5 100.1(9) . . . . ? N C11 C1 C2 -81.2(9) . . . . ? N C11 C1 Fe -170.2(5) . . . . ? C9 Fe C1 C5 164.7(7) . . . . ? C10 Fe C1 C5 -163.4(12) . . . . ? C6 Fe C1 C5 50.3(13) . . . . ? C8 Fe C1 C5 121.3(6) . . . . ? C2 Fe C1 C5 -118.8(7) . . . . ? C7 Fe C1 C5 80.2(6) . . . . ? C3 Fe C1 C5 -80.9(6) . . . . ? C4 Fe C1 C5 -37.3(5) . . . . ? C9 Fe C1 C2 -76.5(7) . . . . ? C10 Fe C1 C2 -44.5(14) . . . . ? C6 Fe C1 C2 169.1(11) . . . . ? C8 Fe C1 C2 -119.9(6) . . . . ? C7 Fe C1 C2 -161.0(5) . . . . ? C3 Fe C1 C2 37.9(5) . . . . ? C4 Fe C1 C2 81.5(5) . . . . ? C5 Fe C1 C2 118.8(7) . . . . ? C9 Fe C1 C11 44.3(9) . . . . ? C10 Fe C1 C11 76.3(14) . . . . ? C6 Fe C1 C11 -70.1(14) . . . . ? C8 Fe C1 C11 1.0(8) . . . . ? C2 Fe C1 C11 120.8(9) . . . . ? C7 Fe C1 C11 -40.2(8) . . . . ? C3 Fe C1 C11 158.7(8) . . . . ? C4 Fe C1 C11 -157.7(8) . . . . ? C5 Fe C1 C11 -120.4(9) . . . . ? C5 C1 C2 C3 0.9(9) . . . . ? C11 C1 C2 C3 -178.1(7) . . . . ? Fe C1 C2 C3 -59.4(6) . . . . ? C5 C1 C2 Fe 60.3(5) . . . . ? C11 C1 C2 Fe -118.6(7) . . . . ? C9 Fe C2 C3 -120.1(8) . . . . ? C10 Fe C2 C3 -79.3(8) . . . . ? C1 Fe C2 C3 118.9(8) . . . . ? C6 Fe C2 C3 -52.4(12) . . . . ? C8 Fe C2 C3 -162.2(7) . . . . ? C7 Fe C2 C3 170.2(11) . . . . ? C4 Fe C2 C3 37.5(6) . . . . ? C5 Fe C2 C3 81.0(6) . . . . ? C9 Fe C2 C1 120.9(7) . . . . ? C10 Fe C2 C1 161.8(6) . . . . ? C6 Fe C2 C1 -171.4(9) . . . . ? C8 Fe C2 C1 78.9(7) . . . . ? C7 Fe C2 C1 51.3(13) . . . . ? C3 Fe C2 C1 -118.9(8) . . . . ? C4 Fe C2 C1 -81.4(5) . . . . ? C5 Fe C2 C1 -37.9(5) . . . . ? C14 C13 C18 C17 0.1(13) . . . . ? C12 C13 C18 C17 -176.9(8) . . . . ? C18 C13 C14 C15 0.7(12) . . . . ? C12 C13 C14 C15 177.5(7) . . . . ? C1 C2 C3 C4 -0.4(9) . . . . ? Fe C2 C3 C4 -59.5(6) . . . . ? C1 C2 C3 Fe 59.1(5) . . . . ? C9 Fe C3 C2 77.1(8) . . . . ? C10 Fe C3 C2 118.6(7) . . . . ? C1 Fe C3 C2 -38.1(5) . . . . ? C6 Fe C3 C2 158.2(6) . . . . ? C8 Fe C3 C2 45.3(15) . . . . ? C7 Fe C3 C2 -170.7(10) . . . . ? C4 Fe C3 C2 -119.2(8) . . . . ? C5 Fe C3 C2 -82.1(6) . . . . ? C9 Fe C3 C4 -163.7(7) . . . . ? C10 Fe C3 C4 -122.1(7) . . . . ? C1 Fe C3 C4 81.1(5) . . . . ? C6 Fe C3 C4 -82.6(7) . . . . ? C8 Fe C3 C4 164.5(11) . . . . ? C2 Fe C3 C4 119.2(8) . . . . ? C7 Fe C3 C4 -51.5(14) . . . . ? C5 Fe C3 C4 37.1(5) . . . . ? C13 C14 C15 C16 -0.9(13) . . . . ? C13 C18 C17 C16 -0.7(15) . . . . ? C9 Fe C7 C6 79.4(8) . . . . ? C10 Fe C7 C6 35.7(7) . . . . ? C1 Fe C7 C6 -166.0(6) . . . . ? C8 Fe C7 C6 118.5(10) . . . . ? C2 Fe C7 C6 155.5(10) . . . . ? C3 Fe C7 C6 -42.3(15) . . . . ? C4 Fe C7 C6 -80.2(7) . . . . ? C5 Fe C7 C6 -122.8(6) . . . . ? C9 Fe C7 C8 -39.1(8) . . . . ? C10 Fe C7 C8 -82.8(8) . . . . ? C1 Fe C7 C8 75.6(8) . . . . ? C6 Fe C7 C8 -118.5(10) . . . . ? C2 Fe C7 C8 37.1(15) . . . . ? C3 Fe C7 C8 -160.8(12) . . . . ? C4 Fe C7 C8 161.3(7) . . . . ? C5 Fe C7 C8 118.7(8) . . . . ? C9 C10 C6 C7 -0.4(13) . . . . ? Fe C10 C6 C7 58.9(7) . . . . ? C9 C10 C6 Fe -59.3(8) . . . . ? C8 C7 C6 C10 0.5(11) . . . . ? Fe C7 C6 C10 -59.1(8) . . . . ? C8 C7 C6 Fe 59.5(6) . . . . ? C9 Fe C6 C10 37.6(9) . . . . ? C1 Fe C6 C10 160.4(11) . . . . ? C8 Fe C6 C10 82.9(9) . . . . ? C2 Fe C6 C10 -37.9(14) . . . . ? C7 Fe C6 C10 121.0(11) . . . . ? C3 Fe C6 C10 -75.9(9) . . . . ? C4 Fe C6 C10 -119.0(9) . . . . ? C5 Fe C6 C10 -161.2(8) . . . . ? C9 Fe C6 C7 -83.4(8) . . . . ? C10 Fe C6 C7 -121.0(11) . . . . ? C1 Fe C6 C7 39.4(15) . . . . ? C8 Fe C6 C7 -38.1(7) . . . . ? C2 Fe C6 C7 -158.9(9) . . . . ? C3 Fe C6 C7 163.2(6) . . . . ? C4 Fe C6 C7 120.0(6) . . . . ? C5 Fe C6 C7 77.8(7) . . . . ? C18 C17 C16 C15 0.6(15) . . . . ? C14 C15 C16 C17 0.2(14) . . . . ? C6 C10 C9 C8 0.1(13) . . . . ? Fe C10 C9 C8 -59.9(7) . . . . ? C6 C10 C9 Fe 60.0(8) . . . . ? C1 Fe C9 C10 161.8(7) . . . . ? C6 Fe C9 C10 -36.3(7) . . . . ? C8 Fe C9 C10 -117.9(10) . . . . ? C2 Fe C9 C10 120.3(8) . . . . ? C7 Fe C9 C10 -80.0(8) . . . . ? C3 Fe C9 C10 78.8(8) . . . . ? C4 Fe C9 C10 49.8(15) . . . . ? C5 Fe C9 C10 -169.1(10) . . . . ? C10 Fe C9 C8 117.9(10) . . . . ? C1 Fe C9 C8 -80.2(7) . . . . ? C6 Fe C9 C8 81.7(7) . . . . ? C2 Fe C9 C8 -121.8(7) . . . . ? C7 Fe C9 C8 37.9(6) . . . . ? C3 Fe C9 C8 -163.3(6) . . . . ? C4 Fe C9 C8 167.7(9) . . . . ? C5 Fe C9 C8 -51.2(15) . . . . ? C25 C20 C21 C22 1.1(13) . . . . ? Hg C20 C21 C22 -179.6(7) . . . . ? C23 C22 C21 C20 -2.3(15) . . . . ? C6 C7 C8 C9 -0.4(10) . . . . ? Fe C7 C8 C9 59.3(7) . . . . ? C6 C7 C8 Fe -59.7(6) . . . . ? C10 C9 C8 C7 0.2(12) . . . . ? Fe C9 C8 C7 -60.1(6) . . . . ? C10 C9 C8 Fe 60.3(8) . . . . ? C9 Fe C8 C7 118.1(10) . . . . ? C10 Fe C8 C7 80.1(7) . . . . ? C1 Fe C8 C7 -123.2(6) . . . . ? C6 Fe C8 C7 38.0(6) . . . . ? C2 Fe C8 C7 -165.8(6) . . . . ? C3 Fe C8 C7 160.8(10) . . . . ? C4 Fe C8 C7 -48.8(14) . . . . ? C5 Fe C8 C7 -81.3(7) . . . . ? C10 Fe C8 C9 -38.0(7) . . . . ? C1 Fe C8 C9 118.7(8) . . . . ? C6 Fe C8 C9 -80.1(8) . . . . ? C2 Fe C8 C9 76.1(8) . . . . ? C7 Fe C8 C9 -118.1(10) . . . . ? C3 Fe C8 C9 42.7(15) . . . . ? C4 Fe C8 C9 -166.9(11) . . . . ? C5 Fe C8 C9 160.6(7) . . . . ? C1 C5 C4 C3 0.7(9) . . . . ? Fe C5 C4 C3 58.9(6) . . . . ? C1 C5 C4 Fe -58.3(5) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? Fe C3 C4 C5 -59.3(6) . . . . ? C2 C3 C4 Fe 59.1(6) . . . . ? C9 Fe C4 C5 159.8(11) . . . . ? C10 Fe C4 C5 -163.9(6) . . . . ? C1 Fe C4 C5 37.7(5) . . . . ? C6 Fe C4 C5 -122.8(6) . . . . ? C8 Fe C4 C5 -43.9(13) . . . . ? C2 Fe C4 C5 82.1(5) . . . . ? C7 Fe C4 C5 -80.1(6) . . . . ? C3 Fe C4 C5 120.1(7) . . . . ? C9 Fe C4 C3 39.8(14) . . . . ? C10 Fe C4 C3 76.0(7) . . . . ? C1 Fe C4 C3 -82.3(5) . . . . ? C6 Fe C4 C3 117.2(6) . . . . ? C8 Fe C4 C3 -164.0(10) . . . . ? C2 Fe C4 C3 -37.9(5) . . . . ? C7 Fe C4 C3 159.9(6) . . . . ? C5 Fe C4 C3 -120.1(7) . . . . ? C21 C20 C25 C24 0.2(14) . . . . ? Hg C20 C25 C24 -179.2(7) . . . . ? C23 C24 C25 C20 -0.3(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.109 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.150 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 745815' #TrackingRef 'cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H46 Fe2 Hg2 N2 S4' _chemical_formula_sum 'C42 H46 Fe2 Hg2 N2 S4' _chemical_formula_weight 1219.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.41660(10) _cell_length_b 23.7015(3) _cell_length_c 11.94360(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.8990(10) _cell_angle_gamma 90.00 _cell_volume 2008.84(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42253 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 8.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1964 _exptl_absorpt_correction_T_max 0.4234 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '589 1.1 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40590 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5874 _reflns_number_gt 4656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0594P)^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 5874 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.17921(2) 0.053829(7) -0.038387(14) 0.02689(7) Uani 1 1 d . . . Fe Fe -0.21696(7) -0.10446(3) -0.57907(5) 0.02086(13) Uani 1 1 d . . . S1 S 0.30045(15) -0.03962(5) -0.05123(10) 0.0266(2) Uani 1 1 d . . . S2 S -0.09898(15) -0.01961(5) -0.19106(10) 0.0281(2) Uani 1 1 d . . . N N 0.0992(5) -0.11189(15) -0.2087(3) 0.0219(7) Uani 1 1 d . . . C1 C 0.0960(6) -0.06199(18) -0.1575(4) 0.0224(8) Uani 1 1 d . . . C2 C -0.0656(6) -0.13096(19) -0.3049(4) 0.0245(8) Uani 1 1 d . . . H2A H -0.1774 -0.1083 -0.3041 0.029 Uiso 1 1 calc R . . H2B H -0.0928 -0.1710 -0.2921 0.029 Uiso 1 1 calc R . . C3 C -0.0303(5) -0.12504(18) -0.4217(3) 0.0223(8) Uani 1 1 d . . . C4 C -0.0420(6) -0.1688(2) -0.5055(4) 0.0261(9) Uani 1 1 d . . . H4 H -0.0781 -0.2068 -0.4979 0.031 Uiso 1 1 calc R . . C5 C 0.0093(6) -0.1463(2) -0.6020(4) 0.0292(9) Uani 1 1 d . . . H5 H 0.0129 -0.1663 -0.6703 0.035 Uiso 1 1 calc R . . C6 C 0.0541(6) -0.0885(2) -0.5780(4) 0.0298(10) Uani 1 1 d . . . H6 H 0.0940 -0.0630 -0.6273 0.036 Uiso 1 1 calc R . . C7 C 0.0289(6) -0.0755(2) -0.4668(4) 0.0268(9) Uani 1 1 d . . . H7 H 0.0486 -0.0397 -0.4296 0.032 