# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address '' _publ_contact_author_email custelceanr@ornl.gov _publ_contact_author_name 'Radu Custelcean' _publ_author_name R.Custelcean data_c:\frames\469\work\469sq _database_code_depnum_ccdc_archive 'CCDC 879402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H1a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H80 N24 Ni O18 S' _chemical_formula_weight 1792.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.867(3) _cell_length_b 18.673(4) _cell_length_c 18.691(4) _cell_angle_alpha 74.412(4) _cell_angle_beta 77.467(4) _cell_angle_gamma 69.753(4) _cell_volume 4332.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1868 _exptl_absorpt_coefficient_mu 0.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9102 _exptl_absorpt_correction_T_max 0.9398 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41988 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15248 _reflns_number_gt 8114 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Crystal diffracted poorly due to its high content of disordered solvent, with very few reflections observed at 2theta > 45 degrees. Two DMF and one CH3CN solvent molecules could be located from the difference Fourier maps. The remaining electron density inside the crystal's pores, comprising 229 A(3), could not be assigned unambiguously, and was therefore treated with the SQUEEZE routine in PLATON. 49 residual electrons/unit cell were thus found, and their contribution was substracted from the hkl file. ; _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^)+(0.1612P)^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 15248 _refine_ls_number_parameters 1139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1407 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2797 _refine_ls_wR_factor_gt 0.2471 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.81919(6) 0.83743(4) 0.33012(3) 0.0760(3) Uani 1 1 d . . . S1 S 0.67272(9) 1.24988(8) 0.22812(6) 0.0620(4) Uani 1 1 d . . . O1 O 0.7405(3) 1.2901(2) 0.23822(18) 0.0724(10) Uani 1 1 d . . . N1 N 0.8832(4) 0.7611(3) 0.2558(2) 0.0782(13) Uani 1 1 d . . . C1 C 0.9661(5) 0.7736(3) 0.2085(3) 0.0756(16) Uani 1 1 d . . . O2 O 0.7193(3) 1.1640(2) 0.25300(19) 0.0773(10) Uani 1 1 d . . . N2 N 0.9356(3) 0.8827(3) 0.2638(2) 0.0671(12) Uani 1 1 d . . . C2 C 1.0242(5) 0.7237(4) 0.1593(3) 0.0851(18) Uani 1 1 d . . . H2 H 1.0841 0.7324 0.1270 0.102 Uiso 1 1 calc R . . O3 O 0.6603(2) 1.2668(2) 0.14833(17) 0.0732(10) Uani 1 1 d . . . N3 N 0.6951(5) 0.7927(3) 0.3771(3) 0.0915(16) Uani 1 1 d . . . C3 C 0.9913(6) 0.6618(4) 0.1595(4) 0.094(2) Uani 1 1 d . . . H3 H 1.0286 0.6274 0.1266 0.113 Uiso 1 1 calc R . . O4 O 0.5711(3) 1.2741(2) 0.27319(18) 0.0751(10) Uani 1 1 d . . . N4 N 0.7072(4) 0.9078(3) 0.2614(2) 0.0658(11) Uani 1 1 d . . . C4 C 0.9048(6) 0.6494(4) 0.2072(4) 0.0927(19) Uani 1 1 d . . . H4 H 0.8813 0.6073 0.2072 0.111 Uiso 1 1 calc R . . O5 O 0.8588(3) 1.0627(2) 0.0208(2) 0.0792(10) Uani 1 1 d . . . N5 N 0.9148(4) 0.7690(3) 0.4108(2) 0.0897(15) Uani 1 1 d . . . C5 C 0.8532(6) 0.7000(4) 0.2549(3) 0.0889(18) Uani 1 1 d . . . H5 H 0.7942 0.6914 0.2885 0.107 Uiso 1 1 calc R . . O6 O 0.8998(3) 1.4068(2) 0.00434(18) 0.0692(9) Uani 1 1 d . . . N6 N 0.7781(3) 0.9091(3) 0.4071(2) 0.0689(12) Uani 1 1 d . . . C6 C 0.9909(4) 0.8441(3) 0.2101(3) 0.0694(15) Uani 1 1 d . . . O7 O 0.4598(3) 1.0503(3) 0.3923(2) 0.1001(15) Uani 1 1 d . . . N7 N 0.9425(3) 1.1071(3) 0.2580(2) 0.0705(12) Uani 1 1 d . . . H7 H 0.8837 1.1298 0.2391 0.085 Uiso 1 1 calc R . . C7 C 1.0615(5) 0.8745(4) 0.1561(3) 0.0800(17) Uani 1 1 d . . . H7A H 1.1011 0.8471 0.1180 0.096 Uiso 1 1 calc R . . O8 O 0.3001(3) 1.3508(3) 0.1247(2) 0.0963(13) Uani 1 1 d . . . N8 N 0.8547(3) 1.1490(3) 0.3652(2) 0.0694(12) Uani 1 1 d . . . H8 H 0.7993 1.1659 0.3424 0.083 Uiso 1 1 calc R . . C8 C 1.0740(4) 0.9434(4) 0.1575(3) 0.0738(16) Uani 1 1 d . . . H8A H 1.1215 0.9644 0.1203 0.089 Uiso 1 1 calc R . . O9 O 1.0316(3) 1.0998(2) 0.3496(2) 0.0830(11) Uani 1 1 d . . . N9 N 0.7183(3) 1.2828(3) 0.4074(2) 0.0767(13) Uani 1 1 d . . . H9 H 0.7360 1.2765 0.3608 0.092 Uiso 1 1 calc R . . C9 C 1.0170(4) 0.9823(3) 0.2136(3) 0.0653(14) Uani 1 1 d . . . O10 O 0.6149(3) 1.3742(2) 0.47522(18) 0.0740(10) Uani 1 1 d . . . N10 N 0.5878(3) 1.3823(3) 0.3574(2) 0.0812(14) Uani 1 1 d . . . H10 H 0.6077 1.3563 0.3211 0.097 Uiso 1 1 calc R . . C10 C 0.9496(4) 0.9496(3) 0.2667(3) 0.0635(13) Uani 1 1 d . . . H10A H 0.9118 0.9751 0.3065 0.076 Uiso 1 1 calc R . . O11 O 0.2739(4) 1.7398(3) 0.0451(2) 0.1073(15) Uani 1 1 d . . . N11 N 0.7227(3) 1.1135(3) 0.1017(2) 0.0705(12) Uani 1 1 d . . . H11 H 0.6992 1.1428 0.1354 0.085 Uiso 1 1 calc R . . C11 C 1.0301(4) 1.0603(4) 0.2167(3) 0.0751(16) Uani 1 1 d . . . H11A H 1.0928 1.0491 0.2401 0.090 Uiso 1 1 calc R . . H11B H 1.0411 1.0905 0.1649 0.090 Uiso 1 1 calc R . . O12 O 0.4385(5) 1.7266(3) 0.0292(3) 0.1130(16) Uani 1 1 d . . . N12 N 0.8589(3) 1.1618(2) 0.0736(2) 0.0615(11) Uani 1 1 d . . . H12 H 0.8216 1.1913 0.1056 0.074 Uiso 1 1 calc R . . C12 C 0.9497(4) 1.1165(3) 0.3259(3) 0.0663(14) Uani 1 1 d . . . O13 O 0.2317(7) 1.6689(6) 0.2289(5) 0.279(7) Uani 1 1 d . . . N13 N 0.8968(3) 1.2921(3) 0.0875(2) 0.0649(11) Uani 1 1 d . . . H13 H 0.8654 1.2721 0.1305 0.078 Uiso 1 1 calc R . . C13 C 0.8420(4) 1.1566(3) 0.4400(3) 0.0720(15) Uani 1 1 d . . . O14 O 0.2276(8) 1.6979(5) 0.3285(5) 0.248(6) Uani 1 1 d . . . N14 N 0.8000(3) 1.4068(3) 0.1202(2) 0.0666(11) Uani 1 1 d . . . H14 H 0.7791 1.3749 0.1597 0.080 Uiso 1 1 calc R . . C14 C 0.8973(5) 1.0969(4) 0.4927(3) 0.0821(17) Uani 1 1 d . . . H14A H 0.9441 1.0508 0.4778 0.099 Uiso 1 1 calc R . . O15 O 0.6223(4) 1.7724(3) 0.0843(4) 0.1119(15) Uani 1 1 d . . . N15 N 0.5461(3) 1.1343(3) 0.3905(2) 0.0694(12) Uani 1 1 d . . . H15 H 0.5643 1.1757 0.3649 0.083 Uiso 1 1 calc R . . C15 C 0.8853(6) 1.1036(4) 0.5650(3) 0.105(2) Uani 1 1 d . . . H15A H 0.9207 1.0611 0.6006 0.126 Uiso 1 1 calc R . . O16 O 0.5781(5) 1.7340(3) 0.2017(4) 0.140(2) Uani 1 1 d . . . N16 N 0.4502(3) 1.1595(3) 0.2964(2) 0.0788(14) Uani 1 1 d . . . H16 H 0.4651 1.2038 0.2826 0.095 Uiso 1 1 calc R . . C16 C 0.8242(6) 1.1691(4) 0.5864(3) 0.121(3) Uani 1 1 d . . . H16A H 0.8203 1.1745 0.6361 0.145 Uiso 1 1 calc R . . N17 N 0.4440(3) 1.2487(3) 0.1536(2) 0.0725(13) Uani 1 1 d . . . H17 H 0.5115 1.2344 0.1537 0.087 Uiso 1 1 calc R . . C17 C 0.7651(6) 1.2309(4) 0.5353(3) 0.106(2) Uani 1 1 d . . . H17A H 0.7194 1.2769 0.5509 0.128 Uiso 1 1 calc R . . N18 N 0.4560(3) 1.3734(3) 0.1165(2) 0.0680(12) Uani 1 1 d . . . H18 H 0.5223 1.3487 0.1194 0.082 Uiso 1 1 calc R . . C18 C 0.7748(5) 1.2232(3) 0.4621(3) 0.0801(17) Uani 1 1 d . . . N19 N 0.2694(8) 1.6566(6) 0.2855(5) 0.220(6) Uani 1 1 d . . . C19 C 0.6401(4) 1.3482(3) 0.4194(3) 0.0610(13) Uani 1 1 d . . . N20 N 0.6208(5) 1.7217(4) 0.1413(4) 0.1008(17) Uani 1 1 d . . . C20 C 0.5081(4) 1.4521(4) 0.3452(3) 0.0753(16) Uani 1 1 d . . . N21 N 0.3649(5) 1.6997(3) 0.0433(3) 0.0875(15) Uani 1 1 d . . . C21 C 0.4565(5) 1.4647(5) 0.2845(3) 0.109(3) Uani 1 1 d . . . H21 H 0.4750 1.4252 0.2565 0.131 Uiso 1 1 calc R . . C22 C 0.3805(6) 1.5322(6) 0.2650(3) 0.137(4) Uani 1 1 d . . . H22 H 0.3483 1.5409 0.2221 0.165 Uiso 1 1 calc R . . C23 C 0.3518(6) 1.5849(5) 0.3051(4) 0.121(3) Uani 1 1 d . . . C24 C 0.3981(6) 1.5718(5) 0.3684(4) 0.126(3) Uani 1 1 d . . . H24 H 0.3741 1.6092 0.3992 0.151 Uiso 1 1 calc R . . C25 C 0.4774(5) 1.5058(4) 0.3865(3) 0.093(2) Uani 1 1 d . . . H25 H 0.5108 1.4981 0.4285 0.111 Uiso 1 1 calc R . . C26 C 0.6100(6) 0.8261(4) 0.3423(3) 0.0825(17) Uani 1 1 d . . . C27 C 0.5242(7) 0.8013(5) 0.3651(4) 0.110(2) Uani 1 1 d . . . H27 H 0.4664 0.8259 0.3382 0.132 Uiso 1 1 calc R . . C28 C 0.5201(10) 0.7432(7) 0.4244(6) 0.142(4) Uani 1 1 d . . . H28 H 0.4602 0.7262 0.4395 0.170 Uiso 1 1 calc R . . C29 C 0.6007(10) 0.7094(5) 0.4622(5) 0.138(4) Uani 1 1 d . . . H29 H 0.5978 0.6689 0.5053 0.165 Uiso 1 1 calc R . . C30 C 0.6923(7) 0.7337(4) 0.4385(4) 0.117(3) Uani 1 1 d . . . H30 H 0.7504 0.7089 0.4651 0.141 Uiso 1 1 calc R . . C31 C 0.6186(5) 0.8904(4) 0.2764(3) 0.0746(15) Uani 1 1 d . . . C32 C 0.5439(6) 0.9275(5) 0.2324(4) 0.107(2) Uani 1 1 d . . . H32 H 0.4827 0.9123 0.2427 0.129 Uiso 1 1 calc R . . C33 C 0.5544(5) 0.9857(4) 0.1742(4) 0.097(2) Uani 1 1 d . . . H33 H 0.4997 1.0121 0.1445 0.116 Uiso 1 1 calc R . . C34 C 0.6416(4) 1.0078(3) 0.1566(3) 0.0693(14) Uani 1 1 d . . . C35 C 0.7177(4) 0.9656(3) 0.2032(2) 0.0599(12) Uani 1 1 d . . . H35 H 0.7804 0.9787 0.1929 0.072 Uiso 1 1 calc R . . C36 C 0.6587(4) 1.0716(3) 0.0907(3) 0.0727(15) Uani 1 1 d . . . H36A H 0.6914 1.0483 0.0463 0.087 Uiso 1 1 calc R . . H36B H 0.5904 1.1094 0.0798 0.087 Uiso 1 1 calc R . . C37 C 0.8168(4) 1.1092(3) 0.0622(3) 0.0614(13) Uani 1 1 d . . . C38 C 0.9548(4) 1.1729(3) 0.0396(2) 0.0589(13) Uani 1 1 d . . . C39 C 1.0330(4) 1.1177(3) 0.0035(3) 0.0616(13) Uani 1 1 d . . . H39 H 1.0224 1.0712 0.0001 0.074 Uiso 1 1 calc R . . C40 C 1.1275(4) 1.1333(3) -0.0274(3) 0.0694(15) Uani 1 1 d . . . H40 H 1.1809 1.0967 -0.0524 0.083 Uiso 1 1 calc R . . C41 C 1.1446(4) 1.1999(4) -0.0225(3) 0.0752(15) Uani 1 1 d . . . H41 H 1.2087 1.2094 -0.0446 0.090 Uiso 1 1 calc R . . C42 C 1.0695(4) 1.2523(3) 0.0141(3) 0.0704(14) Uani 1 1 d . . . H42 H 1.0819 1.2978 0.0184 0.085 Uiso 1 1 calc R . . C43 C 0.9730(4) 1.2392(3) 0.0457(3) 0.0595(13) Uani 1 1 d . . . C44 C 0.8687(4) 1.3724(3) 0.0653(3) 0.0601(12) Uani 1 1 d . . . C45 C 0.7589(4) 1.4864(3) 0.1215(3) 0.0636(13) Uani 1 1 d . . . C46 C 0.7015(4) 1.5044(4) 0.1887(3) 0.0776(16) Uani 1 1 d . . . H46 H 0.6938 1.4637 0.2305 0.093 Uiso 1 1 calc R . . C47 C 0.6559(5) 1.5808(4) 0.1946(3) 0.0849(18) Uani 1 1 d . . . H47 H 0.6150 1.5932 0.2400 0.102 Uiso 1 1 calc R . . C48 C 0.6694(4) 1.6393(4) 0.1348(3) 0.0783(16) Uani 1 1 d . . . C49 C 0.7282(4) 1.6233(4) 0.0676(3) 0.0750(15) Uani 1 1 d . . . H49 H 0.7375 1.6647 0.0269 0.090 Uiso 1 1 calc R . . C50 C 0.7732(4) 1.5468(3) 0.0604(3) 0.0687(14) Uani 1 1 d . . . H50 H 0.8134 1.5349 0.0146 0.082 Uiso 1 1 calc R . . C51 C 0.9078(5) 0.8038(4) 0.4680(3) 0.0848(18) Uani 1 1 d . . . C52 C 0.9689(6) 0.7627(4) 0.5264(3) 0.104(2) Uani 1 1 d . . . H52 H 0.9648 0.7866 0.5664 0.125 Uiso 1 1 calc R . . C53 C 1.0329(8) 0.6897(5) 0.5254(4) 0.150(4) Uani 1 1 d . . . H53 H 1.0758 0.6629 0.5637 0.180 Uiso 1 1 calc R . . C54 C 1.0363(8) 0.6535(5) 0.4682(4) 0.159(4) Uani 1 1 d . . . H54 H 1.0765 0.6006 0.4686 0.191 Uiso 1 1 calc R . . C55 C 0.9790(7) 0.6977(4) 0.4112(4) 0.129(3) Uani 1 1 d . . . H55 H 0.9860 0.6755 0.3695 0.155 Uiso 1 1 calc R . . C56 C 0.8326(4) 0.8808(3) 0.4665(3) 0.0704(15) Uani 1 1 d . . . C57 C 0.8144(4) 0.9235(3) 0.5205(3) 0.0724(15) Uani 1 1 d . . . H57 H 0.8563 0.9047 0.5596 0.087 Uiso 1 1 calc R . . C58 C 0.7360(4) 0.9932(3) 0.5179(3) 0.0679(14) Uani 1 1 d . . . H58 H 0.7231 1.0224 0.5553 0.081 Uiso 1 1 calc R . . C59 C 0.6754(4) 1.0206(3) 0.4598(2) 0.0586(12) Uani 1 1 d . . . C60 C 0.7010(4) 0.9781(3) 0.4056(3) 0.0662(14) Uani 1 1 d . . . H60 H 0.6626 0.9980 0.3643 0.079 Uiso 1 1 calc R . . C61 C 0.5826(4) 1.0927(3) 0.4621(3) 0.0698(14) Uani 1 1 d . . . H61A H 0.5248 1.0774 0.4969 0.084 Uiso 1 1 calc R . . H61B H 0.6003 1.1291 0.4831 0.084 Uiso 1 1 calc R . . C62 C 0.4838(4) 1.1086(4) 0.3636(3) 0.0756(16) Uani 1 1 d . . . C63 C 0.3946(4) 1.1448(4) 0.2496(3) 0.0840(18) Uani 1 1 d . . . C64 C 0.3434(5) 1.0903(5) 0.2709(4) 0.114(3) Uani 1 1 d . . . H64 H 0.3440 1.0596 0.3205 0.137 Uiso 1 1 calc R . . C65 C 0.2907(6) 1.0784(6) 0.2225(5) 0.138(3) Uani 1 1 d . . . H65 H 0.2546 1.0406 0.2393 0.166 Uiso 1 1 calc R . . C66 C 0.2904(6) 1.1214(5) 0.1498(4) 0.123(3) Uani 1 1 d . . . H66 H 0.2544 1.1135 0.1162 0.148 Uiso 1 1 calc R . . C67 C 0.3424(5) 1.1754(5) 0.1270(4) 0.102(2) Uani 1 1 d . . . H67 H 0.3443 1.2035 0.0764 0.122 Uiso 1 1 calc R . . C68 C 0.3939(4) 1.1909(4) 0.1765(3) 0.0834(18) Uani 1 1 d . . . C69 C 0.3920(4) 1.3264(4) 0.1310(3) 0.0697(15) Uani 1 1 d . . . C70 C 0.4287(4) 1.4540(3) 0.0982(2) 0.0628(14) Uani 1 1 d . . . C71 C 0.5058(4) 1.4871(4) 0.0917(3) 0.0684(15) Uani 1 1 d . . . H71 H 0.5738 1.4542 0.1000 0.082 Uiso 1 1 calc R . . C72 C 0.4863(4) 1.5670(3) 0.0733(3) 0.0697(14) Uani 1 1 d . . . H72 H 0.5403 1.5891 0.0683 0.084 Uiso 1 1 calc R . . C73 C 0.3873(4) 1.6141(3) 0.0623(3) 0.0718(15) Uani 1 1 d . . . C74 C 0.3094(4) 1.5826(4) 0.0679(3) 0.0764(17) Uani 1 1 d . . . H74 H 0.2417 1.6162 0.0595 0.092 Uiso 1 1 calc R . . C75 C 0.3280(4) 1.5031(4) 0.0856(3) 0.0712(15) Uani 1 1 d . . . H75 H 0.2738 1.4816 0.0892 0.085 Uiso 1 1 calc R . . O1S O 0.8783(5) 1.3987(4) 0.2913(4) 0.157(3) Uani 1 1 d . . . N1S N 1.0174(5) 1.3411(6) 0.2168(4) 0.126(3) Uani 1 1 d . . . C1S C 0.9416(8) 1.3419(7) 0.2757(6) 0.130(3) Uani 1 1 d . . . H1S H 0.9388 1.2931 0.3070 0.156 Uiso 1 1 calc R . . O2S O 1.2404(7) 1.4257(6) 0.4487(4) 0.200(4) Uani 1 1 d . . . N2S N 1.2019(7) 1.4085(7) 0.3429(5) 0.165(3) Uani 1 1 d . . . C2S C 1.0352(7) 1.4099(6) 0.1550(5) 0.130(3) Uani 1 1 d . . . H2S1 H 1.0096 1.4108 0.1098 0.195 Uiso 1 1 calc R . . H2S2 H 1.1096 1.4041 0.1438 0.195 Uiso 1 1 calc R . . H2S3 H 0.9979 1.4588 0.1721 0.195 Uiso 1 1 calc R . . N3S N 0.9227(9) 1.5389(5) 0.3896(6) 0.170(3) Uani 1 1 d . . . C3S C 1.0922(6) 1.2656(5) 0.2112(5) 0.124(3) Uani 1 1 d . . . H3S1 H 1.0780 1.2264 0.2554 0.187 Uiso 1 1 calc R . . H3S2 H 1.1623 1.2682 0.2086 0.187 Uiso 1 1 calc R . . H3S3 H 1.0869 1.2511 0.1659 0.187 Uiso 1 1 calc R . . C4S C 1.1884(10) 1.4501(8) 0.3969(6) 0.161(4) Uani 1 1 d . . . H4S H 1.1368 1.4996 0.3939 0.193 Uiso 1 1 calc R . . C5S C 1.2763(14) 1.3369(10) 0.3388(9) 0.238(7) Uiso 1 1 d . . . H5S1 H 1.3156 1.3198 0.3813 0.357 Uiso 1 1 calc R . . H5S2 H 1.3236 1.3419 0.2918 0.357 Uiso 1 1 calc R . . H5S3 H 1.2422 1.2983 0.3406 0.357 Uiso 1 1 calc R . . C6S C 1.1390(15) 1.4535(12) 0.2782(11) 0.277(8) Uiso 1 1 d . . . H6S1 H 1.0855 1.4298 0.2797 0.415 Uiso 1 1 calc R . . H6S2 H 1.1851 1.4518 0.2305 0.415 Uiso 1 1 calc R . . H6S3 H 1.1059 1.5080 0.2831 0.415 Uiso 1 1 calc R . . C7S C 0.7507(8) 1.5118(6) 0.4084(7) 0.163(4) Uani 1 1 d . . . H7S1 H 0.7214 1.5071 0.4615 0.245 Uiso 1 1 calc R . . H7S2 H 0.7605 1.4633 0.3930 0.245 Uiso 1 1 calc R . . H7S3 H 0.7032 1.5554 0.3782 0.245 Uiso 1 1 calc R . . C8S C 0.8416(10) 1.5246(5) 0.3984(6) 0.136(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0943(6) 0.0733(5) 0.0403(4) -0.0001(3) -0.0218(3) -0.0024(4) S1 0.0474(7) 0.0836(9) 0.0398(6) 0.0003(6) -0.0197(5) -0.0032(6) O1 0.071(2) 0.087(3) 0.0486(19) 0.0104(17) -0.0208(16) -0.022(2) N1 0.085(3) 0.078(3) 0.053(3) -0.009(2) -0.017(2) -0.002(3) C1 0.086(4) 0.072(4) 0.048(3) -0.008(3) -0.035(3) 0.014(3) O2 0.064(2) 0.083(3) 0.063(2) 0.0088(19) -0.0264(17) -0.0035(19) N2 0.065(3) 0.070(3) 0.045(2) -0.005(2) -0.0286(19) 0.012(2) C2 0.089(4) 0.081(4) 0.058(3) -0.006(3) -0.026(3) 0.010(4) O3 0.060(2) 0.093(3) 0.0447(17) -0.0054(17) -0.0284(15) 0.0100(19) N3 0.127(5) 0.082(3) 0.046(2) -0.009(2) 0.007(3) -0.022(3) C3 0.109(5) 0.082(5) 0.063(4) -0.012(3) -0.030(4) 0.014(4) O4 0.060(2) 0.105(3) 0.0510(19) -0.0164(19) -0.0079(16) -0.014(2) N4 0.078(3) 0.079(3) 0.037(2) -0.008(2) -0.0115(19) -0.021(2) C4 0.107(5) 0.090(5) 0.068(4) -0.012(3) -0.023(4) -0.011(4) O5 0.069(2) 0.080(3) 0.081(3) -0.026(2) -0.009(2) -0.007(2) N5 0.118(4) 0.069(3) 0.053(3) -0.005(2) -0.031(3) 0.013(3) C5 0.106(5) 0.084(4) 0.061(4) -0.014(3) -0.014(3) -0.010(4) O6 0.067(2) 0.073(2) 0.0488(19) -0.0006(17) -0.0114(16) -0.0053(18) N6 0.077(3) 0.078(3) 0.035(2) 0.0009(19) -0.0190(19) -0.005(2) C6 0.064(3) 0.076(4) 0.039(3) 0.004(3) -0.024(2) 0.012(3) O7 0.091(3) 0.130(4) 0.069(3) 0.036(3) -0.026(2) -0.055(3) N7 0.057(2) 0.082(3) 0.057(2) -0.010(2) -0.030(2) 0.007(2) C7 0.079(4) 0.082(4) 0.054(3) -0.010(3) -0.027(3) 0.015(3) O8 0.048(2) 0.125(4) 0.102(3) -0.004(3) -0.028(2) -0.014(2) N8 0.067(3) 0.076(3) 0.048(2) 0.000(2) -0.028(2) 0.001(2) C8 0.061(3) 0.080(4) 0.057(3) 0.002(3) -0.024(3) 0.004(3) O9 0.063(2) 0.105(3) 0.065(2) -0.010(2) -0.0387(18) 0.005(2) N9 0.078(3) 0.084(3) 0.037(2) 0.002(2) -0.0253(19) 0.013(3) C9 0.052(3) 0.066(3) 0.059(3) -0.004(3) -0.035(2) 0.013(3) O10 0.089(3) 0.074(2) 0.0406(18) -0.0035(17) -0.0296(17) 0.002(2) N10 0.082(3) 0.090(3) 0.040(2) -0.011(2) -0.031(2) 0.024(3) C10 0.059(3) 0.071(4) 0.047(3) 0.001(2) -0.027(2) -0.001(3) O11 0.090(3) 0.103(3) 0.078(3) 0.005(2) -0.038(2) 0.031(3) N11 0.062(3) 0.082(3) 0.057(2) -0.003(2) -0.018(2) -0.013(2) C11 0.045(3) 0.102(5) 0.055(3) -0.003(3) -0.022(2) 0.004(3) O12 0.106(4) 0.096(4) 0.113(4) 0.002(3) -0.032(3) -0.009(3) N12 0.056(2) 0.063(3) 0.050(2) 0.0015(19) -0.0157(19) -0.006(2) C12 0.065(3) 0.066(3) 0.053(3) 0.005(2) -0.030(3) -0.002(3) O13 0.267(9) 0.289(10) 0.184(7) -0.124(7) -0.174(7) 0.176(8) N13 0.061(2) 0.068(3) 0.051(2) -0.003(2) -0.0144(19) -0.005(2) C13 0.074(3) 0.073(4) 0.048(3) 0.001(2) -0.025(2) 0.003(3) O14 0.328(11) 0.171(7) 0.182(7) -0.108(6) -0.161(7) 0.132(7) N14 0.063(2) 0.070(3) 0.050(2) -0.003(2) -0.0162(19) -0.002(2) C14 0.086(4) 0.079(4) 0.052(3) 0.004(3) -0.034(3) 0.013(3) O15 0.096(3) 0.084(3) 0.137(5) -0.017(3) -0.011(3) -0.013(3) N15 0.062(3) 0.079(3) 0.048(2) 0.002(2) -0.019(2) -0.003(2) C15 0.124(5) 0.089(5) 0.061(4) 0.002(3) -0.047(4) 0.024(4) O16 0.166(5) 0.100(4) 0.128(5) -0.046(4) -0.016(4) 0.007(4) N16 0.062(3) 0.108(4) 0.052(2) 0.016(2) -0.024(2) -0.022(3) C16 0.145(6) 0.109(6) 0.048(3) -0.002(3) -0.040(4) 