Uiso 1 1 calc R . . C8 C -0.4750(6) -0.0921(2) -0.5542(5) 0.0348(11) Uani 1 1 d . . . H8 H -0.5060 -0.0962 -0.4828 0.042 Uiso 1 1 calc R . . C9 C -0.4851(6) -0.1355(2) -0.6382(4) 0.0366(11) Uani 1 1 d . . . H9 H -0.5230 -0.1734 -0.6328 0.044 Uiso 1 1 calc R . . C10 C -0.4277(6) -0.1115(3) -0.7319(4) 0.0379(12) Uani 1 1 d . . . H10 H -0.4193 -0.1308 -0.8000 0.045 Uiso 1 1 calc R . . C11 C -0.3850(7) -0.0532(2) -0.7054(5) 0.0339(11) Uani 1 1 d . . . H11 H -0.3460 -0.0268 -0.7536 0.041 Uiso 1 1 calc R . . C12 C -0.4111(7) -0.0416(2) -0.5943(5) 0.0371(11) Uani 1 1 d . . . H12 H -0.3897 -0.0065 -0.5542 0.045 Uiso 1 1 calc R . . C13 C 0.2736(6) -0.14669(18) -0.1813(4) 0.0255(9) Uani 1 1 d . . . H13 H 0.3439 -0.1399 -0.0973 0.031 Uiso 1 1 calc R . . C14 C 0.4024(6) -0.1287(2) -0.2544(4) 0.0308(10) Uani 1 1 d . . . H14A H 0.3447 -0.1393 -0.3363 0.046 Uiso 1 1 calc R . . H14B H 0.5248 -0.1475 -0.2248 0.046 Uiso 1 1 calc R . . H14C H 0.4203 -0.0877 -0.2490 0.046 Uiso 1 1 calc R . . C15 C 0.2302(8) -0.2098(2) -0.1954(4) 0.0368(11) Uani 1 1 d . . . H15A H 0.1484 -0.2204 -0.1475 0.055 Uiso 1 1 calc R . . H15B H 0.3480 -0.2312 -0.1699 0.055 Uiso 1 1 calc R . . H15C H 0.1664 -0.2181 -0.2777 0.055 Uiso 1 1 calc R . . C16 C 0.0884(6) 0.13676(19) -0.0507(4) 0.0253(9) Uani 1 1 d . . . C17 C -0.1020(7) 0.1474(2) -0.1045(4) 0.0304(10) Uani 1 1 d . . . H17 H -0.1857 0.1170 -0.1334 0.036 Uiso 1 1 calc R . . C18 C -0.1704(6) 0.2026(2) -0.1161(4) 0.0314(10) Uani 1 1 d . . . H18 H -0.3008 0.2092 -0.1519 0.038 Uiso 1 1 calc R . . C19 C -0.0515(6) 0.2478(2) -0.0765(4) 0.0302(10) Uani 1 1 d . . . H19 H -0.0992 0.2853 -0.0849 0.036 Uiso 1 1 calc R . . C20 C 0.1400(7) 0.2377(2) -0.0239(5) 0.0370(11) Uani 1 1 d . . . H20 H 0.2239 0.2683 0.0030 0.044 Uiso 1 1 calc R . . C21 C 0.2072(6) 0.1828(2) -0.0110(4) 0.0326(10) Uani 1 1 d . . . H21 H 0.3374 0.1764 0.0259 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 Hg 0.03056(11) 0.02460(11) 0.02665(11) -0.00136(6) 0.01009(7) -0.00076(6) Fe 0.0177(3) 0.0263(3) 0.0191(3) 0.0014(2) 0.0060(2) 0.0011(2) S1 0.0253(5) 0.0288(5) 0.0235(5) -0.0034(4) 0.0036(4) -0.0007(4) S2 0.0262(5) 0.0309(6) 0.0274(5) 0.0018(4) 0.0080(4) 0.0040(4) N 0.0222(16) 0.0248(18) 0.0189(16) 0.0005(14) 0.0064(13) -0.0018(14) C1 0.0230(19) 0.029(2) 0.0170(19) 0.0032(16) 0.0094(16) 0.0006(16) C2 0.0232(19) 0.029(2) 0.020(2) -0.0019(17) 0.0049(15) -0.0039(17) C3 0.0175(17) 0.027(2) 0.0199(19) 0.0012(16) 0.0014(14) -0.0016(15) C4 0.0248(19) 0.029(2) 0.023(2) 0.0038(18) 0.0041(16) 0.0043(17) C5 0.027(2) 0.040(3) 0.023(2) 0.0009(19) 0.0109(17) 0.0057(19) C6 0.0210(19) 0.042(3) 0.028(2) 0.0084(19) 0.0094(17) 0.0024(18) C7 0.0211(19) 0.030(2) 0.028(2) 0.0011(19) 0.0053(16) -0.0028(17) C8 0.0199(19) 0.050(3) 0.038(3) 0.006(2) 0.0129(18) 0.0064(19) C9 0.021(2) 0.052(3) 0.033(3) 0.008(2) 0.0016(18) -0.008(2) C10 0.024(2) 0.063(4) 0.022(2) 0.006(2) -0.0014(17) 0.001(2) C11 0.027(2) 0.043(3) 0.032(3) 0.014(2) 0.0082(19) 0.0085(19) C12 0.033(2) 0.040(3) 0.043(3) 0.008(2) 0.018(2) 0.014(2) C13 0.028(2) 0.024(2) 0.024(2) 0.0034(17) 0.0071(16) 0.0043(16) C14 0.027(2) 0.037(3) 0.031(2) 0.003(2) 0.0128(18) 0.0066(19) C15 0.049(3) 0.028(2) 0.031(3) 0.005(2) 0.008(2) 0.006(2) C16 0.024(2) 0.026(2) 0.026(2) -0.0007(17) 0.0079(16) -0.0026(17) C17 0.033(2) 0.031(2) 0.028(2) -0.0040(18) 0.0109(18) -0.0092(19) C18 0.026(2) 0.038(3) 0.029(2) -0.001(2) 0.0058(17) 0.0015(18) C19 0.032(2) 0.025(2) 0.034(2) 0.0022(18) 0.0098(18) 0.0021(18) C20 0.033(2) 0.029(3) 0.047(3) -0.003(2) 0.009(2) -0.012(2) C21 0.027(2) 0.036(3) 0.032(2) -0.002(2) 0.0050(17) -0.0010(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg C16 2.069(4) . ? Hg S1 2.4121(12) . ? Hg S2 2.9025(11) . ? Hg S2 3.0773(11) 3 ? Fe C4 2.030(4) . ? Fe C5 2.035(4) . ? Fe C10 2.036(4) . ? Fe C8 2.042(4) . ? Fe C6 2.042(4) . ? Fe C7 2.043(4) . ? Fe C12 2.043(5) . ? Fe C3 2.043(4) . ? Fe C9 2.044(4) . ? Fe C11 2.053(5) . ? S1 C1 1.753(4) . ? S2 C1 1.710(4) . ? N C1 1.335(5) . ? N C2 1.483(5) . ? N C13 1.488(5) . ? C2 C3 1.499(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C7 1.415(6) . ? C3 C4 1.428(6) . ? C4 C5 1.419(6) . ? C4 H4 0.9500 . ? C5 C6 1.418(7) . ? C5 H5 0.9500 . ? C6 C7 1.427(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C12 1.421(7) . ? C8 C9 1.423(8) . ? C8 H8 0.9500 . ? C9 C10 1.427(7) . ? C9 H9 0.9500 . ? C10 C11 1.433(7) . ? C10 H10 0.9500 . ? C11 C12 1.422(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.528(6) . ? C13 C14 1.531(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.394(6) . ? C16 C21 1.397(6) . ? C17 C18 1.396(7) . ? C17 H17 0.9500 . ? C18 C19 1.380(6) . ? C18 H18 0.9500 . ? C19 C20 1.397(7) . ? C19 H19 0.9500 . ? C20 C21 1.384(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 C16 Hg S1 170.91(12) . . ? C16 Hg S2 111.57(12) . . ? S1 Hg S2 67.63(3) . . ? C16 Hg S2 99.82(12) . 3 ? S1 Hg S2 89.24(4) . 3 ? S2 Hg S2 96.62(3) . 3 ? C4 Fe C5 40.87(17) . . ? C4 Fe C10 123.7(2) . . ? C5 Fe C10 106.7(2) . . ? C4 Fe C8 123.58(19) . . ? C5 Fe C8 159.1(2) . . ? C10 Fe C8 68.6(2) . . ? C4 Fe C6 68.40(18) . . ? C5 Fe C6 40.71(19) . . ? C10 Fe C6 121.24(19) . . ? C8 Fe C6 159.3(2) . . ? C4 Fe C7 68.42(18) . . ? C5 Fe C7 68.80(19) . . ? C10 Fe C7 157.2(2) . . ? C8 Fe C7 123.5(2) . . ? C6 Fe C7 40.90(18) . . ? C4 Fe C12 158.7(2) . . ? C5 Fe C12 158.5(2) . . ? C10 Fe C12 69.0(2) . . ? C8 Fe C12 40.7(2) . . ? C6 Fe C12 122.2(2) . . ? C7 Fe C12 106.6(2) . . ? C4 Fe C3 41.03(17) . . ? C5 Fe C3 69.10(17) . . ? C10 Fe C3 160.7(2) . . ? C8 Fe C3 108.25(18) . . ? C6 Fe C3 68.65(17) . . ? C7 Fe C3 40.51(17) . . ? C12 Fe C3 121.8(2) . . ? C4 Fe C9 108.3(2) . . ? C5 Fe C9 122.4(2) . . ? C10 Fe C9 40.95(19) . . ? C8 Fe C9 40.8(2) . . ? C6 Fe C9 157.8(2) . . ? C7 Fe C9 160.20(19) . . ? C12 Fe C9 69.0(2) . . ? C3 Fe C9 124.24(18) . . ? C4 Fe C11 159.8(2) . . ? C5 Fe C11 122.5(2) . . ? C10 Fe C11 41.0(2) . . ? C8 Fe C11 68.1(2) . . ? C6 Fe C11 106.35(19) . . ? C7 Fe C11 121.2(2) . . ? C12 Fe C11 40.6(2) . . ? C3 Fe C11 157.2(2) . . ? C9 Fe C11 68.7(2) . . ? C1 S1 Hg 93.65(15) . . ? C1 S2 Hg 78.85(15) . . ? C1 N C2 120.3(4) . . ? C1 N C13 121.3(3) . . ? C2 N C13 118.0(3) . . ? N C1 S2 122.6(3) . . ? N C1 S1 118.2(3) . . ? S2 C1 S1 119.1(3) . . ? N C2 C3 111.4(3) . . ? N C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C7 C3 C4 107.4(4) . . ? C7 C3 C2 126.2(4) . . ? C4 C3 C2 126.4(4) . . ? C7 C3 Fe 69.7(2) . . ? C4 C3 Fe 69.0(2) . . ? C2 C3 Fe 128.6(3) . . ? C5 C4 C3 108.7(4) . . ? C5 C4 Fe 69.7(2) . . ? C3 C4 Fe 70.0(2) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 126.2 . . ? C6 C5 C4 107.5(4) . . ? C6 C5 Fe 69.9(2) . . ? C4 C5 Fe 69.4(2) . . ? C6 C5 H5 126.2 . . ? C4 C5 H5 126.2 . . ? Fe C5 H5 126.1 . . ? C5 C6 C7 108.1(4) . . ? C5 C6 Fe 69.4(2) . . ? C7 C6 Fe 69.6(2) . . ? C5 C6 H6 125.9 . . ? C7 C6 H6 125.9 . . ? Fe C6 H6 126.7 . . ? C3 C7 C6 108.3(4) . . ? C3 C7 Fe 69.8(2) . . ? C6 C7 Fe 69.5(2) . . ? C3 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe C7 H7 126.4 . . ? C12 C8 C9 109.0(5) . . ? C12 C8 Fe 69.7(3) . . ? C9 C8 Fe 69.7(3) . . ? C12 C8 H8 125.5 . . ? C9 C8 H8 125.5 . . ? Fe C8 H8 126.7 . . ? C8 C9 C10 107.4(5) . . ? C8 C9 Fe 69.5(3) . . ? C10 C9 Fe 69.2(3) . . ? C8 C9 H9 126.3 . . ? C10 C9 H9 126.3 . . ? Fe C9 H9 126.5 . . ? C9 C10 C11 107.9(5) . . ? C9 C10 Fe 69.8(2) . . ? C11 C10 Fe 70.1(3) . . ? C9 C10 H10 126.0 . . ? C11 C10 H10 126.0 . . ? Fe C10 H10 125.6 . . ? C12 C11 C10 108.1(4) . . ? C12 C11 Fe 69.3(3) . . ? C10 C11 Fe 68.8(2) . . ? C12 C11 H11 125.9 . . ? C10 C11 H11 125.9 . . ? Fe C11 H11 127.5 . . ? C8 C12 C11 107.6(5) . . ? C8 C12 Fe 69.6(3) . . ? C11 C12 Fe 70.1(3) . . ? C8 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? Fe C12 H12 125.7 . . ? N C13 C15 112.1(4) . . ? N C13 C14 111.5(3) . . ? C15 C13 C14 110.9(4) . . ? N C13 H13 107.4 . . ? C15 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 118.0(4) . . ? C17 C16 Hg 118.1(3) . . ? C21 C16 Hg 123.9(3) . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.0(4) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.9(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 121.7(4) . . ? C20 C21 H21 119.2 . . ? C16 C21 H21 119.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.303 _refine_diff_density_min -3.260 _refine_diff_density_rms 0.337 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 745816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H25 Fe Hg N S2' _chemical_formula_sum 'C22 H25 Fe Hg N S2' _chemical_formula_weight 623.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.4157(2) _cell_length_b 12.9206(3) _cell_length_c 17.6156(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.5530(10) _cell_angle_gamma 90.00 _cell_volume 2113.33(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 53199 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'irregular plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 8.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2604 _exptl_absorpt_correction_T_max 0.4417 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '276 1.3 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31040 _diffrn_reflns_av_R_equivalents 0.1112 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4829 _reflns_number_gt 3774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.1046P)^2^+98.8939P] 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 0.0063(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4829 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2583 _refine_ls_wR_factor_gt 0.2455 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.35180(7) 0.14342(5) 0.98961(4) 0.0354(3) Uani 1 1 d . . . Fe Fe 0.7738(3) -0.09866(18) 1.39451(13) 0.0298(5) Uani 1 1 d . . . S1 S 0.5674(5) 0.2052(3) 1.0688(2) 0.0350(9) Uani 1 1 d . . . S2 S 0.4732(5) -0.0051(3) 1.1106(3) 0.0336(9) Uani 1 1 d . . . N1 N 0.6994(14) 0.0967(10) 1.1867(8) 0.027(3) Uani 1 1 d . . . C1 C 0.5899(16) 0.0968(12) 1.1289(10) 0.027(3) Uani 1 1 d . . . C2 C 0.7444(18) 0.0033(13) 1.2339(9) 0.033(3) Uani 1 1 d . . . H2A H 0.8508 -0.0015 1.2423 0.039 Uiso 1 1 calc R . . H2B H 0.7057 -0.0589 1.2047 0.039 Uiso 1 1 calc R . . C3 C 0.6954(19) 0.0023(13) 1.3105(9) 0.032(3) Uani 1 1 d . . . C4 C 0.757(2) 0.0572(13) 1.3776(11) 0.038(4) Uani 1 1 d . . . H4 H 0.8339 0.1052 1.3817 0.046 Uiso 1 1 calc R . . C5 C 0.681(2) 0.0273(14) 1.4379(10) 0.039(4) Uani 1 1 d . . . H5 H 0.6981 0.0526 1.4893 0.047 Uiso 1 1 calc R . . C6 C 0.5752(19) -0.0479(16) 1.4071(11) 0.040(4) Uani 1 1 d . . . H6 H 0.5112 -0.0821 1.4352 0.048 Uiso 1 1 calc R . . C7 C 0.5808(18) -0.0628(14) 1.3298(11) 0.037(4) Uani 1 1 d . . . H7 H 0.5207 -0.1075 1.2957 0.044 Uiso 1 1 calc R . . C8 C 0.985(2) -0.1314(16) 1.4153(14) 0.050(5) Uani 1 1 d . . . H8 H 1.0597 -0.0817 1.4151 0.060 Uiso 1 1 calc R . . C9 C 0.926(2) -0.1584(19) 1.4781(14) 0.057(6) Uani 1 1 d . . . H9 H 0.9549 -0.1323 1.5288 0.068 Uiso 1 1 calc R . . C10 C 0.816(2) -0.2313(14) 1.4559(12) 0.045(5) Uani 1 1 d . . . H10 H 0.7559 -0.2615 1.4885 0.054 Uiso 1 1 calc R . . C11 C 0.809(2) -0.2516(15) 1.3764(13) 0.047(5) Uani 1 1 d . . . H11 H 0.7447 -0.2977 1.3458 0.057 Uiso 1 1 calc R . . C12 C 0.919(2) -0.1888(17) 1.3505(13) 0.049(5) Uani 1 1 d . . . H12 H 0.9421 -0.1865 1.3001 0.059 Uiso 1 1 calc R . . C13 C 0.7866(17) 0.1910(14) 1.2079(10) 0.033(4) Uani 1 1 d . . . H13A H 0.8046 0.2260 1.1604 0.040 Uiso 1 1 calc R . . H13B H 0.8809 0.1708 1.2379 0.040 Uiso 1 1 calc R . . C14 C 0.7128(18) 0.2663(13) 1.2551(10) 0.033(4) Uani 1 1 d . . . H14A H 0.6238 0.2925 1.2230 0.040 Uiso 1 1 calc R . . H14B H 0.6847 0.2290 1.2994 0.040 Uiso 1 1 calc R . . C15 C 0.808(2) 0.3574(14) 1.2847(13) 0.045(5) Uani 1 1 d . . . H15A H 0.8330 0.3971 1.2408 0.054 Uiso 1 1 calc R . . H15B H 0.8979 0.3321 1.3162 0.054 Uiso 1 1 calc R . . C16 C 0.727(2) 0.4277(16) 1.3338(12) 0.048(5) Uani 1 1 d . . . H16A H 0.7889 0.4865 1.3528 0.071 Uiso 1 1 calc R . . H16B H 0.7034 0.3883 1.3775 0.071 Uiso 1 1 calc R . . H16C H 0.6386 0.4532 1.3023 0.071 Uiso 1 1 calc R . . C17 C 0.1483(19) 0.1205(14) 0.9257(10) 0.035(4) Uani 1 1 d . . . C18 C 0.085(2) 0.0238(15) 0.9204(11) 0.044(4) Uani 1 1 d . . . H18 H 0.1361 -0.0338 0.9453 0.053 Uiso 1 1 calc R . . C19 C -0.058(2) 0.0101(16) 0.8770(12) 0.049(5) Uani 1 1 d . . . H19 H -0.1039 -0.0553 0.8753 0.059 Uiso 1 1 calc R . . C20 C -0.125(2) 0.0927(17) 0.8386(12) 0.048(5) Uani 1 1 d . . . H20 H -0.2193 0.0848 0.8107 0.057 Uiso 1 1 calc R . . C21 C -0.058(2) 0.1866(15) 0.8397(11) 0.043(4) Uani 1 1 d . . . H21 H -0.1059 0.2424 0.8110 0.051 Uiso 1 1 calc R . . C22 C 0.075(2) 0.2017(14) 0.8809(10) 0.039(4) Uani 1 1 d . . . H22 H 0.1193 0.2674 0.8799 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg 0.0347(4) 0.0366(4) 0.0338(4) -0.0027(3) 0.0022(2) 0.0018(3) Fe 0.0316(12) 0.0267(12) 0.0299(11) 0.0010(9) 0.0013(9) 0.0012(9) S1 0.041(2) 0.028(2) 0.033(2) 0.0038(16) -0.0022(17) -0.0069(17) S2 0.033(2) 0.030(2) 0.038(2) -0.0008(16) 0.0064(17) -0.0054(16) N1 0.028(6) 0.020(6) 0.036(7) 0.001(5) 0.010(5) 0.002(5) C1 0.021(7) 0.025(7) 0.038(8) 0.002(6) 0.011(6) 0.005(6) C2 0.031(8) 0.033(9) 0.030(8) -0.002(7) -0.005(6) 0.000(7) C3 0.042(9) 0.027(8) 0.027(8) 0.001(6) 0.005(7) 0.007(7) C4 0.047(10) 0.024(8) 0.041(9) -0.004(7) -0.005(8) 0.006(7) C5 0.061(12) 0.031(9) 0.025(8) -0.006(7) 0.004(8) 0.009(8) C6 0.029(8) 0.051(11) 0.042(10) 0.011(8) 0.013(7) 0.020(8) C7 0.029(8) 0.039(9) 0.040(9) -0.003(7) 0.000(7) 0.005(7) C8 0.032(9) 0.045(11) 0.074(15) 0.026(10) 0.009(9) 0.008(8) C9 0.040(11) 0.070(15) 0.051(12) 0.013(11) -0.016(9) 0.008(10) C10 0.053(11) 0.032(9) 0.051(11) 0.020(8) 0.009(9) 0.021(8) C11 0.038(10) 0.032(9) 0.067(13) -0.002(9) -0.006(9) 0.013(8) C12 0.052(12) 0.048(11) 0.047(11) -0.002(9) 0.006(9) 0.013(9) C13 0.021(7) 0.038(9) 0.039(9) 0.001(7) 0.001(6) -0.010(6) C14 0.032(8) 0.028(8) 0.038(9) -0.004(7) 0.002(7) -0.003(6) C15 0.053(12) 0.030(9) 0.054(12) -0.010(8) 0.012(9) 0.002(8) C16 0.060(12) 0.036(10) 0.048(11) -0.011(8) 0.013(9) 0.004(9) C17 0.032(8) 0.035(9) 0.036(9) 0.006(7) 0.004(7) -0.001(7) C18 0.059(12) 0.033(9) 0.039(10) 0.010(8) 0.004(9) 0.011(9) C19 0.059(13) 0.041(11) 0.043(11) -0.005(8) -0.004(9) -0.017(9) C20 0.049(11) 0.055(12) 0.040(10) -0.006(9) 0.012(9) -0.006(9) C21 0.058(12) 0.036(9) 0.035(9) 0.005(8) 0.008(8) 0.001(9) C22 0.051(11) 0.030(9) 0.034(9) -0.001(7) 0.001(8) 0.002(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 Hg C17 2.076(18) . ? Hg S1 2.401(4) . ? Hg S2 2.954(4) . ? Hg S2 3.161(4) 3_657 ? Fe C8 2.01(2) . ? Fe C3 2.018(16) . ? Fe C6 2.029(16) . ? Fe C10 2.030(17) . ? Fe C9 2.03(2) . ? Fe C7 2.032(17) . ? Fe C11 2.038(19) . ? Fe C4 2.038(17) . ? Fe C12 2.04(2) . ? Fe C5 2.053(17) . ? S1 C1 1.748(16) . ? S2 C1 1.711(16) . ? N1 C1 1.32(2) . ? N1 C13 1.48(2) . ? N1 C2 1.49(2) . ? C2 C3 1.50(2) . ? C3 C4 1.42(2) . ? C3 C7 1.45(3) . ? C4 C5 1.43(3) . ? C5 C6 1.43(3) . ? C6 C7 1.38(3) . ? C8 C9 1.36(3) . ? C8 C12 1.42(3) . ? C9 C10 1.41(3) . ? C10 C11 1.42(3) . ? C11 C12 1.45(3) . ? C13 C14 1.52(2) . ? C14 C15 1.52(2) . ? C15 C16 1.54(3) . ? C17 C18 1.38(3) . ? C17 C22 1.42(2) . ? C18 C19 1.44(3) . ? C19 C20 1.36(3) . ? C20 C21 1.36(3) . ? C21 C22 1.35(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Hg S1 167.9(5) . . ? C17 Hg S2 120.7(5) . . ? S1 Hg S2 66.94(13) . . ? C17 Hg S2 97.8(5) . 3_657 ? S1 Hg S2 92.50(14) . 3_657 ? S2 Hg S2 82.00(13) . 