0.041(5) N17 0.052(2) 0.098(4) 0.054(2) 0.015(2) -0.0251(19) -0.019(3) C17 0.124(5) 0.102(5) 0.042(3) -0.004(3) -0.036(3) 0.034(4) N18 0.043(2) 0.087(3) 0.053(2) 0.005(2) -0.0235(18) 0.000(2) C18 0.088(4) 0.082(4) 0.043(3) 0.010(3) -0.029(3) 0.004(3) N19 0.238(10) 0.211(9) 0.137(6) -0.102(7) -0.135(7) 0.138(8) C19 0.056(3) 0.073(3) 0.041(3) 0.008(2) -0.018(2) -0.012(3) N20 0.094(4) 0.094(5) 0.097(4) -0.031(4) -0.013(3) 0.002(3) C20 0.066(3) 0.094(4) 0.034(2) -0.003(3) -0.021(2) 0.015(3) N21 0.089(4) 0.081(4) 0.061(3) 0.000(3) -0.028(3) 0.011(3) C21 0.088(4) 0.152(6) 0.046(3) -0.025(3) -0.033(3) 0.033(4) C22 0.105(5) 0.181(8) 0.052(3) -0.037(4) -0.036(3) 0.071(5) C23 0.120(6) 0.122(6) 0.079(4) -0.032(4) -0.058(4) 0.051(5) C24 0.147(7) 0.119(6) 0.075(4) -0.032(4) -0.062(4) 0.043(5) C25 0.110(5) 0.085(4) 0.054(3) -0.013(3) -0.044(3) 0.025(4) C26 0.111(5) 0.087(4) 0.054(3) -0.021(3) -0.004(3) -0.036(4) C27 0.135(6) 0.117(6) 0.076(4) -0.018(4) 0.027(4) -0.065(5) C28 0.173(10) 0.137(8) 0.094(6) -0.021(6) 0.019(7) -0.046(8) C29 0.196(10) 0.098(6) 0.082(6) 0.005(5) 0.048(7) -0.059(7) C30 0.162(7) 0.092(5) 0.057(4) 0.004(3) 0.004(4) -0.014(5) C31 0.090(4) 0.087(4) 0.051(3) -0.011(3) -0.004(3) -0.038(4) C32 0.091(5) 0.152(7) 0.093(5) 0.003(5) -0.032(4) -0.065(5) C33 0.078(4) 0.136(6) 0.076(4) 0.018(4) -0.037(3) -0.048(4) C34 0.063(3) 0.093(4) 0.047(3) -0.005(3) -0.022(2) -0.017(3) C35 0.052(3) 0.080(3) 0.044(3) -0.007(2) -0.010(2) -0.019(3) C36 0.055(3) 0.093(4) 0.054(3) -0.006(3) -0.021(2) -0.002(3) C37 0.053(3) 0.064(3) 0.048(3) 0.010(2) -0.023(2) -0.001(3) C38 0.052(3) 0.067(3) 0.043(2) 0.011(2) -0.026(2) -0.006(3) C39 0.065(3) 0.057(3) 0.051(3) -0.001(2) -0.022(2) -0.003(3) C40 0.060(3) 0.070(4) 0.055(3) -0.001(3) -0.021(2) 0.006(3) C41 0.056(3) 0.089(4) 0.067(3) -0.005(3) -0.015(3) -0.010(3) C42 0.063(3) 0.078(4) 0.061(3) -0.005(3) -0.020(3) -0.009(3) C43 0.056(3) 0.064(3) 0.045(3) 0.002(2) -0.018(2) -0.005(3) C44 0.051(3) 0.070(3) 0.049(3) -0.004(3) -0.016(2) -0.007(3) C45 0.055(3) 0.069(3) 0.055(3) -0.005(3) -0.023(2) -0.001(3) C46 0.073(3) 0.081(4) 0.056(3) -0.009(3) -0.020(3) 0.008(3) C47 0.075(4) 0.097(5) 0.059(3) -0.017(3) -0.017(3) 0.007(3) C48 0.072(4) 0.076(4) 0.079(4) -0.025(3) -0.024(3) 0.001(3) C49 0.064(3) 0.075(4) 0.079(4) -0.003(3) -0.022(3) -0.015(3) C50 0.057(3) 0.076(4) 0.059(3) -0.008(3) -0.017(2) -0.002(3) C51 0.101(4) 0.077(4) 0.048(3) -0.002(3) -0.030(3) 0.011(3) C52 0.139(6) 0.082(4) 0.055(3) 0.003(3) -0.048(4) 0.019(4) C53 0.206(9) 0.104(6) 0.079(5) -0.013(4) -0.082(5) 0.061(6) C54 0.220(10) 0.104(6) 0.092(5) -0.020(5) -0.088(6) 0.066(6) C55 0.197(8) 0.085(5) 0.065(4) -0.017(4) -0.047(5) 0.026(5) C56 0.088(4) 0.066(3) 0.038(2) 0.009(2) -0.022(2) -0.007(3) C57 0.083(4) 0.084(4) 0.039(3) 0.004(3) -0.024(2) -0.015(3) C58 0.075(3) 0.075(4) 0.039(2) 0.001(2) -0.017(2) -0.010(3) C59 0.064(3) 0.062(3) 0.036(2) 0.000(2) -0.012(2) -0.009(3) C60 0.071(3) 0.071(3) 0.040(2) 0.006(2) -0.016(2) -0.010(3) C61 0.070(3) 0.082(4) 0.037(2) 0.008(2) -0.012(2) -0.010(3) C62 0.063(3) 0.103(5) 0.041(3) 0.014(3) -0.003(2) -0.025(3) C63 0.054(3) 0.118(5) 0.066(3) 0.013(3) -0.014(3) -0.030(4) C64 0.079(4) 0.165(7) 0.084(4) 0.027(5) -0.029(4) -0.049(5) C65 0.110(6) 0.206(10) 0.107(6) 0.024(6) -0.050(5) -0.080(6) C66 0.105(5) 0.165(8) 0.112(6) 0.025(5) -0.062(5) -0.071(6) C67 0.085(4) 0.139(6) 0.072(4) 0.026(4) -0.040(3) -0.041(5) C68 0.060(3) 0.118(5) 0.060(3) 0.013(3) -0.027(3) -0.026(4) C69 0.042(3) 0.105(4) 0.046(3) 0.001(3) -0.016(2) -0.010(3) C70 0.051(3) 0.080(4) 0.039(2) 0.003(2) -0.020(2) -0.001(3) C71 0.047(3) 0.094(4) 0.045(3) 0.002(3) -0.021(2) -0.001(3) C72 0.063(3) 0.083(4) 0.045(3) 0.003(3) -0.025(2) -0.002(3) C73 0.064(3) 0.082(4) 0.047(3) 0.001(3) -0.024(2) 0.005(3) C74 0.058(3) 0.095(5) 0.046(3) -0.004(3) -0.023(2) 0.014(3) C75 0.045(3) 0.098(4) 0.047(3) 0.001(3) -0.024(2) 0.005(3) O1S 0.115(4) 0.161(6) 0.187(6) -0.086(5) -0.077(4) 0.038(4) N1S 0.076(4) 0.201(9) 0.107(5) -0.054(6) -0.020(4) -0.028(5) C1S 0.121(7) 0.153(9) 0.121(7) -0.032(6) -0.060(6) -0.018(7) O2S 0.222(8) 0.246(9) 0.109(5) -0.046(5) -0.054(5) -0.017(7) N2S 0.126(6) 0.236(10) 0.119(6) -0.071(7) 0.001(5) -0.024(7) C2S 0.111(6) 0.143(7) 0.131(7) -0.025(6) -0.038(5) -0.021(6) N3S 0.176(9) 0.145(7) 0.169(8) 0.002(6) -0.020(7) -0.055(7) C3S 0.094(5) 0.125(7) 0.150(7) -0.032(6) -0.040(5) -0.011(5) C4S 0.195(11) 0.189(11) 0.094(6) -0.045(7) -0.022(7) -0.039(9) C7S 0.111(7) 0.143(9) 0.231(13) -0.037(8) -0.033(7) -0.029(7) C8S 0.126(8) 0.085(6) 0.165(9) 0.007(5) -0.021(7) -0.017(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 Ni1 N5 2.079(5) . ? Ni1 N4 2.082(4) . ? Ni1 N6 2.082(4) . ? Ni1 N2 2.090(5) . ? Ni1 N3 2.091(6) . ? Ni1 N1 2.099(5) . ? S1 O1 1.457(4) . ? S1 O4 1.466(4) . ? S1 O3 1.474(3) . ? S1 O2 1.489(4) . ? N1 C1 1.339(8) . ? N1 C5 1.346(8) . ? C1 C2 1.407(8) . ? C1 C6 1.480(9) . ? N2 C6 1.338(7) . ? N2 C10 1.344(7) . ? C2 C3 1.382(9) . ? N3 C26 1.347(8) . ? N3 C30 1.365(8) . ? C3 C4 1.380(9) . ? N4 C31 1.331(7) . ? N4 C35 1.334(6) . ? C4 C5 1.382(9) . ? O5 C37 1.227(6) . ? N5 C55 1.320(8) . ? N5 C51 1.363(7) . ? O6 C44 1.218(6) . ? N6 C60 1.358(6) . ? N6 C56 1.362(6) . ? C6 C7 1.396(8) . ? O7 C62 1.201(7) . ? N7 C12 1.356(6) . ? N7 C11 1.433(6) . ? C7 C8 1.364(8) . ? O8 C69 1.217(6) . ? N8 C12 1.383(7) . ? N8 C13 1.410(6) . ? C8 C9 1.379(7) . ? O9 C12 1.217(6) . ? N9 C19 1.358(7) . ? N9 C18 1.424(6) . ? C9 C10 1.378(7) . ? C9 C11 1.547(8) . ? O10 C19 1.201(6) . ? N10 C19 1.387(6) . ? N10 C20 1.387(6) . ? O11 N21 1.223(6) . ? N11 C37 1.339(6) . ? N11 C36 1.445(7) . ? O12 N21 1.238(7) . ? N12 C37 1.383(7) . ? N12 C38 1.404(6) . ? O13 N19 1.213(9) . ? N13 C44 1.378(6) . ? N13 C43 1.428(6) . ? C13 C18 1.375(8) . ? C13 C14 1.395(7) . ? O14 N19 1.183(9) . ? N14 C44 