3_657 ? C8 Fe C3 120.1(8) . . ? C8 Fe C6 162.2(9) . . ? C3 Fe C6 68.9(7) . . ? C8 Fe C10 68.1(8) . . ? C3 Fe C10 162.0(8) . . ? C6 Fe C10 108.4(8) . . ? C8 Fe C9 39.5(10) . . ? C3 Fe C9 155.0(9) . . ? C6 Fe C9 126.6(9) . . ? C10 Fe C9 40.7(9) . . ? C8 Fe C7 156.6(9) . . ? C3 Fe C7 42.0(7) . . ? C6 Fe C7 39.9(7) . . ? C10 Fe C7 124.6(9) . . ? C9 Fe C7 162.2(9) . . ? C8 Fe C11 69.0(9) . . ? C3 Fe C11 124.1(8) . . ? C6 Fe C11 120.5(9) . . ? C10 Fe C11 40.8(9) . . ? C9 Fe C11 68.4(9) . . ? C7 Fe C11 106.7(8) . . ? C8 Fe C4 106.7(8) . . ? C3 Fe C4 40.9(7) . . ? C6 Fe C4 69.2(8) . . ? C10 Fe C4 156.3(8) . . ? C9 Fe C4 120.7(9) . . ? C7 Fe C4 69.6(8) . . ? C11 Fe C4 161.1(9) . . ? C8 Fe C12 40.9(9) . . ? C3 Fe C12 106.1(8) . . ? C6 Fe C12 155.9(9) . . ? C10 Fe C12 68.8(9) . . ? C9 Fe C12 67.8(10) . . ? C7 Fe C12 120.6(8) . . ? C11 Fe C12 41.5(9) . . ? C4 Fe C12 123.3(9) . . ? C8 Fe C5 124.6(9) . . ? C3 Fe C5 68.5(7) . . ? C6 Fe C5 41.1(8) . . ? C10 Fe C5 121.8(8) . . ? C9 Fe C5 108.9(9) . . ? C7 Fe C5 68.4(7) . . ? C11 Fe C5 156.5(9) . . ? C4 Fe C5 40.8(8) . . ? C12 Fe C5 160.9(9) . . ? C1 S1 Hg 95.3(6) . . ? C1 S2 Hg 78.2(6) . . ? C1 N1 C13 121.4(14) . . ? C1 N1 C2 123.0(13) . . ? C13 N1 C2 115.6(13) . . ? N1 C1 S2 122.5(12) . . ? N1 C1 S1 117.9(12) . . ? S2 C1 S1 119.5(10) . . ? N1 C2 C3 114.1(14) . . ? C4 C3 C7 108.1(16) . . ? C4 C3 C2 127.2(17) . . ? C7 C3 C2 124.6(15) . . ? C4 C3 Fe 70.3(10) . . ? C7 C3 Fe 69.5(9) . . ? C2 C3 Fe 122.4(11) . . ? C3 C4 C5 107.6(17) . . ? C3 C4 Fe 68.8(9) . . ? C5 C4 Fe 70.2(10) . . ? C4 C5 C6 107.6(15) . . ? C4 C5 Fe 69.0(10) . . ? C6 C5 Fe 68.5(9) . . ? C7 C6 C5 109.2(16) . . ? C7 C6 Fe 70.2(10) . . ? C5 C6 Fe 70.4(10) . . ? C6 C7 C3 107.5(16) . . ? C6 C7 Fe 69.9(10) . . ? C3 C7 Fe 68.5(9) . . ? C9 C8 C12 110(2) . . ? C9 C8 Fe 71.1(12) . . ? C12 C8 Fe 70.8(12) . . ? C8 C9 C10 109(2) . . ? C8 C9 Fe 69.4(12) . . ? C10 C9 Fe 69.7(11) . . ? C9 C10 C11 108(2) . . ? C9 C10 Fe 69.7(11) . . ? C11 C10 Fe 69.9(11) . . ? C10 C11 C12 107.0(19) . . ? C10 C11 Fe 69.3(11) . . ? C12 C11 Fe 69.4(11) . . ? C8 C12 C11 106.5(19) . . ? C8 C12 Fe 68.3(12) . . ? C11 C12 Fe 69.0(11) . . ? N1 C13 C14 112.3(13) . . ? C15 C14 C13 112.9(15) . . ? C14 C15 C16 109.6(17) . . ? C18 C17 C22 117.8(17) . . ? C18 C17 Hg 120.8(13) . . ? C22 C17 Hg 121.2(13) . . ? C17 C18 C19 119.8(17) . . ? C20 C19 C18 118.8(19) . . ? C19 C20 C21 121(2) . . ? C22 C21 C20 121.1(19) . . ? C21 C22 C17 121.0(18) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 10.628 _refine_diff_density_min -2.588 _refine_diff_density_rms 0.393 #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 745817' #TrackingRef 'cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H55 Fe2 Hg2 N2 O S4' _chemical_formula_weight 1341.08 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' Fe Fe 0.3463 0.8444 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 16.1120(6) _cell_length_b 8.1550(2) _cell_length_c 33.8880(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.104(1) _cell_angle_gamma 90.00 _cell_volume 4449.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 78224 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2612 _exptl_absorpt_coefficient_mu 7.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.397 _exptl_absorpt_correction_T_max 0.472 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10212 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9728 _reflns_number_gt 4967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Every so often a conundrum of a crystal, such as this one, becomes a crystallographic candidate. The sample is usually interesting, and the data turn out to less than satisfactory. Thus, several datasets were collected for this sample, the underlying suspicion being that the sample was twinned (for example, there is a non-real 21 screw axis absence along b present). The refinement from the optimum dataset is presented herein. There may well be some residual twinning present, but not at a level that is resolvable via any common or obvious twin law(s). However, the structural model is unambiguous. Solvent present in 2 cavities in the unit cell was treated using SQUEEZE - as it was heavily disordered. Overall, this solvent contribution equates to 1.5 molecules of diethyl-ether per ASU. Two of the cp rings present were refined subject to being perfect pentagons. There is evidence of some smearing of electron density in these aromatic groups, evidenced by the ADPs which were restricted to having relative similarity restraints in the final least-squares cycles. The residual electron density maxima are at non-chemically significant distances from C13 and C14. ; _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^)+(0.0956P)^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 8310 _refine_ls_number_parameters 460 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.018 _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 0.48974(3) 0.88414(5) -0.066537(13) 0.03904(17) Uani 1 1 d . . . Hg2 Hg 0.38321(3) 0.61871(5) 0.037686(12) 0.03596(16) Uani 1 1 d . . . Fe1 Fe 0.90953(13) 0.7728(2) -0.13580(5) 0.0551(5) Uani 1 1 d . . . Fe2 Fe 0.57426(12) 0.7327(2) 0.24302(5) 0.0516(5) Uani 1 1 d . . . S1 S 0.64025(18) 0.7233(4) -0.08826(8) 0.0395(7) Uani 1 1 d . . . S2 S 0.60169(19) 0.9394(4) -0.01969(8) 0.0381(7) Uani 1 1 d . . . S3 S 0.52891(19) 0.5680(4) 0.04895(8) 0.0378(7) Uani 1 1 d . . . S4 S 0.44609(17) 0.7800(3) 0.10830(8) 0.0352(7) Uani 1 1 d . . . N1 N 0.7529(6) 0.8276(11) -0.0343(2) 0.033(2) Uani 1 1 d . . . N2 N 0.6027(5) 0.6765(10) 0.1148(2) 0.028(2) Uani 1 1 d . . . C1 C 0.3867(8) 0.8460(13) -0.1046(4) 0.042(3) Uani 1 1 d . . . C2 C 0.3972(8) 0.7989(12) -0.1432(3) 0.036(3) Uani 1 1 d . . . H2 H 0.4513 0.7763 -0.1520 0.044 Uiso 1 1 calc R . . C3 C 0.3316(9) 0.7851(13) -0.1680(4) 0.045(3) Uani 1 1 d . . . H3 H 0.3405 0.7554 -0.1946 0.054 Uiso 1 1 calc R . . C4 C 0.2549(11) 0.8109(15) -0.1574(4) 0.065(4) Uani 1 1 d . . . H4 H 0.2098 0.7996 -0.1760 0.078 Uiso 1 1 calc R . . C5 C 0.2401(8) 0.8563(14) -0.1171(4) 0.049(4) Uani 1 1 d . . . H5 H 0.1851 0.8713 -0.1085 0.059 Uiso 1 1 calc R . . C6 C 0.3070(7) 0.8771(12) -0.0916(4) 0.040(3) Uani 1 1 d . . . H6 H 0.2993 0.9125 -0.0653 0.047 Uiso 1 1 calc R . . C7 C 0.2585(8) 0.6540(12) 0.0253(4) 0.040(3) Uani 1 1 d . . . C8 C 0.2223(8) 0.6213(11) -0.0129(3) 0.036(3) Uani 1 1 d . . . H8 H 0.2567 0.5896 -0.0337 0.044 Uiso 1 1 calc R . . C9 C 0.1368(7) 0.6352(13) -0.0200(4) 0.043(3) Uani 1 1 d . . . H9 H 0.1130 0.6129 -0.0455 0.052 Uiso 1 1 calc R . . C10 C 0.0861(8) 0.6825(14) 0.0109(4) 0.048(3) Uani 1 1 d . . . H10 H 0.0277 0.6899 0.0065 0.057 Uiso 1 1 calc R . . C11 C 0.1211(8) 0.7177(13) 0.0472(3) 0.041(3) Uani 1 1 d . . . H11 H 0.0871 0.7527 0.0680 0.049 Uiso 1 1 calc R . . C12 C 0.2051(7) 0.7025(14) 0.0537(3) 0.043(3) Uani 1 1 d . . . H12 H 0.2277 0.7268 0.0793 0.051 Uiso 1 1 calc R . . C13 C 0.6722(8) 0.8280(12) -0.0466(3) 0.037(3) Uani 1 1 d . . . C14 C 0.5314(7) 0.6753(12) 0.0932(3) 0.032(3) Uani 1 1 d . . . C15 C 0.8166(6) 0.7406(13) -0.0548(3) 0.036(3) Uani 1 1 d . . . H15A H 0.7906 0.6479 -0.0695 0.043 Uiso 1 1 calc R . . H15B H 0.8569 0.6942 -0.0351 0.043 Uiso 1 1 calc R . . C16 C 0.7856(7) 0.9274(13) -0.0013(3) 0.036(3) Uani 1 1 d . . . H16A H 0.7464 1.0181 0.0036 0.043 Uiso 1 1 calc R . . H16B H 0.8392 0.9764 -0.0085 0.043 Uiso 1 1 calc R . . C17 C 0.7986(7) 0.8276(12) 0.0364(3) 0.029(2) Uani 1 1 d . . . C18 C 0.8775(7) 0.8162(14) 0.0537(4) 0.045(3) Uani 1 1 d . . . H18 H 0.9231 0.8671 0.0417 0.053 Uiso 1 1 calc R . . C19 C 0.8895(7) 0.7303(16) 0.0887(4) 0.054(4) Uani 1 1 d . . . H19 H 0.9432 0.7261 0.1011 0.064 Uiso 1 1 calc R . . C20 C 0.8245(8) 0.6511(13) 0.1054(3) 0.041(3) Uani 1 1 d . . . H20 H 0.8343 0.5869 0.1285 0.049 Uiso 1 1 calc R . . C21 C 0.7444(6) 0.6638(12) 0.0889(3) 0.023(2) Uani 1 1 d . . . C22 C 0.7329(6) 0.7504(11) 0.0542(3) 0.026(2) Uani 1 1 d . . . H22 H 0.6789 0.7572 0.0421 0.031 Uiso 1 1 calc R . . C23 C 0.6734(6) 0.5702(12) 0.1068(3) 0.028(3) Uani 1 1 d . . . H23A H 0.6549 0.4821 0.0884 0.034 Uiso 1 1 calc R . . H23B H 0.6935 0.5180 0.1317 0.034 Uiso 1 1 calc R . . C24 C 0.6127(6) 0.7715(12) 0.1520(3) 0.027(2) Uani 1 1 d . . . H24A H 0.5708 0.8604 0.1521 0.032 Uiso 1 1 calc R . . H24B H 0.6685 0.8226 0.1534 0.032 Uiso 1 1 calc R . . C25 C 0.8625(7) 0.8449(13) -0.0831(3) 0.034(3) Uani 1 1 d . . . C26 C 0.9473(8) 0.8680(16) -0.0837(4) 0.059(4) Uani 1 1 d . . . H26 H 0.9879 0.8194 -0.0663 0.071 Uiso 1 1 calc R . . C27 C 0.9632(8) 0.9811(16) -0.1159(4) 0.055(4) Uani 1 1 d . . . H27 H 1.0165 1.0205 -0.1224 0.066 Uiso 1 1 calc R . . C28 C 0.8924(8) 1.0209(14) -0.1349(3) 0.047(3) Uani 1 1 d . . . H28 H 0.8861 1.0899 -0.1574 0.057 Uiso 1 1 calc R . . C29 C 0.8265(7) 0.9383(14) -0.1145(3) 0.041(3) Uani 1 1 d . . . H29 H 0.7688 0.9458 -0.1211 0.049 Uiso 1 1 calc R . . C30 C 0.8853(9) 0.5227(9) -0.1416(2) 0.144(5) Uani 1 1 d GU . . H30 H 0.8621 0.4509 -0.1228 