1.372(6) . ? N14 C45 1.399(6) . ? C14 C15 1.360(8) . ? O15 N20 1.222(7) . ? N15 C62 1.354(7) . ? N15 C61 1.453(6) . ? C15 C16 1.332(9) . ? O16 N20 1.197(7) . ? N16 C63 1.415(8) . ? N16 C62 1.416(6) . ? C16 C17 1.417(8) . ? N17 C69 1.373(7) . ? N17 C68 1.404(7) . ? C17 C18 1.387(8) . ? N18 C70 1.382(7) . ? N18 C69 1.392(7) . ? N19 C23 1.446(10) . ? N20 C48 1.478(8) . ? C20 C25 1.326(8) . ? C20 C21 1.395(8) . ? N21 C73 1.477(8) . ? C21 C22 1.355(9) . ? C22 C23 1.299(10) . ? C23 C24 1.393(9) . ? C24 C25 1.357(9) . ? C26 C27 1.366(9) . ? C26 C31 1.487(8) . ? C27 C28 1.334(12) . ? C28 C29 1.327(14) . ? C29 C30 1.436(13) . ? C31 C32 1.339(9) . ? C32 C33 1.340(9) . ? C33 C34 1.356(8) . ? C34 C35 1.396(7) . ? C34 C36 1.508(7) . ? C38 C43 1.382(7) . ? C38 C39 1.406(7) . ? C39 C40 1.407(7) . ? C40 C41 1.374(8) . ? C41 C42 1.362(8) . ? C42 C43 1.416(7) . ? C45 C46 1.390(7) . ? C45 C50 1.407(7) . ? C46 C47 1.371(8) . ? C47 C48 1.368(9) . ? C48 C49 1.385(8) . ? C49 C50 1.378(8) . ? C51 C52 1.414(8) . ? C51 C56 1.453(8) . ? C52 C53 1.347(9) . ? C53 C54 1.395(11) . ? C54 C55 1.375(10) . ? C56 C57 1.378(7) . ? C57 C58 1.373(7) . ? C58 C59 1.396(7) . ? C59 C60 1.365(7) . ? C59 C61 1.510(7) . ? C63 C64 1.363(9) . ? C63 C68 1.405(8) . ? C64 C65 1.382(11) . ? C65 C66 1.380(10) . ? C66 C67 1.362(9) . ? C67 C68 1.423(9) . ? C70 C71 1.378(7) . ? C70 C75 1.410(7) . ? C71 C72 1.379(8) . ? C72 C73 1.375(7) . ? C73 C74 1.370(8) . ? C74 C75 1.373(8) . ? O1S C1S 1.180(10) . ? N1S C1S 1.347(11) . ? N1S C3S 1.447(10) . ? N1S C2S 1.531(11) . ? O2S C4S 1.225(12) . ? N2S C4S 1.378(12) . ? N2S C5S 1.387(16) . ? N2S C6S 1.53(2) . ? N3S C8S 1.210(13) . ? C7S C8S 1.329(13) . ? 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 N5 Ni1 N4 172.23(18) . . ? N5 Ni1 N6 78.72(18) . . ? N4 Ni1 N6 96.13(16) . . ? N5 Ni1 N2 92.53(19) . . ? N4 Ni1 N2 93.80(16) . . ? N6 Ni1 N2 95.97(18) . . ? N5 Ni1 N3 96.1(2) . . ? N4 Ni1 N3 78.1(2) . . ? N6 Ni1 N3 92.06(18) . . ? N2 Ni1 N3 169.20(19) . . ? N5 Ni1 N1 94.65(19) . . ? N4 Ni1 N1 90.99(17) . . ? N6 Ni1 N1 171.50(19) . . ? N2 Ni1 N1 78.9(2) . . ? N3 Ni1 N1 94.0(2) . . ? O1 S1 O4 110.2(2) . . ? O1 S1 O3 110.2(2) . . ? O4 S1 O3 109.9(2) . . ? O1 S1 O2 109.6(2) . . ? O4 S1 O2 108.5(2) . . ? O3 S1 O2 108.3(2) . . ? C1 N1 C5 119.0(5) . . ? C1 N1 Ni1 114.3(4) . . ? C5 N1 Ni1 126.7(4) . . ? N1 C1 C2 121.9(6) . . ? N1 C1 C6 115.7(5) . . ? C2 C1 C6 122.4(6) . . ? C6 N2 C10 120.1(5) . . ? C6 N2 Ni1 114.2(4) . . ? C10 N2 Ni1 125.2(4) . . ? C3 C2 C1 117.8(7) . . ? C26 N3 C30 117.5(7) . . ? C26 N3 Ni1 115.7(4) . . ? C30 N3 Ni1 126.8(6) . . ? C4 C3 C2 120.5(7) . . ? C31 N4 C35 118.1(4) . . ? C31 N4 Ni1 115.6(4) . . ? C35 N4 Ni1 126.3(4) . . ? C3 C4 C5 118.2(7) . . ? C55 N5 C51 119.0(5) . . ? C55 N5 Ni1 126.7(4) . . ? C51 N5 Ni1 114.3(4) . . ? N1 C5 C4 122.6(7) . . ? C60 N6 C56 117.7(4) . . ? C60 N6 Ni1 127.0(3) . . ? C56 N6 Ni1 115.3(4) . . ? N2 C6 C7 119.6(6) . . ? N2 C6 C1 116.5(5) . . ? C7 C6 C1 123.7(5) . . ? C12 N7 C11 120.4(4) . . ? C8 C7 C6 120.6(6) . . ? C12 N8 C13 123.4(4) . . ? C7 C8 C9 119.1(6) . . ? C19 N9 C18 127.0(4) . . ? C10 C9 C8 118.6(6) . . ? C10 C9 C11 121.2(5) . . ? C8 C9 C11 120.2(5) . . ? C19 N10 C20 128.3(5) . . ? N2 C10 C9 122.0(5) . . ? C37 N11 C36 122.1(5) . . ? N7 C11 C9 113.1(5) . . ? C37 N12 C38 126.9(4) . . ? O9 C12 N7 123.8(5) . . ? O9 C12 N8 122.8(5) . . ? N7 C12 N8 113.4(4) . . ? C44 N13 C43 124.7(4) . . ? C18 C13 C14 119.1(5) . . ? C18 C13 N8 120.3(4) . . ? C14 C13 N8 120.6(5) . . ? C44 N14 C45 128.2(4) . . ? C15 C14 C13 121.0(6) . . ? C62 N15 C61 119.3(5) . . ? C16 C15 C14 120.6(5) . . ? C63 N16 C62 125.3(5) . . ? C15 C16 C17 120.3(6) . . ? C69 N17 C68 122.6(4) . . ? C18 C17 C16 119.1(6) . . ? C70 N18 C69 128.2(4) . . ? C13 C18 C17 119.8(5) . . ? C13 C18 N9 117.9(5) . . ? C17 C18 N9 122.3(5) . . ? O14 N19 O13 118.5(8) . . ? O14 N19 C23 121.2(7) . . ? O13 N19 C23 119.3(8) . . ? O10 C19 N9 127.2(4) . . ? O10 C19 N10 122.4(5) . . ? N9 C19 N10 110.3(4) . . ? O16 N20 O15 124.4(7) . . ? O16 N20 C48 117.5(7) . . ? O15 N20 C48 118.1(6) . . ? C25 C20 N10 125.6(5) . . ? C25 C20 C21 118.7(5) . . ? N10 C20 C21 115.6(5) . . ? O11 N21 O12 124.0(6) . . ? O11 N21 C73 117.5(6) . . ? O12 N21 C73 118.4(5) . . ? C22 C21 C20 121.1(7) . . ? C23 C22 C21 119.7(6) . . ? C22 C23 C24 120.1(6) . . ? C22 C23 N19 120.2(7) . . ? C24 C23 N19 119.7(7) . . ? C25 C24 C23 120.4(7) . . ? C20 C25 C24 119.7(6) . . ? N3 C26 C27 122.3(6) . . ? N3 C26 C31 114.4(6) . . ? C27 C26 C31 123.3(7) . . ? C28 C27 C26 121.3(10) . . ? C29 C28 C27 119.1(11) . . ? C28 C29 C30 120.5(8) . . ? N3 C30 C29 119.3(8) . . ? N4 C31 C32 121.1(5) . . ? N4 C31 C26 116.1(6) . . ? C32 C31 C26 122.8(6) . . ? C31 C32 C33 120.7(6) . . ? C32 C33 C34 121.4(6) . . ? C33 C34 C35 115.2(5) . . ? C33 C34 C36 123.7(5) . . ? C35 C34 C36 121.1(5) . . ? N4 C35 C34 123.5(5) . . ? N11 C36 C34 114.4(4) . . ? O5 C37 N11 121.9(5) . . ? O5 C37 N12 125.2(5) . . ? N11 C37 N12 112.9(5) . . ? C43 C38 N12 117.7(5) . . ? C43 C38 C39 119.9(5) . . ? N12 C38 C39 122.3(5) . . ? C38 C39 C40 118.1(5) . . ? C41 C40 C39 121.7(5) . . ? C42 C41 C40 119.9(5) . . ? C41 C42 C43 120.2(6) . . ? C38 C43 C42 120.0(5) . . ? C38 C43 N13 119.9(4) . . ? C42 C43 N13 119.9(5) . . ? O6 C44 N14 125.5(5) . . ? O6 C44 N13 123.7(5) . . ? N14 C44 N13 110.7(4) . . ? C46 C45 N14 116.0(5) . . ? C46 C45 C50 119.8(5) . . ? N14 C45 C50 124.2(5) . . ? C47 C46 C45 120.1(5) . . ? C48 C47 C46 119.8(5) . . ? C47 C48 C49 121.5(6) . . ? C47 C48 N20 119.8(6) . . ? C49 C48 N20 118.7(6) . . ? C50 C49 C48 119.4(5) . . ? C49 C50 C45 119.4(5) . . ? N5 C51 C52 119.4(6) . . ? N5 C51 C56 116.7(5) . . ? C52 C51 C56 123.8(5) . . ? C53 C52 C51 120.0(6) . . ? C52 C53 C54 120.1(6) . . ? C55 C54 C53 117.1(7) . . ? N5 C55 C54 124.1(7) . . ? N6 C56 C57 120.9(5) . . ? N6 C56 C51 114.9(5) . . ? C57 C56 C51 124.2(5) . . ? C58 C57 C56 120.3(5) . . ? C57 C58 C59 119.4(5) . . ? C60 C59 C58 117.6(5) . . ? C60 C59 C61 123.6(4) . . ? C58 C59 C61 118.7(4) . . ? N6 C60 C59 123.9(4) . . ? N15 C61 C59 115.7(4) . . ? O7 C62 N15 125.1(5) . . ? O7 C62 N16 123.7(6) . . ? N15 C62 N16 111.1(5) . . ? C64 C63 C68 119.7(6) . . ? C64 C63 N16 124.5(5) . . ? C68 C63 N16 115.8(5) . . ? C63 C64 C65 121.9(7) . . ? C66 C65 C64 120.0(8) . . ? C67 C66 C65 119.1(7) . . ? C66 C67 C68 122.1(6) . . ? N17 C68 C63 120.8(5) . . ? N17 C68 C67 122.0(5) . . ? C63 C68 C67 117.2(6) . . ? O8 C69 N17 123.2(6) . . ? O8 C69 N18 124.3(6) . . ? N17 C69 N18 112.5(4) . . ? C71 C70 N18 117.1(4) . . ? C71 C70 C75 119.1(5) . . ? N18 C70 C75 123.9(5) . . ? C70 C71 C72 121.4(5) . . ? C73 C72 C71 118.7(6) . . ? C74 C73 C72 121.0(6) . . ? C74 C73 N21 119.6(5) . . ? C72 C73 N21 119.4(6) . . ? C73 C74 C75 120.9(5) . . ? C74 C75 C70 118.9(6) . . ? C1S N1S C3S 116.0(9) . . ? C1S N1S C2S 128.4(9) . . ? C3S N1S C2S 115.6(7) . . ? O1S C1S N1S 124.8(11) . . ? C4S N2S C5S 124.9(12) . . ? C4S N2S C6S 114.1(12) . . ? C5S N2S C6S 120.3(12) . . ? O2S C4S N2S 122.6(12) . . ? N3S C8S C7S 177.8(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.993 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.084 # Attachment '- H1b.cif' data_c:\frames\470\work\470sq _database_code_depnum_ccdc_archive 'CCDC 879403' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H1b _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H89 N23 Ni O21 S' _chemical_formula_weight 1883.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7888(11) _cell_length_b 19.1350(15) _cell_length_c 19.5872(16) _cell_angle_alpha 95.997(2) _cell_angle_beta 104.132(2) _cell_angle_gamma 108.688(2) _cell_volume 4652.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9400 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45983 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16391 _reflns_number_gt 11542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Crystal diffracted poorly due to its high content of disordered solvent, with very few reflections observed at 2theta > 45 degrees. Two DMF and 1.5 dioxane solvent molecules could be located from the difference Fourier maps. The remaining electron density inside the crystal's pores, comprising 360 Ang3 could not be assigned unambiguously, and was therefore treated with the SQUEEZE routine in PLATON. 73 residual electrons/unit cell were thus found, and their contribution was substracted from the hkl file. ; _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^)+(0.1363P)^2^+0.4837P] 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 16391 _refine_ls_number_parameters 1200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2147 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ni1 Ni 0.67727(3) 0.86281(2) 0.66305(2) 0.04498(15) Uani 1 1 d . . . S1 S 0.96397(7) 1.26277(5) 0.78205(4) 0.0428(2) Uani 1 1 d . . . O1 O 1.04155(18) 1.22723(13) 0.81316(12) 0.0460(5) Uani 1 1 d . . . N1 N 0.7010(2) 0.79271(17) 0.58501(16) 0.0514(7) Uani 1 1 d . . . C1 C 0.7192(3) 0.8218(2) 0.52789(19) 0.0493(8) Uani 1 1 d . . . O2 O 0.8641(2) 1.22709(18) 0.80002(16) 0.0731(8) Uani 1 1 d . . . N2 N 0.7017(2) 0.93074(16) 0.58803(14) 0.0471(7) Uani 1 1 d . . . C2 C 0.7336(3) 0.7819(2) 0.4701(2) 0.0641(10) Uani 1 1 d . . . H2 H 0.7454 0.8038 0.4301 0.077 Uiso 1 1 calc R . . O3 O 0.9398(2) 1.24827(15) 0.70447(13) 0.0578(6) Uani 1 1 d . . . N3 N 0.7174(3) 1.15615(18) 0.61594(17) 0.0594(8) Uani 1 1 d . . . H3 H 0.7787 1.1824 0.6487 0.071 Uiso 1 1 calc R . . C3 C 0.7300(3) 0.7092(3) 0.4728(3) 0.0772(13) Uani 1 1 d . . . H3A H 0.7384 0.6799 0.4339 0.093 Uiso 1 1 calc R . . O4 O 1.0078(2) 1.34257(15) 0.81225(17) 0.0787(9) Uani 1 1 d . . . N4 N 0.6396(2) 1.1819(2) 0.70013(18) 0.0642(9) Uani 1 1 d . . . H4 H 0.7056 1.2112 0.7243 0.077 Uiso 1 1 calc R . . C4 C 0.7144(4) 0.6793(3) 0.5320(3) 0.0725(12) Uani 1 1 d . . . H4A H 0.7135 0.6299 0.5351 0.087 Uiso 1 1 calc R . . O5 O 0.93383(19) 1.07868(13) 0.99019(13) 0.0512(6) Uani 1 1 d . . . N5 N 0.7045(2) 1.26992(16) 0.83587(17) 0.0527(7) Uani 1 1 d . . . H5 H 0.7572 1.2527 0.8395 0.063 Uiso 1 1 calc R . . C5 C 0.7001(3) 0.7232(2) 0.5871(2) 0.0639(10) Uani 1 1 d . . . H5A H 0.6892 0.7028 0.6279 0.077 Uiso 1 1 calc R . . O6 O 1.3323(2) 1.38750(14) 1.02230(14) 0.0584(7) Uani 1 1 d . . . N6 N 0.8367(2) 1.38517(15) 0.87151(15) 0.0449(6) Uani 1 1 d . . . H6 H 0.8764 1.3592 0.8632 0.054 Uiso 1 1 calc R . . C6 C 0.7225(2) 0.9001(2) 0.53019(17) 0.0468(8) Uani 1 1 d . . . O7 O 1.3505(4) 1.7196(2) 0.8479(2) 0.1246(16) Uani 1 1 d . . . N7 N 1.0704(4) 1.6945(2) 0.9731(2) 0.0726(10) Uani 1 1 d . . . C7 C 0.7450(3) 0.9408(2) 0.47766(18) 0.0548(9) Uani 1 1 d . . . H7 H 0.7607 0.9189 0.4379 0.066 Uiso 1 1 calc R . . O8 O 1.4138(3) 1.74955(17) 0.9628(2) 0.0835(9) Uani 1 1 d . . . N8 N 0.5113(2) 0.82509(16) 0.62035(15) 0.0486(7) Uani 1 1 d . . . C8 C 0.7444(3) 1.0127(2) 0.48323(19) 0.0566(9) Uani 1 1 d . . . H8 H 0.7596 1.0408 0.4474 0.068 Uiso 1 1 calc R . . O9 O 1.1037(2) 1.07238(16) 0.62220(15) 0.0659(7) Uani 1 1 d . . . N9 N 0.6378(2) 0.93471(15) 0.73042(14) 0.0430(6) Uani 1 1 d . . . C9 C 0.7215(3) 1.0441(2) 0.54175(19) 0.0536(9) Uani 1 1 d . . . O10 O 0.9278(2) 1.35638(16) 0.51822(15) 0.0738(8) Uani 1 1 d . . . N10 N 0.8605(2) 1.11668(15) 0.88999(14) 0.0459(7) Uani 1 1 d . . . H10 H 0.8725 1.1361 0.8527 0.055 Uiso 1 1 calc R . . C10 C 0.7013(3) 1.0011(2) 0.59238(18) 0.0521(9) Uani 1 1 d . . . H10A H 0.6862 1.0225 0.6327 0.063 Uiso 1 1 calc R . . O11 O 0.8884(4) 1.6854(2) 0.6724(2) 0.1237(16) Uani 1 1 d . . . N11 N 1.0411(2) 1.14921(15) 0.93035(15) 0.0455(6) Uani 1 1 d . . . H11 H 1.0387 1.1692 0.8918 0.055 Uiso 1 1 calc R . . C11 C 0.7171(4) 1.1220(2) 0.5465(2) 