0.173 Uiso 1 1 calc R . . C31 C 0.9705(9) 0.5645(13) -0.1438(2) 0.146(5) Uani 1 1 d GU . . H31 H 1.0144 0.5256 -0.1268 0.175 Uiso 1 1 calc R . . C32 C 0.9786(9) 0.6746(12) -0.1759(2) 0.142(5) Uani 1 1 d GU . . H32 H 1.0289 0.7223 -0.1842 0.171 Uiso 1 1 calc R . . C33 C 0.8983(10) 0.7008(11) -0.1935(2) 0.140(5) Uani 1 1 d GU . . H33 H 0.8855 0.7692 -0.2156 0.168 Uiso 1 1 calc R . . C34 C 0.8406(9) 0.6069(13) -0.17226(18) 0.143(5) Uani 1 1 d GU . . H34 H 0.7824 0.6014 -0.1777 0.171 Uiso 1 1 calc R . . C35 C 0.6024(5) 0.6629(9) 0.18744(16) 0.026(2) Uani 1 1 d G . . C36 C 0.6715(5) 0.6179(9) 0.21459(15) 0.051(3) Uani 1 1 d G . . H36 H 0.7280 0.6508 0.2140 0.061 Uiso 1 1 calc R . . C37 C 0.6307(6) 0.5058(8) 0.24394(17) 0.057(4) Uani 1 1 d G . . H37 H 0.6582 0.4536 0.2658 0.068 Uiso 1 1 calc R . . C38 C 0.5422(8) 0.4909(15) 0.2331(3) 0.051(3) Uani 1 1 d . . . H38 H 0.5022 0.4312 0.2472 0.061 Uiso 1 1 calc R . . C39 C 0.5271(8) 0.5823(14) 0.1977(3) 0.050(3) Uani 1 1 d . . . H39 H 0.4755 0.5887 0.1833 0.060 Uiso 1 1 calc R . . C40 C 0.5413(10) 0.9782(12) 0.2411(3) 0.105(4) Uani 1 1 d GU . . H40 H 0.5317 1.0433 0.2181 0.126 Uiso 1 1 calc R . . C41 C 0.6183(8) 0.9605(14) 0.2624(4) 0.108(4) Uani 1 1 d GU . . H41 H 0.6692 1.0116 0.2562 0.129 Uiso 1 1 calc R . . C42 C 0.6059(9) 0.8529(14) 0.2946(3) 0.109(4) Uani 1 1 d GU . . H42 H 0.6470 0.8194 0.3138 0.131 Uiso 1 1 calc R . . C43 C 0.5212(10) 0.8041(12) 0.2932(3) 0.107(4) Uani 1 1 d GU . . H43 H 0.4957 0.7322 0.3112 0.128 Uiso 1 1 calc R . . C44 C 0.4813(7) 0.8816(15) 0.2601(4) 0.109(4) Uani 1 1 d GU . . H44 H 0.4245 0.8706 0.2521 0.130 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 0.0389(3) 0.0386(3) 0.0398(3) 0.0070(2) 0.0040(2) 0.0013(2) Hg2 0.0368(3) 0.0382(3) 0.0328(2) 0.0003(2) 0.0015(2) -0.0049(2) Fe1 0.0798(15) 0.0485(12) 0.0388(10) 0.0011(9) 0.0276(10) 0.0112(10) Fe2 0.0821(15) 0.0477(11) 0.0263(8) 0.0018(8) 0.0171(9) 0.0083(10) S1 0.0457(19) 0.0388(18) 0.0340(15) -0.0041(13) 0.0035(14) 0.0005(14) S2 0.0435(19) 0.0428(18) 0.0283(14) 0.0016(12) 0.0075(13) 0.0104(15) S3 0.0409(19) 0.0443(17) 0.0286(14) -0.0088(12) 0.0077(13) -0.0058(15) S4 0.0314(17) 0.0413(18) 0.0332(14) -0.0047(13) 0.0038(13) 0.0034(13) N1 0.042(6) 0.039(6) 0.020(4) 0.003(4) 0.001(4) 0.001(5) N2 0.032(6) 0.021(5) 0.033(5) 0.000(4) 0.010(4) -0.001(4) C1 0.051(9) 0.027(7) 0.048(7) -0.004(5) -0.007(6) 0.001(6) C2 0.051(8) 0.030(7) 0.029(6) -0.009(5) 0.004(6) 0.002(6) C3 0.064(10) 0.028(7) 0.042(7) 0.001(5) 0.002(7) 0.002(7) C4 0.100(13) 0.027(8) 0.066(10) 0.003(7) -0.032(9) -0.010(8) C5 0.028(8) 0.038(8) 0.082(10) 0.010(7) 0.002(7) 0.006(6) C6 0.029(7) 0.033(7) 0.056(8) -0.014(6) -0.004(6) 0.009(5) C7 0.053(9) 0.019(6) 0.048(7) 0.011(5) -0.009(6) -0.009(5) C8 0.051(9) 0.020(6) 0.038(6) -0.008(5) -0.007(6) 0.005(5) C9 0.031(8) 0.049(8) 0.049(7) -0.013(6) -0.010(6) -0.002(6) C10 0.028(7) 0.036(7) 0.078(10) 0.013(7) -0.002(7) 0.002(6) C11 0.055(9) 0.033(7) 0.036(6) 0.001(5) 0.016(6) 0.007(6) C12 0.037(8) 0.053(8) 0.038(7) 0.008(6) 0.007(6) -0.007(6) C13 0.079(10) 0.013(6) 0.020(5) 0.004(4) 0.006(6) -0.023(6) C14 0.038(7) 0.022(6) 0.036(6) 0.018(5) 0.026(6) 0.012(5) C15 0.035(7) 0.041(7) 0.032(6) -0.004(5) 0.004(5) 0.016(6) C16 0.045(8) 0.040(7) 0.023(5) -0.008(5) 0.006(5) -0.009(6) C17 0.031(7) 0.028(6) 0.028(5) 0.001(4) 0.004(5) -0.001(5) C18 0.034(8) 0.050(8) 0.050(7) 0.013(6) 0.009(6) -0.012(6) C19 0.025(7) 0.084(10) 0.052(8) 0.011(7) -0.011(6) 0.001(7) C20 0.052(8) 0.045(7) 0.025(5) 0.011(5) 0.000(6) -0.011(6) C21 0.022(6) 0.029(6) 0.019(5) -0.009(4) 0.001(4) 0.007(5) C22 0.028(6) 0.020(6) 0.030(5) -0.008(4) 0.011(5) 0.001(5) C23 0.036(7) 0.030(6) 0.018(5) 0.006(4) 0.007(5) 0.002(5) C24 0.026(6) 0.034(6) 0.020(5) 0.007(4) -0.003(4) -0.003(5) C25 0.041(8) 0.042(7) 0.020(5) -0.006(5) 0.003(5) 0.002(5) C26 0.037(9) 0.102(12) 0.039(7) 0.006(7) 0.003(6) 0.012(7) C27 0.043(9) 0.081(10) 0.042(7) -0.002(7) 0.023(7) -0.023(7) C28 0.062(9) 0.044(8) 0.038(7) 0.000(6) 0.022(7) 0.006(7) C29 0.041(8) 0.046(7) 0.037(6) 0.009(5) 0.018(6) 0.014(6) C30 0.242(15) 0.104(8) 0.090(8) -0.044(6) 0.041(9) 0.019(9) C31 0.243(15) 0.106(8) 0.092(8) -0.044(6) 0.042(9) 0.029(9) C32 0.239(15) 0.104(8) 0.087(8) -0.049(6) 0.048(9) 0.028(9) C33 0.240(15) 0.101(8) 0.082(8) -0.049(6) 0.040(9) 0.022(9) C34 0.240(15) 0.103(8) 0.088(8) -0.050(6) 0.038(9) 0.014(9) C35 0.030(6) 0.022(6) 0.027(5) 0.004(4) 0.006(5) -0.003(5) C36 0.079(10) 0.040(8) 0.034(6) 0.007(5) -0.004(6) -0.007(6) C37 0.112(13) 0.040(8) 0.019(5) -0.003(5) 0.005(7) 0.010(8) C38 0.058(9) 0.068(9) 0.028(6) 0.022(6) 0.010(6) -0.012(7) C39 0.064(9) 0.062(8) 0.024(6) 0.011(6) 0.006(6) -0.010(7) C40 0.176(11) 0.073(7) 0.069(6) -0.026(5) 0.032(7) 0.028(7) C41 0.180(11) 0.074(7) 0.072(6) -0.030(5) 0.029(7) 0.020(7) C42 0.181(11) 0.076(7) 0.071(6) -0.027(5) 0.027(7) 0.024(7) C43 0.178(11) 0.074(7) 0.071(6) -0.026(5) 0.035(7) 0.026(7) C44 0.175(11) 0.077(7) 0.076(6) -0.030(5) 0.033(7) 0.030(6) _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 C1 2.088(12) . ? Hg1 S2 2.401(3) . ? Hg1 S1 2.876(3) . ? Hg2 C7 2.058(12) . ? Hg2 S3 2.400(3) . ? Hg2 S4 2.882(3) . ? Fe1 C32 1.959(7) . ? Fe1 C31 1.986(10) . ? Fe1 C26 2.004(13) . ? Fe1 C27 2.011(13) . ? Fe1 C28 2.043(12) . ? Fe1 C33 2.043(7) . ? Fe1 C29 2.050(11) . ? Fe1 C25 2.051(10) . ? Fe1 C30 2.085(8) . ? Fe1 C34 2.118(11) . ? Fe2 C43 2.016(10) . ? Fe2 C44 2.028(11) . ? Fe2 C35 2.035(6) . ? Fe2 C42 2.052(10) . ? Fe2 C38 2.063(13) . ? Fe2 C37 2.062(7) . ? Fe2 C40 2.071(10) . ? Fe2 C39 2.087(12) . ? Fe2 C41 2.086(11) . ? Fe2 C36 2.091(7) . ? S1 C13 1.713(10) . ? S2 C13 1.739(12) . ? S3 C14 1.737(11) . ? S4 C14 1.711(10) . ? N1 C13 1.350(14) . ? N1 C15 1.448(12) . ? N1 C16 1.465(13) . ? N2 C14 1.339(13) . ? N2 C23 1.465(13) . ? N2 C24 1.482(12) . ? C1 C2 1.379(14) . ? C1 C6 1.396(16) . ? C2 C3 1.332(15) . ? C2 H2 0.9500 . ? C3 C4 1.316(18) . ? C3 H3 0.9500 . ? C4 C5 1.443(18) . ? C4 H4 0.9500 . ? C5 C6 1.368(16) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.374(16) . ? C7 C8 1.425(15) . ? C8 C9 1.394(16) . ? C8 H8 0.9500 . ? C9 C10 1.405(17) . ? C9 H9 0.9500 . ? C10 C11 1.365(16) . ? C10 H10 0.9500 . ? C11 C12 1.369(15) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C15 C25 1.497(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.522(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.384(15) . ? C17 C22 1.387(13) . ? C18 C19 1.383(15) . ? C18 H18 0.9500 . ? C19 C20 1.371(15) . ? C19 H19 0.9500 . ? C20 C21 1.391(15) . ? C20 H20 0.9500 . ? C21 C22 1.381(13) . ? C21 C23 1.519(14) . ? C22 H22 0.9500 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C35 1.507(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.380(16) . ? C25 C29 1.415(14) . ? C26 C27 1.460(16) . ? C26 H26 0.9500 . ? C27 C28 1.329(16) . ? C27 H27 0.9500 . ? C28 C29 1.454(15) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C34 1.4200 . ? C30 C31 1.4200 . ? C30 H30 0.9500 . ? C31 C32 1.4200 . ? C31 H31 0.9500 . ? C32 C33 1.4200 . ? C32 H32 0.9500 . ? C33 C34 1.4200 . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C39 1.435(14) . ? C35 C36 1.4644 . ? C36 C37 1.5185 . ? C36 H36 0.9500 . ? C37 C38 1.463(15) . ? C37 H37 0.9500 . ? C38 C39 1.426(14) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.4200 . ? C40 C44 1.4200 . ? C40 H40 0.9500 . ? C41 C42 1.4200 . ? C41 H41 0.9500 . ? C42 C43 1.4200 . ? C42 H42 0.9500 . ? C43 C44 1.4200 . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? 