0.0657(11) Uani 1 1 d . . . H11A H 0.7793 1.1548 0.5340 0.079 Uiso 1 1 calc R . . H11B H 0.6514 1.1196 0.5101 0.079 Uiso 1 1 calc R . . O12 O 0.9188(5) 1.6689(3) 0.7794(2) 0.1398(19) Uani 1 1 d . . . N12 N 1.2095(2) 1.28117(16) 0.94295(17) 0.0527(7) Uani 1 1 d . . . H12 H 1.1599 1.2658 0.9011 0.063 Uiso 1 1 calc R . . C12 C 0.6254(3) 1.1482(2) 0.6310(2) 0.0636(10) Uani 1 1 d . . . O13 O 0.5373(2) 1.1135(2) 0.58809(17) 0.0931(11) Uani 1 1 d . . . N13 N 1.2232(2) 1.39591(15) 0.91706(16) 0.0483(7) Uani 1 1 d . . . H13 H 1.1662 1.3689 0.8811 0.058 Uiso 1 1 calc R . . C13 C 0.5634(3) 1.1758(2) 0.7374(2) 0.0606(10) Uani 1 1 d . . . O14 O 0.6637(2) 1.37307(15) 0.86604(17) 0.0682(8) Uani 1 1 d . . . N14 N 1.3689(3) 1.7027(2) 0.9074(3) 0.0765(10) Uani 1 1 d . . . C14 C 0.4567(3) 1.1280(3) 0.7083(3) 0.0763(13) Uani 1 1 d . . . H14 H 0.4329 1.0999 0.6605 0.092 Uiso 1 1 calc R . . O15 O 1.0199(3) 1.73705(18) 0.9763(2) 0.1100(13) Uani 1 1 d . . . N15 N 0.6726(2) 0.79098(16) 0.73654(15) 0.0514(7) Uani 1 1 d . . . C15 C 0.3859(3) 1.1209(3) 0.7478(3) 0.0861(15) Uani 1 1 d . . . H15 H 0.3133 1.0885 0.7271 0.103 Uiso 1 1 calc R . . O16 O 1.1684(3) 1.71547(17) 0.9891(2) 0.0954(11) Uani 1 1 d . . . N16 N 0.8375(2) 0.90313(15) 0.72544(14) 0.0432(6) Uani 1 1 d . . . C16 C 0.4195(3) 1.1607(3) 0.8175(3) 0.0885(15) Uani 1 1 d . . . H16 H 0.3701 1.1550 0.8448 0.106 Uiso 1 1 calc R . . N17 N 1.0581(2) 1.11225(17) 0.71877(16) 0.0533(7) Uani 1 1 d . . . H17 H 1.0284 1.1413 0.7365 0.064 Uiso 1 1 calc R . . C17 C 0.5267(3) 1.2098(2) 0.8486(3) 0.0719(12) Uani 1 1 d . . . H17A H 0.5506 1.2369 0.8967 0.086 Uiso 1 1 calc R . . N18 N 1.0219(2) 1.15978(17) 0.61726(16) 0.0542(7) Uani 1 1 d . . . H18 H 0.9988 1.1879 0.6428 0.065 Uiso 1 1 calc R . . C18 C 0.5970(3) 1.2177(2) 0.8067(2) 0.0564(9) Uani 1 1 d . . . N19 N 1.0264(2) 1.29582(16) 0.58095(15) 0.0497(7) Uani 1 1 d . . . H19 H 1.0714 1.3003 0.6231 0.060 Uiso 1 1 calc R . . C19 C 0.7295(3) 1.3449(2) 0.85828(19) 0.0495(8) Uani 1 1 d . . . N20 N 0.9905(3) 1.38743(17) 0.64081(16) 0.0550(8) Uani 1 1 d . . . H20 H 1.0161 1.3701 0.6784 0.066 Uiso 1 1 calc R . . C20 C 0.8899(3) 1.46267(18) 0.89669(17) 0.0423(7) Uani 1 1 d . . . N21 N 0.9102(4) 1.6490(3) 0.7163(2) 0.0900(12) Uani 1 1 d . . . C21 C 1.0018(3) 1.48982(19) 0.91369(17) 0.0442(8) Uani 1 1 d . . . H21 H 1.0373 1.4555 0.9077 0.053 Uiso 1 1 calc R . . C22 C 1.0611(3) 1.5651(2) 0.93894(18) 0.0503(8) Uani 1 1 d . . . H22 H 1.1370 1.5830 0.9508 0.060 Uiso 1 1 calc R . . C23 C 1.0081(3) 1.6140(2) 0.94662(19) 0.0551(9) Uani 1 1 d . . . C24 C 0.8977(3) 1.5895(2) 0.9298(2) 0.0560(9) Uani 1 1 d . . . H24 H 0.8631 1.6245 0.9351 0.067 Uiso 1 1 calc R . . C25 C 0.8383(3) 1.5137(2) 0.90540(19) 0.0519(9) Uani 1 1 d . . . H25 H 0.7625 1.4962 0.8945 0.062 Uiso 1 1 calc R . . C26 C 0.4606(3) 0.85786(19) 0.65719(17) 0.0467(8) Uani 1 1 d . . . C27 C 0.3500(3) 0.8324(2) 0.63968(19) 0.0547(9) Uani 1 1 d . . . H27 H 0.3159 0.8559 0.6663 0.066 Uiso 1 1 calc R . . C28 C 0.2896(3) 0.7724(2) 0.5832(2) 0.0572(10) Uani 1 1 d . . . H28 H 0.2136 0.7537 0.5711 0.069 Uiso 1 1 calc R . . C29 C 0.3401(3) 0.7403(2) 0.5450(2) 0.0569(9) Uani 1 1 d . . . H29 H 0.2999 0.6996 0.5054 0.068 Uiso 1 1 calc R . . C30 C 0.4510(3) 0.7681(2) 0.56465(19) 0.0566(9) Uani 1 1 d . . . H30 H 0.4859 0.7459 0.5375 0.068 Uiso 1 1 calc R . . C31 C 0.5324(3) 0.92089(19) 0.71644(18) 0.0464(8) Uani 1 1 d . . . C32 C 0.4938(3) 0.9647(2) 0.7561(2) 0.0581(9) Uani 1 1 d . . . H32 H 0.4193 0.9562 0.7440 0.070 Uiso 1 1 calc R . . C33 C 0.5651(3) 1.0207(2) 0.8132(2) 0.0596(10) Uani 1 1 d . . . H33 H 0.5395 1.0505 0.8409 0.071 Uiso 1 1 calc R . . C34 C 0.6739(3) 1.03380(19) 0.83048(18) 0.0451(8) Uani 1 1 d . . . C35 C 0.7064(3) 0.98965(18) 0.78615(17) 0.0417(7) Uani 1 1 d . . . H35 H 0.7808 0.9989 0.7958 0.050 Uiso 1 1 calc R . . C36 C 0.7530(3) 1.09035(19) 0.89540(18) 0.0484(8) Uani 1 1 d . . . H36A H 0.7300 1.1339 0.9023 0.058 Uiso 1 1 calc R . . H36B H 0.7526 1.0673 0.9383 0.058 Uiso 1 1 calc R . . C37 C 0.9449(3) 1.11221(17) 0.94166(18) 0.0422(7) Uani 1 1 d . . . C38 C 1.1431(3) 1.15825(19) 0.97456(18) 0.0449(8) Uani 1 1 d . . . C39 C 1.1615(3) 1.1029(2) 1.0104(2) 0.0522(9) Uani 1 1 d . . . H39 H 1.1036 1.0579 1.0067 0.063 Uiso 1 1 calc R . . C40 C 1.2634(3) 1.1128(2) 1.0513(2) 0.0588(10) Uani 1 1 d . . . H40 H 1.2752 1.0749 1.0764 0.071 Uiso 1 1 calc R . . C41 C 1.3484(3) 1.1776(2) 1.0561(3) 0.0677(11) Uani 1 1 d . . . H41 H 1.4185 1.1839 1.0842 0.081 Uiso 1 1 calc R . . C42 C 1.3322(3) 1.2329(2) 1.0203(2) 0.0631(11) Uani 1 1 d . . . H42 H 1.3913 1.2766 1.0227 0.076 Uiso 1 1 calc R . . C43 C 1.2285(3) 1.22477(19) 0.9802(2) 0.0492(8) Uani 1 1 d . . . C44 C 1.2615(3) 1.35731(19) 0.9665(2) 0.0470(8) Uani 1 1 d . . . C45 C 1.2646(3) 1.47293(18) 0.91765(19) 0.0447(8) Uani 1 1 d . . . C46 C 1.3349(3) 1.5269(2) 0.9775(2) 0.0533(9) Uani 1 1 d . . . H46 H 1.3590 1.5122 1.0215 0.064 Uiso 1 1 calc R . . C47 C 1.3695(3) 1.6018(2) 0.9730(2) 0.0577(9) Uani 1 1 d . . . H47 H 1.4180 1.6388 1.0138 0.069 Uiso 1 1 calc R . . C48 C 1.3341(3) 1.6228(2) 0.9101(2) 0.0567(9) Uani 1 1 d . . . C49 C 1.2652(3) 1.5707(2) 0.8498(2) 0.0627(10) Uani 1 1 d . . . H49 H 1.2424 1.5862 0.8060 0.075 Uiso 1 1 calc R . . C50 C 1.2297(3) 1.4959(2) 0.8537(2) 0.0554(9) Uani 1 1 d . . . H50 H 1.1810 1.4596 0.8127 0.066 Uiso 1 1 calc R . . C51 C 0.7686(3) 0.8039(2) 0.78527(18) 0.0486(8) Uani 1 1 d . . . C52 C 0.7807(3) 0.7564(2) 0.8325(2) 0.0604(10) Uani 1 1 d . . . H52 H 0.8486 0.7661 0.8659 0.072 Uiso 1 1 calc R . . C53 C 0.6931(4) 0.6943(2) 0.8309(2) 0.0729(12) Uani 1 1 d . . . H53 H 0.7005 0.6604 0.8622 0.088 Uiso 1 1 calc R . . C54 C 0.5950(4) 0.6827(2) 0.7830(2) 0.0761(13) Uani 1 1 d . . . H54 H 0.5331 0.6417 0.7819 0.091 Uiso 1 1 calc R . . C55 C 0.5887(3) 0.7315(2) 0.7367(2) 