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 C1 Hg1 S2 175.8(3) . . ? C1 Hg1 S1 115.6(3) . . ? S2 Hg1 S1 68.58(9) . . ? C7 Hg2 S3 176.8(4) . . ? C7 Hg2 S4 114.6(3) . . ? S3 Hg2 S4 68.57(8) . . ? C32 Fe1 C31 42.18(19) . . ? C32 Fe1 C26 127.4(6) . . ? C31 Fe1 C26 108.4(5) . . ? C32 Fe1 C27 109.2(5) . . ? C31 Fe1 C27 124.0(6) . . ? C26 Fe1 C27 42.6(5) . . ? C32 Fe1 C28 119.7(4) . . ? C31 Fe1 C28 156.5(5) . . ? C26 Fe1 C28 68.9(5) . . ? C27 Fe1 C28 38.3(5) . . ? C32 Fe1 C33 41.50(10) . . ? C31 Fe1 C33 69.52(19) . . ? C26 Fe1 C33 165.5(5) . . ? C27 Fe1 C33 125.8(4) . . ? C28 Fe1 C33 107.0(4) . . ? C32 Fe1 C29 155.2(5) . . ? C31 Fe1 C29 160.7(4) . . ? C26 Fe1 C29 67.4(5) . . ? C27 Fe1 C29 66.7(5) . . ? C28 Fe1 C29 41.6(4) . . ? C33 Fe1 C29 119.4(5) . . ? C32 Fe1 C25 163.4(5) . . ? C31 Fe1 C25 124.4(4) . . ? C26 Fe1 C25 39.8(5) . . ? C27 Fe1 C25 68.5(4) . . ? C28 Fe1 C25 69.4(4) . . ? C33 Fe1 C25 153.2(6) . . ? C29 Fe1 C25 40.4(4) . . ? C32 Fe1 C30 69.2(2) . . ? C31 Fe1 C30 40.74(15) . . ? C26 Fe1 C30 120.8(5) . . ? C27 Fe1 C30 159.2(6) . . ? C28 Fe1 C30 161.0(6) . . ? C33 Fe1 C30 67.6(2) . . ? C29 Fe1 C30 123.7(5) . . ? C25 Fe1 C30 106.7(3) . . ? C32 Fe1 C34 68.5(2) . . ? C31 Fe1 C34 68.0(2) . . ? C26 Fe1 C34 153.8(4) . . ? C27 Fe1 C34 160.8(5) . . ? C28 Fe1 C34 125.0(5) . . ? C33 Fe1 C34 39.85(18) . . ? C29 Fe1 C34 106.9(5) . . ? C25 Fe1 C34 119.2(4) . . ? C30 Fe1 C34 39.48(17) . . ? C43 Fe2 C44 41.11(19) . . ? C43 Fe2 C35 167.7(5) . . ? C44 Fe2 C35 128.6(4) . . ? C43 Fe2 C42 40.85(17) . . ? C44 Fe2 C42 68.54(19) . . ? C35 Fe2 C42 149.9(5) . . ? C43 Fe2 C38 107.5(4) . . ? C44 Fe2 C38 115.8(5) . . ? C35 Fe2 C38 69.2(4) . . ? C42 Fe2 C38 130.3(5) . . ? C43 Fe2 C37 116.5(4) . . ? C44 Fe2 C37 149.6(5) . . ? C35 Fe2 C37 69.5(2) . . ? C42 Fe2 C37 108.7(4) . . ? C38 Fe2 C37 41.6(4) . . ? C43 Fe2 C40 68.4(2) . . ? C44 Fe2 C40 40.51(18) . . ? C35 Fe2 C40 107.9(3) . . ? C42 Fe2 C40 67.7(2) . . ? C38 Fe2 C40 148.9(6) . . ? C37 Fe2 C40 168.6(5) . . ? C43 Fe2 C39 129.5(5) . . ? C44 Fe2 C39 108.0(5) . . ? C35 Fe2 C39 40.7(4) . . ? C42 Fe2 C39 168.5(5) . . ? C38 Fe2 C39 40.2(4) . . ? C37 Fe2 C39 68.4(4) . . ? C40 Fe2 C39 117.3(5) . . ? C43 Fe2 C41 68.1(2) . . ? C44 Fe2 C41 67.9(2) . . ? C35 Fe2 C41 117.1(4) . . ? C42 Fe2 C41 40.13(19) . . ? C38 Fe2 C41 169.3(5) . . ? C37 Fe2 C41 130.5(5) . . ? C40 Fe2 C41 39.94(17) . . ? C39 Fe2 C41 150.0(5) . . ? C43 Fe2 C36 150.0(5) . . ? C44 Fe2 C36 166.7(5) . . ? C35 Fe2 C36 41.56(11) . . ? C42 Fe2 C36 116.1(4) . . ? C38 Fe2 C36 71.6(4) . . ? C37 Fe2 C36 42.89(14) . . ? C40 Fe2 C36 127.9(4) . . ? C39 Fe2 C36 69.9(4) . . ? C41 Fe2 C36 107.0(4) . . ? C13 S1 Hg1 78.0(5) . . ? C13 S2 Hg1 92.6(4) . . ? C14 S3 Hg2 92.4(4) . . ? C14 S4 Hg2 77.7(4) . . ? C13 N1 C15 122.9(9) . . ? C13 N1 C16 123.3(9) . . ? C15 N1 C16 113.5(9) . . ? C14 N2 C23 123.5(8) . . ? C14 N2 C24 122.1(8) . . ? C23 N2 C24 114.0(8) . . ? C2 C1 C6 119.7(11) . . ? C2 C1 Hg1 120.3(9) . . ? C6 C1 Hg1 119.8(9) . . ? C3 C2 C1 120.1(11) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 123.0(13) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 119.4(13) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 118.4(12) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C1 119.4(12) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C12 C7 C8 116.4(11) . . ? C12 C7 Hg2 122.0(9) . . ? C8 C7 Hg2 121.6(10) . . ? C9 C8 C7 120.7(11) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.5(11) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 119.8(11) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.9(11) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 123.7(11) . . ? C11 C12 H12 118.1 . . ? C7 C12 H12 118.1 . . ? N1 C13 S1 120.7(9) . . ? N1 C13 S2 118.6(7) . . ? S1 C13 S2 120.6(8) . . ? N2 C14 S4 121.1(8) . . ? N2 C14 S3 117.8(7) . . ? S4 C14 S3 121.1(7) . . ? N1 C15 C25 113.9(9) . . ? N1 C15 H15A 108.8 . . ? C25 C15 H15A 108.8 . . ? N1 C15 H15B 108.8 . . ? C25 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N1 C16 C17 112.2(9) . . ? N1 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? N1 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C22 119.2(10) . . ? C18 C17 C16 119.2(10) . . ? C22 C17 C16 121.6(10) . . ? C17 C18 C19 119.7(10) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.5(11) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.6(10) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 118.4(9) . . ? C22 C21 C23 121.1(9) . . ? C20 C21 C23 120.2(9) . . ? C21 C22 C17 121.5(10) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? N2 C23 C21 112.3(8) . . ? N2 C23 H23A 109.2 . . ? C21 C23 H23A 109.2 . . ? N2 C23 H23B 109.2 . . ? C21 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? N2 C24 C35 111.0(8) . . ? N2 C24 H24A 109.4 . . ? C35 C24 H24A 109.4 . . ? N2 C24 H24B 109.4 . . ? C35 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C29 107.2(10) . . ? C26 C25 C15 126.8(10) . . ? C29 C25 C15 126.0(10) . . ? C26 C25 Fe1 68.3(7) . . ? C29 C25 Fe1 69.8(6) . . ? C15 C25 Fe1 127.0(7) . . ? C25 C26 C27 107.3(11) . . ? C25 C26 Fe1 71.9(7) . . ? C27 C26 Fe1 68.9(7) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? Fe1 C26 H26 124.4 . . ? C28 C27 C26 110.2(11) . . ? C28 C27 Fe1 72.1(8) . . ? C26 C27 Fe1 68.4(7) . . ? C28 C27 H27 124.9 . . ? C26 C27 H27 124.9 . . ? Fe1 C27 H27 126.1 . . ? C27 C28 C29 106.6(11) . . ? C27 C28 Fe1 69.6(8) . . ? C29 C28 Fe1 69.5(6) . . ? C27 C28 H28 126.7 . . ? C29 C28 H28 126.7 . . ? Fe1 C28 H28 125.8 . . ? C25 C29 C28 108.7(11) . . ? C25 C29 Fe1 69.8(6) . . ? C28 C29 Fe1 68.9(6) . . ? C25 C29 H29 125.7 . . ? C28 C29 H29 125.7 . . ? Fe1 C29 H29 127.2 . . ? C34 C30 C31 108.0 . . ? C34 C30 Fe1 71.5(4) . . ? C31 C30 Fe1 65.9(4) . . ? C34 C30 H30 126.0 . . ? C31 C30 H30 126.0 . . ? Fe1 C30 H30 128.1 . . ? C32 C31 C30 108.0 . . ? C32 C31 Fe1 67.89(17) . . ? C30 C31 Fe1 73.4(4) . . ? C32 C31 H31 126.0 . . ? C30 C31 H31 126.0 . . ? Fe1 C31 H31 124.3 . . ? C33 C32 C31 108.0 . . ? C33 C32 Fe1 72.4(4) . . ? C31 C32 Fe1 69.9(3) . . ? C33 C32 H32 126.0 . . ? C31 C32 H32 126.0 . . ? Fe1 C32 H32 123.3 . . ? C34 C33 C32 108.0 . . ? C34 C33 Fe1 72.9(3) . . ? C32 C33 Fe1 66.1(4) . . ? C34 C33 H33 126.0 . . ? C32 C33 H33 126.0 . . ? Fe1 C33 H33 126.5 . . ? C33 C34 C30 108.0 . . ? C33 C34 Fe1 67.21(17) . . ? C30 C34 Fe1 69.0(3) . . ? C33 C34 H34 126.0 . . ? C30 C34 H34 126.0 . . ? Fe1 C34 H34 129.4 . . ? C39 C35 C36 111.3(6) . . ? C39 C35 C24 125.6(8) . . ? C36 C35 C24 123.1(6) . . ? C39 C35 Fe2 71.6(5) . . ? C36 C35 Fe2 71.3(3) . . ? C24 C35 Fe2 127.5(6) . . ? C35 C36 C37 103.0 . . ? C35 C36 Fe2 67.2(2) . . ? C37 C36 Fe2 67.56(19) . . ? C35 C36 H36 128.5 . . ? C37 C36 H36 128.5 . . ? Fe2 C36 H36 128.2 . . ? C38 C37 C36 109.1(5) . . ? C38 C37 Fe2 69.3(6) . . ? C36 C37 Fe2 69.56(19) . . ? C38 C37 H37 125.4 . . ? C36 C37 H37 125.4 . . ? Fe2 C37 H37 127.3 . . ? C39 C38 C37 107.6(9) . . ? C39 C38 Fe2 70.8(7) . . ? C37 C38 Fe2 69.2(6) . . ? C39 C38 H38 126.2 . . ? C37 C38 H38 126.2 . . ? Fe2 C38 H38 125.4 . . ? C38 C39 C35 108.9(11) . . ? C38 C39 Fe2 69.0(7) . . ? C35 C39 Fe2 67.7(5) . . ? C38 C39 H39 125.6 . . ? C35 C39 H39 125.6 . . ? Fe2 C39 H39 129.4 . . ? C41 C40 C44 108.0 . . ? C41 C40 Fe2 70.6(4) . . ? C44 C40 Fe2 68.1(4) . . ? C41 C40 H40 126.0 . . ? C44 C40 H40 126.0 . . ? Fe2 C40 H40 126.9 . . ? C40 C41 C42 108.0 . . ? C40 C41 Fe2 69.5(4) . . ? C42 C41 Fe2 68.7(4) . . ? C40 C41 H41 126.0 . . ? C42 C41 H41 126.0 . . ? Fe2 C41 H41 127.4 . . ? C41 C42 C43 108.0 . . ? C41 C42 Fe2 71.2(4) . . ? C43 C42 Fe2 68.2(4) . . ? C41 C42 H42 126.0 . . ? C43 C42 H42 126.0 . . ? Fe2 C42 H42 126.1 . . ? C44 C43 C42 108.0 . . ? C44 C43 Fe2 69.9(4) . . ? C42 C43 Fe2 70.9(5) . . ? C44 C43 H43 126.0 . . ? C42 C43 H43 126.0 . . ? Fe2 C43 H43 124.8 . . ? C43 C44 C40 108.0 . . ? C43 C44 Fe2 69.0(4) . . ? C40 C44 Fe2 71.4(4) . . ? C43 C44 H44 126.0 . . ? C40 C44 H44 126.0 . . ? Fe2 C44 H44 125.2 . . ? 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 C1 Hg1 S1 C13 177.9(5) . . . . ? S2 Hg1 S1 C13 -2.3(3) . . . . ? C1 Hg1 S2 C13 179(100) . . . . ? S1 Hg1 S2 C13 2.3(3) . . . . ? C7 Hg2 S3 C14 -175(5) . . . . ? S4 Hg2 S3 C14 3.2(3) . . . . ? C7 Hg2 S4 C14 176.6(4) . . . . ? S3 Hg2 S4 C14 -3.3(3) . . . . ? S2 Hg1 C1 C2 161(4) . . . . ? S1 Hg1 C1 C2 -22.0(10) . . . . ? S2 Hg1 C1 C6 -15(5) . . . . ? S1 Hg1 C1 C6 161.7(8) . . . . ? C6 C1 C2 C3 0.8(17) . . . . ? Hg1 C1 C2 C3 -175.6(8) . . . . ? C1 C2 C3 C4 -1.7(18) . . . . ? C2 C3 C4 C5 0.1(19) . . . . ? C3 C4 C5 C6 2.4(18) . . . . ? C4 C5 C6 C1 -3.3(16) . . . . ? C2 C1 C6 C5 1.7(16) . . . . ? Hg1 C1 C6 C5 178.1(8) . . . . ? S3 Hg2 C7 C12 158(5) . . . . ? S4 Hg2 C7 C12 -20.1(10) . . . . ? S3 Hg2 C7 C8 -18(6) . . . . ? S4 Hg2 C7 C8 163.1(7) . . . . ? C12 C7 C8 C9 -1.3(15) . . . . ? Hg2 C7 C8 C9 175.6(8) . . . . ? C7 C8 C9 C10 0.2(16) . . . . ? C8 C9 C10 C11 1.4(17) . . . . ? C9 C10 C11 C12 -1.8(17) . . . . ? C10 C11 C12 C7 0.6(18) . . . . ? C8 C7 C12 C11 1.0(16) . . . . ? Hg2 C7 C12 C11 -175.9(8) . . . . ? C15 N1 C13 S1 -0.1(13) . . . . ? C16 N1 C13 S1 173.7(7) . . . . ? C15 N1 C13 S2 -179.2(7) . . . . ? C16 N1 C13 S2 -5.4(13) . . . . ? Hg1 S1 C13 N1 -175.6(8) . . . . ? Hg1 S1 C13 S2 3.5(5) . . . . ? Hg1 S2 C13 N1 175.0(7) . . . . ? Hg1 S2 C13 S1 -4.1(6) . . . . ? C23 N2 C14 S4 170.3(7) . . . . ? C24 N2 C14 S4 -1.9(13) . . . . ? C23 N2 C14 S3 -11.1(12) . . . . ? C24 N2 C14 S3 176.7(7) . . . . ? Hg2 S4 C14 N2 -176.5(8) . . . . ? Hg2 S4 C14 S3 5.0(5) . . . . ? Hg2 S3 C14 N2 175.5(7) . . . . ? Hg2 S3 C14 S4 -5.9(6) . . . . ? C13 N1 C15 C25 95.4(12) . . . . ? C16 N1 C15 C25 -78.9(11) . . . . ? C13 N1 C16 C17 101.5(11) . . . . ? C15 N1 C16 C17 -84.2(11) . . . . ? N1 C16 C17 C18 119.8(11) . . . . ? N1 C16 C17 C22 -61.4(13) . . . . ? C22 C17 C18 C19 -0.9(17) . . . . ? C16 C17 C18 C19 177.9(11) . . . . ? C17 C18 C19 C20 2.5(19) . . . . ? C18 C19 C20 C21 -3.9(19) . . . . ? C19 C20 C21 C22 3.6(16) . . . . ? C19 C20 C21 C23 177.6(10) . . . . ? C20 C21 C22 C17 -2.0(14) . . . . ? C23 C21 C22 C17 -175.9(9) . . . . ? C18 C17 C22 C21 0.7(15) . . . . ? C16 C17 C22 C21 -178.1(9) . . . . ? C14 N2 C23 C21 106.6(10) . . . . ? C24 N2 C23 C21 -80.6(10) . . . . ? C22 C21 C23 N2 -57.9(12) . . . . ? C20 C21 C23 N2 128.3(10) . . . . ? C14 N2 C24 C35 99.0(10) . . . . ? C23 N2 C24 C35 -73.9(10) . . . . ? N1 C15 C25 C26 124.7(12) . . . . ? N1 C15 C25 C29 -55.5(14) . . . . ? N1 C15 C25 Fe1 -146.2(8) . . . . ? C32 Fe1 C25 C26 45.2(19) . . . . ? C31 Fe1 C25 C26 77.1(9) . . . . ? C27 Fe1 C25 C26 -40.3(8) . . . . ? C28 Fe1 C25 C26 -81.4(8) . . . . ? C33 Fe1 C25 C26 -168.4(9) . . . . ? C29 Fe1 C25 C26 -119.0(10) . . . . ? C30 Fe1 C25 C26 118.3(8) . . . . ? C34 Fe1 C25 C26 159.2(7) . . . . ? C32 Fe1 C25 C29 164.2(15) . . . . ? C31 Fe1 C25 C29 -163.9(8) . . . . ? C26 Fe1 C25 C29 119.0(10) . . . . ? C27 Fe1 C25 C29 78.8(8) . . . . ? C28 Fe1 C25 C29 37.7(7) . . . . ? C33 Fe1 C25 C29 -49.3(12) . . . . ? C30 Fe1 C25 C29 -122.7(8) . . . . ? C34 Fe1 C25 C29 -81.8(8) . . . . ? C32 Fe1 C25 C15 -75(2) . . . . ? C31 Fe1 C25 C15 -43.3(12) . . . . ? C26 Fe1 C25 C15 -120.4(13) . . . . ? C27 Fe1 C25 C15 -160.7(11) . . . . ? C28 Fe1 C25 C15 158.2(11) . . . . ? C33 Fe1 C25 C15 71.2(13) . . . . ? C29 Fe1 C25 C15 120.5(13) . . . . ? C30 Fe1 C25 C15 -2.2(11) . . . . ? C34 Fe1 C25 C15 38.8(11) . . . . ? C29 C25 C26 C27 1.0(13) . . . . ? C15 C25 C26 C27 -179.2(10) . . . . ? Fe1 C25 C26 C27 60.2(8) . . . . ? C29 C25 C26 Fe1 -59.2(8) . . . . ? C15 C25 C26 Fe1 120.7(11) . . . . ? C32 Fe1 C26 C25 -165.2(6) . . . . ? C31 Fe1 C26 C25 -122.0(7) . . . . ? C27 Fe1 C26 C25 117.4(10) . . . . ? C28 Fe1 C26 C25 82.8(7) . . . . ? C33 Fe1 C26 C25 158.7(17) . . . . ? C29 Fe1 C26 C25 37.8(7) . . . . ? C30 Fe1 C26 C25 -79.0(8) . . . . ? C34 Fe1 C26 C25 -44.6(15) . . . . ? C32 Fe1 C26 C27 77.3(9) . . . . ? C31 Fe1 C26 C27 120.6(8) . . . . ? C28 Fe1 C26 C27 -34.6(7) . . . . ? C33 Fe1 C26 C27 41(2) . . . . ? C29 Fe1 C26 C27 -79.6(8) . . . . ? C25 Fe1 C26 C27 -117.4(10) . . . . ? C30 Fe1 C26 C27 163.6(8) . . . . ? C34 Fe1 C26 C27 -162.0(11) . . . . ? C25 C26 C27 C28 -1.9(15) . . . . ? Fe1 C26 C27 C28 60.2(9) . . . . ? C25 C26 C27 Fe1 -62.1(9) . . . . ? C32 Fe1 C27 C28 113.9(8) . . . . ? C31 Fe1 C27 C28 158.6(6) . . . . ? C26 Fe1 C27 C28 -121.2(10) . . . . ? C33 Fe1 C27 C28 70.5(9) . . . . ? C29 Fe1 C27 C28 -39.8(7) . . . . ? C25 Fe1 C27 C28 -83.6(7) . . . . ? C30 Fe1 C27 C28 -164.3(9) . . . . ? C34 Fe1 C27 C28 34.3(18) . . . . ? C32 Fe1 C27 C26 -124.9(8) . . . . ? C31 Fe1 C27 C26 -80.2(8) . . . . ? C28 Fe1 C27 C26 121.2(10) . . . . ? C33 Fe1 C27 C26 -168.3(7) . . . . ? C29 Fe1 C27 C26 81.4(7) . . . . ? C25 Fe1 C27 C26 37.6(7) . . . . ? C30 Fe1 C27 C26 -43.1(15) . . . . ? C34 Fe1 C27 C26 155.5(13) . . . . ? C26 C27 C28 C29 2.0(14) . . . . ? Fe1 C27 C28 C29 59.9(8) . . . . ? C26 C27 C28 Fe1 -58.0(9) . . . . ? C32 Fe1 C28 C27 -83.6(9) . . . . ? C31 Fe1 C28 C27 -49.4(15) . . . . ? C26 Fe1 C28 C27 38.4(7) . . . . ? C33 Fe1 C28 C27 -126.9(8) . . . . ? C29 Fe1 C28 C27 117.7(10) . . . . ? C25 Fe1 C28 C27 81.1(7) . . . . ? C30 Fe1 C28 C27 162.7(9) . . . . ? C34 Fe1 C28 C27 -166.9(6) . . . . ? C32 Fe1 C28 C29 158.7(8) . . . . ? C31 Fe1 C28 C29 -167.1(10) . . . . ? C26 Fe1 C28 C29 -79.3(7) . . . . ? C27 Fe1 C28 C29 -117.7(10) . . . . ? C33 Fe1 C28 C29 115.4(8) . . . . ? C25 Fe1 C28 C29 -36.6(7) . . . . ? C30 Fe1 C28 C29 45.0(14) . . . . ? C34 Fe1 C28 C29 75.4(8) . . . . ? C26 C25 C29 C28 0.2(13) . . . . ? C15 C25 C29 C28 -179.7(9) . . . . ? Fe1 C25 C29 C28 -58.1(8) . . . . ? C26 C25 C29 Fe1 58.3(8) . . . . ? C15 C25 C29 Fe1 -121.6(10) . . . . ? C27 C28 C29 C25 -1.4(13) . . . . ? Fe1 C28 C29 C25 58.6(8) . . . . ? C27 C28 C29 Fe1 -60.0(9) . . . . ? C32 Fe1 C29 C25 -169.3(11) . . . . ? C31 Fe1 C29 C25 43.9(19) . . . . ? C26 Fe1 C29 C25 -37.3(7) . . . . ? C27 Fe1 C29 C25 -83.8(8) . . . . ? C28 Fe1 C29 C25 -120.5(10) . . . . ? C33 Fe1 C29 C25 156.9(7) . . . . ? C30 Fe1 C29 C25 75.5(8) . . . . ? C34 Fe1 C29 C25 115.5(7) . . . . ? C32 Fe1 C29 C28 -48.8(16) . . . . ? C31 Fe1 C29 C28 164.4(15) . . . . ? C26 Fe1 C29 C28 83.2(8) . . . . ? C27 Fe1 C29 C28 36.7(7) . . . . ? C33 Fe1 C29 C28 -82.6(8) . . . . ? C25 Fe1 C29 C28 120.5(10) . . . . ? C30 Fe1 C29 C28 -164.0(7) . . . . ? C34 Fe1 C29 C28 -124.0(7) . . . . ? C32 Fe1 C30 C34 -81.0(2) . . . . ? C31 Fe1 C30 C34 -120.41(10) . . . . ? C26 Fe1 C30 C34 156.9(5) . . . . ? C27 Fe1 C30 C34 -170.5(12) . . . . ? C28 Fe1 C30 C34 40.6(11) . . . . ? C33 Fe1 C30 C34 -36.3(2) . . . . ? C29 Fe1 C30 C34 75.0(5) . . . . ? C25 Fe1 C30 C34 115.9(4) . . . . ? C32 Fe1 C30 C31 39.4(2) . . . . ? C26 Fe1 C30 C31 -82.7(5) . . . . ? C27 Fe1 C30 C31 -50.1(12) . . . . ? C28 Fe1 C30 C31 161.0(11) . . . . ? C33 Fe1 C30 C31 84.1(2) . . . . ? C29 Fe1 C30 C31 -164.6(5) . . . . ? C25 Fe1 C30 C31 -123.7(4) . . . . ? C34 Fe1 C30 C31 120.41(10) . . . . ? C34 C30 C31 C32 0.0 . . . . ? Fe1 C30 C31 C32 -59.3(3) . . . . ? C34 C30 C31 Fe1 59.3(3) . . . . ? C26 Fe1 C31 C32 -125.9(5) . . . . ? C27 Fe1 C31 C32 -81.2(5) . . . . ? C28 Fe1 C31 C32 -46.6(11) . . . . ? C33 Fe1 C31 C32 38.88(8) . . . . ? C29 Fe1 C31 C32 160.0(17) . . . . ? C25 Fe1 C31 C32 -167.0(6) . . . . ? C30 Fe1 C31 C32 118.0(2) . . . . ? C34 Fe1 C31 C32 81.74(17) . . . . ? C32 Fe1 C31 C30 -118.0(2) . . . . ? C26 Fe1 C31 C30 116.1(4) . . . . ? C27 Fe1 C31 C30 160.8(5) . . . . ? C28 Fe1 C31 C30 -164.6(12) . . . . ? C33 Fe1 C31 C30 -79.1(3) . . . . ? C29 Fe1 C31 C30 42.0(15) . . . . ? C25 Fe1 C31 C30 75.0(5) . . . . ? C34 Fe1 C31 C30 -36.26(11) . . . . ? C30 C31 C32 C33 0.0 . . . . ? Fe1 C31 C32 C33 -62.8(4) . . . . ? C30 C31 C32 Fe1 62.8(4) . . . . ? C31 Fe1 C32 C33 117.45(19) . . . . ? C26 Fe1 C32 C33 -167.2(6) . . . . ? C27 Fe1 C32 C33 -122.7(5) . . . . ? C28 Fe1 C32 C33 -82.0(6) . . . . ? C29 Fe1 C32 C33 -46.9(12) . . . . ? C25 Fe1 C32 C33 158.0(16) . . . . ? C30 Fe1 C32 C33 79.4(3) . . . . ? C34 Fe1 C32 C33 36.92(16) . . . . ? C26 Fe1 C32 C31 75.4(5) . . . . ? C27 Fe1 C32 C31 119.8(6) . . . . ? C28 Fe1 C32 C31 160.5(6) . . . . ? C33 Fe1 C32 C31 -117.45(19) . . . . ? C29 Fe1 C32 C31 -164.3(13) . . . . ? C25 Fe1 C32 C31 40.5(15) . . . . ? C30 Fe1 C32 C31 -38.06(14) . . . . ? C34 Fe1 C32 C31 -80.53(15) . . . . ? C31 C32 C33 C34 0.0 . . . . ? Fe1 C32 C33 C34 -61.2(2) . . . . ? C31 C32 C33 Fe1 61.2(2) . . . . ? C32 Fe1 C33 C34 119.32(16) . . . . ? C31 Fe1 C33 C34 79.82(18) . . . . ? C26 Fe1 C33 C34 164(2) . . . . ? C27 Fe1 C33 C34 -162.4(7) . . . . ? C28 Fe1 C33 C34 -124.7(5) . . . . ? C29 Fe1 C33 C34 -81.2(5) . . . . ? C25 Fe1 C33 C34 -46.9(8) . . . . ? C30 Fe1 C33 C34 35.95(17) . . . . ? C31 Fe1 C33 C32 -39.50(19) . . . . ? C26 Fe1 C33 C32 45(2) . . . . ? C27 Fe1 C33 C32 78.3(7) . . . . ? C28 Fe1 C33 C32 115.9(5) . . . . ? C29 Fe1 C33 C32 159.4(5) . . . . ? C25 Fe1 C33 C32 -166.3(9) . . . . ? C30 Fe1 C33 C32 -83.4(3) . . . . ? C34 Fe1 C33 C32 -119.32(17) . . . . ? C32 C33 C34 C30 0.0 . . . . ? Fe1 C33 C34 C30 -56.9(4) . . . . ? C32 C33 C34 Fe1 56.9(4) . . . . ? C31 C30 C34 C33 0.0 . . . . ? Fe1 C30 C34 C33 55.9(3) . . . . ? C31 C30 C34 Fe1 -55.9(3) . . . . ? C32 Fe1 C34 C33 -38.39(10) . . . . ? C31 Fe1 C34 C33 -83.99(19) . . . . ? C26 Fe1 C34 C33 -171.1(12) . . . . ? C27 Fe1 C34 C33 48.4(14) . . . . ? C28 Fe1 C34 C33 73.6(5) . . . . ? C29 Fe1 C34 C33 115.8(4) . . . . ? C25 Fe1 C34 C33 157.9(5) . . . . ? C30 Fe1 C34 C33 -121.4(2) . . . . ? C32 Fe1 C34 C30 83.0(3) . . . . ? C31 Fe1 C34 C30 37.38(11) . . . . ? C26 Fe1 C34 C30 -49.8(11) . . . . ? C27 Fe1 C34 C30 169.7(15) . . . . ? C28 Fe1 C34 C30 -165.0(4) . . . . ? C33 Fe1 C34 C30 121.4(2) . . . . ? C29 Fe1 C34 C30 -122.8(3) . . . . ? C25 Fe1 C34 C30 -80.8(4) . . . . ? N2 C24 C35 C39 -66.1(12) . . . . ? N2 C24 C35 C36 109.7(8) . . . . ? N2 C24 C35 Fe2 -159.4(6) . . . . ? C43 Fe2 C35 C39 -41.2(18) . . . . ? C44 Fe2 C35 C39 -71.3(8) . . . . ? C42 Fe2 C35 C39 172.4(8) . . . . ? C38 Fe2 C35 C39 35.8(7) . . . . ? C37 Fe2 C35 C39 80.3(7) . . . . ? C40 Fe2 C35 C39 -111.4(8) . . . . ? C41 Fe2 C35 C39 -153.7(7) . . . . ? C36 Fe2 C35 C39 121.1(7) . . . . ? C43 Fe2 C35 C36 -162.3(16) . . . . ? C44 Fe2 C35 C36 167.6(6) . . . . ? C42 Fe2 C35 C36 51.3(8) . . . . ? C38 Fe2 C35 C36 -85.3(5) . . . . ? C37 Fe2 C35 C36 -40.78(14) . . . . ? C40 Fe2 C35 C36 127.5(6) . . . . ? C39 Fe2 C35 C36 -121.1(7) . . . . ? C41 Fe2 C35 C36 85.2(6) . . . . ? C43 Fe2 C35 C24 80.0(19) . . . . ? C44 Fe2 C35 C24 49.9(10) . . . . ? C42 Fe2 C35 C24 -66.5(11) . . . . ? C38 Fe2 C35 C24 156.9(8) . . . . ? C37 Fe2 C35 C24 -158.5(7) . . . . ? C40 Fe2 C35 C24 9.7(9) . . . . ? C39 Fe2 C35 C24 121.1(10) . . . . ? C41 Fe2 C35 C24 -32.5(9) . . . . ? C36 Fe2 C35 C24 -117.8(8) . . . . ? C39 C35 C36 C37 -2.1(7) . . . . ? C24 C35 C36 C37 -178.4(6) . . . . ? Fe2 C35 C36 C37 58.5(3) . . . . ? C39 C35 C36 Fe2 -60.6(6) . . . . ? C24 C35 C36 Fe2 123.1(7) . . . . ? C43 Fe2 C36 C35 172.5(8) . . . . ? C44 Fe2 C36 C35 -46.7(17) . . . . ? C42 Fe2 C36 C35 -154.2(5) . . . . ? C38 Fe2 C36 C35 79.2(4) . . . . ? C37 Fe2 C36 C35 116.0(2) . . . . ? C40 Fe2 C36 C35 -73.1(6) . . . . ? C39 Fe2 C36 C35 36.5(4) . . . . ? C41 Fe2 C36 C35 -112.0(5) . . . . ? C43 Fe2 C36 C37 56.5(7) . . . . ? C44 Fe2 C36 C37 -162.7(18) . . . . ? C35 Fe2 C36 C37 -116.0(2) . . . . ? C42 Fe2 C36 C37 89.8(5) . . . . ? C38 Fe2 C36 C37 -36.8(4) . . . . ? C40 Fe2 C36 C37 171.0(6) . . . . ? C39 Fe2 C36 C37 -79.5(4) . . . . ? C41 Fe2 C36 C37 132.0(5) . . . . ? C35 C36 C37 C38 -0.2(6) . . . . ? Fe2 C36 C37 C38 58.1(6) . . . . ? C35 C36 C37 Fe2 -58.3(3) . . . . ? C43 Fe2 C37 C38 86.8(7) . . . . ? C44 Fe2 C37 C38 51.3(9) . . . . ? C35 Fe2 C37 C38 -81.4(5) . . . . ? C42 Fe2 C37 C38 130.5(7) . . . . ? C40 Fe2 C37 C38 -159.9(16) . . . . ? C39 Fe2 C37 C38 -37.7(6) . . . . ? C41 Fe2 C37 C38 169.9(6) . . . . ? C36 Fe2 C37 C38 -121.0(5) . . . . ? C43 Fe2 C37 C36 -152.2(5) . . . . ? C44 Fe2 C37 C36 172.2(8) . . . . ? C35 Fe2 C37 C36 39.54(12) . . . . ? C42 Fe2 C37 C36 -108.6(5) . . . . ? C38 Fe2 C37 C36 121.0(5) . . . . ? C40 Fe2 C37 C36 -39.0(16) . . . . ? C39 Fe2 C37 C36 83.3(4) . . . . ? C41 Fe2 C37 C36 -69.2(5) . . . . ? C36 C37 C38 C39 2.4(10) . . . . ? Fe2 C37 C38 C39 60.7(8) . . . . ? C36 C37 C38 Fe2 -58.2(3) . . . . ? C43 Fe2 C38 C39 131.2(8) . . . . ? C44 Fe2 C38 C39 87.6(8) . . . . ? C35 Fe2 C38 C39 -36.2(7) . . . . ? C42 Fe2 C38 C39 170.6(7) . . . . ? C37 Fe2 C38 C39 -118.4(9) . . . . ? C40 Fe2 C38 C39 54.1(11) . . . . ? C41 Fe2 C38 C39 -164(2) . . . . ? C36 Fe2 C38 C39 -80.4(7) . . . . ? C43 Fe2 C38 C37 -110.5(6) . . . . ? C44 Fe2 C38 C37 -154.0(5) . . . . ? C35 Fe2 C38 C37 82.1(5) . . . . ? C42 Fe2 C38 C37 -71.0(7) . . . . ? C40 Fe2 C38 C37 172.5(6) . . . . ? C39 Fe2 C38 C37 118.4(9) . . . . ? C41 Fe2 C38 C37 -46(3) . . . . ? C36 Fe2 C38 C37 38.0(3) . . . . ? C37 C38 C39 C35 -3.8(12) . . . . ? Fe2 C38 C39 C35 55.9(8) . . . . ? C37 C38 C39 Fe2 -59.7(7) . . . . ? C36 C35 C39 C38 3.8(11) . . . . ? C24 C35 C39 C38 180.0(9) . . . . ? Fe2 C35 C39 C38 -56.7(8) . . . . ? C36 C35 C39 Fe2 60.5(5) . . . . ? C24 C35 C39 Fe2 -123.4(8) . . . . ? C43 Fe2 C39 C38 -68.3(9) . . . . ? C44 Fe2 C39 C38 -109.0(8) . . . . ? C35 Fe2 C39 C38 122.1(10) . . . . ? C42 Fe2 C39 C38 -38(3) . . . . ? C37 Fe2 C39 C38 38.9(7) . . . . ? C40 Fe2 C39 C38 -151.9(7) . . . . ? C41 Fe2 C39 C38 174.3(9) . . . . ? C36 Fe2 C39 C38 84.9(7) . . . . ? C43 Fe2 C39 C35 169.5(6) . . . . ? C44 Fe2 C39 C35 128.9(6) . . . . ? C42 Fe2 C39 C35 -161(2) . . . . ? C38 Fe2 C39 C35 -122.1(10) . . . . ? C37 Fe2 C39 C35 -83.2(6) . . . . ? C40 Fe2 C39 C35 85.9(7) . . . . ? C41 Fe2 C39 C35 52.1(12) . . . . ? C36 Fe2 C39 C35 -37.2(4) . . . . ? C43 Fe2 C40 C41 81.3(3) . . . . ? C44 Fe2 C40 C41 119.7(2) . . . . ? C35 Fe2 C40 C41 -111.2(5) . . . . ? C42 Fe2 C40 C41 37.1(2) . . . . ? C38 Fe2 C40 C41 169.6(8) . . . . ? C37 Fe2 C40 C41 -36.6(16) . . . . ? C39 Fe2 C40 C41 -154.3(6) . . . . ? C36 Fe2 C40 C41 -69.4(5) . . . . ? C43 Fe2 C40 C44 -38.4(2) . . . . ? C35 Fe2 C40 C44 129.1(5) . . . . ? C42 Fe2 C40 C44 -82.6(3) . . . . ? C38 Fe2 C40 C44 49.9(8) . . . . ? C37 Fe2 C40 C44 -156.2(17) . . . . ? C39 Fe2 C40 C44 86.0(6) . . . . ? C41 Fe2 C40 C44 -119.7(2) . . . . ? C36 Fe2 C40 C44 171.0(5) . . . . ? C44 C40 C41 C42 0.0 . . . . ? Fe2 C40 C41 C42 -58.0(4) . . . . ? C44 C40 C41 Fe2 58.0(4) . . . . ? C43 Fe2 C41 C40 -82.0(3) . . . . ? C44 Fe2 C41 C40 -37.5(2) . . . . ? C35 Fe2 C41 C40 85.7(5) . . . . ? C42 Fe2 C41 C40 -120.0(2) . . . . ? C38 Fe2 C41 C40 -150(2) . . . . ? C37 Fe2 C41 C40 171.1(5) . . . . ? C39 Fe2 C41 C40 50.3(10) . . . . ? C36 Fe2 C41 C40 129.4(5) . . . . ? C43 Fe2 C41 C42 37.99(19) . . . . ? C44 Fe2 C41 C42 82.5(3) . . . . ? C35 Fe2 C41 C42 -154.3(5) . . . . ? C38 Fe2 C41 C42 -30(2) . . . . ? C37 Fe2 C41 C42 -68.9(5) . . . . ? C40 Fe2 C41 C42 120.0(2) . . . . ? C39 Fe2 C41 C42 170.4(10) . . . . ? C36 Fe2 C41 C42 -110.6(5) . . . . ? C40 C41 C42 C43 0.0 . . . . ? Fe2 C41 C42 C43 -58.5(4) . . . . ? C40 C41 C42 Fe2 58.5(4) . . . . ? C43 Fe2 C42 C41 -119.2(2) . . . . ? C44 Fe2 C42 C41 -80.7(3) . . . . ? C35 Fe2 C42 C41 50.4(7) . . . . ? C38 Fe2 C42 C41 173.0(7) . . . . ? C37 Fe2 C42 C41 131.6(5) . . . . ? C40 Fe2 C42 C41 -36.92(19) . . . . ? C39 Fe2 C42 C41 -155(2) . . . . ? C36 Fe2 C42 C41 85.6(5) . . . . ? C44 Fe2 C42 C43 38.5(2) . . . . ? C35 Fe2 C42 C43 169.6(7) . . . . ? C38 Fe2 C42 C43 -67.8(7) . . . . ? C37 Fe2 C42 C43 -109.3(5) . . . . ? C40 Fe2 C42 C43 82.3(3) . . . . ? C39 Fe2 C42 C43 -36(2) . . . . ? C41 Fe2 C42 C43 119.2(2) . . . . ? C36 Fe2 C42 C43 -155.2(5) . . . . ? C41 C42 C43 C44 0.0 . . . . ? Fe2 C42 C43 C44 -60.4(4) . . . . ? C41 C42 C43 Fe2 60.4(4) . . . . ? C35 Fe2 C43 C44 -36.6(16) . . . . ? C42 Fe2 C43 C44 118.3(2) . . . . ? C38 Fe2 C43 C44 -109.4(6) . . . . ? C37 Fe2 C43 C44 -153.4(5) . . . . ? C40 Fe2 C43 C44 37.84(19) . . . . ? C39 Fe2 C43 C44 -70.4(6) . . . . ? C41 Fe2 C43 C44 81.0(3) . . . . ? C36 Fe2 C43 C44 167.2(8) . . . . ? C44 Fe2 C43 C42 -118.3(2) . . . . ? C35 Fe2 C43 C42 -155.0(17) . . . . ? C38 Fe2 C43 C42 132.3(6) . . . . ? C37 Fe2 C43 C42 88.3(5) . . . . ? C40 Fe2 C43 C42 -80.5(3) . . . . ? C39 Fe2 C43 C42 171.2(6) . . . . ? C41 Fe2 C43 C42 -37.3(2) . . . . ? C36 Fe2 C43 C42 48.9(8) . . . . ? C42 C43 C44 C40 0.0 . . . . ? Fe2 C43 C44 C40 -61.0(4) . . . . ? C42 C43 C44 Fe2 61.0(4) . . . . ? C41 C40 C44 C43 0.0 . . . . ? Fe2 C40 C44 C43 59.5(4) . . . . ? C41 C40 C44 Fe2 -59.5(4) . . . . ? C35 Fe2 C44 C43 170.6(6) . . . . ? C42 Fe2 C44 C43 -38.21(18) . . . . ? C38 Fe2 C44 C43 87.4(5) . . . . ? C37 Fe2 C44 C43 52.3(8) . . . . ? C40 Fe2 C44 C43 -118.6(2) . . . . ? C39 Fe2 C44 C43 130.1(5) . . . . ? C41 Fe2 C44 C43 -81.6(3) . . . . ? C36 Fe2 C44 C43 -151.2(18) . . . . ? C43 Fe2 C44 C40 118.6(2) . . . . ? C35 Fe2 C44 C40 -70.8(5) . . . . ? C42 Fe2 C44 C40 80.4(3) . . . . ? C38 Fe2 C44 C40 -154.0(5) . . . . ? C37 Fe2 C44 C40 170.9(8) . . . . ? C39 Fe2 C44 C40 -111.3(5) . . . . ? C41 Fe2 C44 C40 37.03(18) . . . . ? C36 Fe2 C44 C40 -32.6(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.945 _refine_diff_density_min -2.099 _refine_diff_density_rms 0.289