0.0663(11) Uani 1 1 d . . . H55 H 0.5212 0.7226 0.7032 0.080 Uiso 1 1 calc R . . C56 C 0.8566(3) 0.87156(19) 0.78387(17) 0.0446(8) Uani 1 1 d . . . C57 C 0.9510(3) 0.9037(2) 0.83862(19) 0.0512(8) Uani 1 1 d . . . H57 H 0.9627 0.8818 0.8798 0.061 Uiso 1 1 calc R . . C58 C 1.0285(3) 0.9679(2) 0.83343(19) 0.0513(9) Uani 1 1 d . . . H58 H 1.0930 0.9912 0.8717 0.062 Uiso 1 1 calc R . . C59 C 1.0124(3) 0.99847(19) 0.77251(18) 0.0450(8) Uani 1 1 d . . . C60 C 0.9146(3) 0.96446(19) 0.72011(18) 0.0445(8) Uani 1 1 d . . . H60 H 0.9015 0.9855 0.6785 0.053 Uiso 1 1 calc R . . C61 C 1.0986(3) 1.0655(2) 0.7630(2) 0.0519(9) Uani 1 1 d . . . H61A H 1.1427 1.0968 0.8109 0.062 Uiso 1 1 calc R . . H61B H 1.1459 1.0474 0.7410 0.062 Uiso 1 1 calc R . . C62 C 1.0650(3) 1.1123(2) 0.6510(2) 0.0515(9) Uani 1 1 d . . . C63 C 1.0117(3) 1.1673(2) 0.54531(19) 0.0517(9) Uani 1 1 d . . . C64 C 0.9978(3) 1.1071(2) 0.4916(2) 0.0607(10) Uani 1 1 d . . . H64 H 0.9968 1.0603 0.5040 0.073 Uiso 1 1 calc R . . C65 C 0.9857(3) 1.1148(3) 0.4222(2) 0.0709(12) Uani 1 1 d . . . H65 H 0.9757 1.0733 0.3866 0.085 Uiso 1 1 calc R . . C66 C 0.9878(4) 1.1820(3) 0.4036(2) 0.0756(13) Uani 1 1 d . . . H66 H 0.9807 1.1873 0.3551 0.091 Uiso 1 1 calc R . . C67 C 1.0004(3) 1.2429(3) 0.4550(2) 0.0636(10) Uani 1 1 d . . . H67 H 1.0012 1.2893 0.4416 0.076 Uiso 1 1 calc R . . C68 C 1.0119(3) 1.2354(2) 0.52621(18) 0.0513(9) Uani 1 1 d . . . C69 C 0.9782(3) 1.3470(2) 0.57496(19) 0.0513(9) Uani 1 1 d . . . C70 C 0.9677(3) 1.4521(2) 0.6558(2) 0.0582(9) Uani 1 1 d . . . C71 C 0.9693(4) 1.4754(3) 0.7254(2) 0.0699(12) Uani 1 1 d . . . H71 H 0.9825 1.4458 0.7602 0.084 Uiso 1 1 calc R . . C72 C 0.9523(4) 1.5402(3) 0.7451(2) 0.0722(12) Uani 1 1 d . . . H72 H 0.9549 1.5559 0.7934 0.087 Uiso 1 1 calc R . . C73 C 0.9317(4) 1.5816(3) 0.6955(2) 0.0691(11) Uani 1 1 d . . . C74 C 0.9259(5) 1.5590(3) 0.6253(3) 0.0893(16) Uani 1 1 d . . . H74 H 0.9087 1.5875 0.5904 0.107 Uiso 1 1 calc R . . C75 C 0.9453(5) 1.4946(3) 0.6059(2) 0.0852(15) Uani 1 1 d . . . H75 H 0.9432 1.4794 0.5576 0.102 Uiso 1 1 calc R . . O1S O 0.5608(5) 1.0017(3) 1.0699(3) 0.1412(18) Uani 1 1 d . . . N1S N 1.3648(3) 1.3819(2) 0.79498(19) 0.0746(10) Uani 1 1 d . . . C1S C 0.5028(7) 0.9330(4) 1.0166(4) 0.137(3) Uani 1 1 d . . . H1S1 H 0.5413 0.8976 1.0247 0.165 Uiso 1 1 calc R . . H1S2 H 0.4311 0.9094 1.0228 0.165 Uiso 1 1 calc R . . O2S O 1.3656(4) 1.5861(3) 0.6625(3) 0.161(2) Uani 1 1 d . . . N2S N 0.2032(5) 0.8606(4) 0.8280(5) 0.143(3) Uani 1 1 d . . . C2S C 0.5097(7) 1.0560(4) 1.0534(4) 0.138(3) Uani 1 1 d . . . H2S1 H 0.4385 1.0384 1.0615 0.166 Uiso 1 1 calc R . . H2S2 H 0.5532 1.1047 1.0868 0.166 Uiso 1 1 calc R . . O3S O 1.2679(4) 1.4773(3) 0.5355(3) 0.1391(17) Uani 1 1 d . . . C3S C 1.3786(6) 1.4995(5) 0.5735(5) 0.177(4) Uani 1 1 d . . . H3S1 H 1.3880 1.4631 0.6046 0.213 Uiso 1 1 calc R . . H3S2 H 1.4189 1.4970 0.5384 0.213 Uiso 1 1 calc R . . O4S O 1.2191(3) 1.3495(2) 0.69891(19) 0.1009(12) Uani 1 1 d . . . C4S C 1.4207(7) 1.5687(5) 0.6141(6) 0.182(4) Uani 1 1 d . . . H4S1 H 1.4254 1.6052 0.5817 0.218 Uiso 1 1 calc R . . H4S2 H 1.4948 1.5768 0.6424 0.218 Uiso 1 1 calc R . . O5S O 0.2369(3) 0.9221(2) 0.7405(2) 0.0972(11) Uani 1 1 d . . . C5S C 1.2529(7) 1.5675(5) 0.6244(5) 0.165(4) Uani 1 1 d . . . H5S1 H 1.2124 1.5709 0.6592 0.198 Uiso 1 1 calc R . . H5S2 H 1.2452 1.6034 0.5924 0.198 Uiso 1 1 calc R . . C6S C 1.2115(6) 1.4923(5) 0.5827(4) 0.136(3) Uani 1 1 d . . . H6S1 H 1.2101 1.4569 0.6162 0.163 Uiso 1 1 calc R . . H6S2 H 1.1365 1.4814 0.5542 0.163 Uiso 1 1 calc R . . C7S C 1.2691(5) 1.3386(4) 0.7526(3) 0.108(2) Uani 1 1 d . . . H7S H 1.2361 1.2931 0.7668 0.130 Uiso 1 1 calc R . . C8S C 1.4143(5) 1.3594(5) 0.8569(4) 0.143(3) Uani 1 1 d . . . H8S1 H 1.4844 1.3983 0.8819 0.214 Uiso 1 1 calc R . . H8S2 H 1.4235 1.3119 0.8425 0.214 Uiso 1 1 calc R . . H8S3 H 1.3690 1.3525 0.8891 0.214 Uiso 1 1 calc R . . C9S C 1.4218(7) 1.4551(5) 0.7881(6) 0.183(4) Uani 1 1 d . . . H9S1 H 1.4906 1.4758 0.8259 0.274 Uiso 1 1 calc R . . H9S2 H 1.3799 1.4873 0.7926 0.274 Uiso 1 1 calc R . . H9S3 H 1.4344 1.4532 0.7410 0.274 Uiso 1 1 calc R . . C10S C 0.2278(5) 0.9127(5) 0.7980(4) 0.117(2) Uani 1 1 d . . . H10S H 0.2447 0.9592 0.8290 0.140 Uiso 1 1 calc R . . C11S C 0.1656(10) 0.7847(6) 0.7766(7) 0.276(10) Uani 1 1 d . . . H11C H 0.1379 0.7904 0.7273 0.413 Uiso 1 1 calc R . . H11D H 0.1089 0.7476 0.7897 0.413 Uiso 1 1 calc R . . H11E H 0.2260 0.7675 0.7801 0.413 Uiso 1 1 calc R . . C12S C 0.1941(8) 0.8532(7) 0.8974(5) 0.193(5) Uani 1 1 d . . . H12A H 0.2475 0.8972 0.9327 0.289 Uiso 1 1 calc R . . H12B H 0.2063 0.8075 0.9090 0.289 Uiso 1 1 calc R . . H12C H 0.1221 0.8497 0.8987 0.289 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 Ni1 0.0452(3) 0.0436(3) 0.0411(3) 0.00695(19) 0.00864(19) 0.0128(2) S1 0.0469(5) 0.0390(4) 0.0462(5) 0.0097(4) 0.0180(4) 0.0165(4) O1 0.0474(13) 0.0457(13) 0.0509(13) 0.0123(11) 0.0191(10) 0.0204(11) N1 0.0456(16) 0.0493(18) 0.0530(18) 0.0012(14) 0.0088(13) 0.0159(13) C1 0.0362(17) 0.055(2) 0.048(2) -0.0019(17) 0.0067(14) 0.0137(15) O2 0.0630(17) 0.109(2) 0.0811(19) 0.0502(18) 0.0435(15) 0.0487(17) N2 0.0515(17) 0.0521(18) 0.0350(14) 0.0057(13) 0.0102(12) 0.0181(14) C2 0.052(2) 0.069(3) 0.062(2) -0.006(2) 0.0178(18) 0.0153(19) O3 0.0695(16) 0.0644(16) 0.0473(14) 0.0139(12) 0.0201(12) 0.0315(13) N3 0.0557(19) 0.059(2) 0.061(2) 0.0135(16) 0.0137(15) 0.0191(15) C3 0.065(3) 0.069(3) 0.087(3) -0.016(3) 0.025(2) 0.019(2) O4 0.082(2) 0.0447(16) 0.088(2) -0.0037(15) -0.0121(16) 0.0261(14) N4 0.0414(17) 0.070(2) 0.064(2) -0.0022(17) 0.0132(15) 0.0052(15) C4 0.074(3) 0.059(3) 0.082(3) -0.001(2) 0.020(2) 0.027(2) O5 0.0541(14) 0.0417(13) 0.0620(15) 0.0214(12) 0.0248(12) 0.0134(11) N5 0.0388(15) 0.0451(17) 0.069(2) 0.0010(15) 0.0139(14) 0.0137(13) C5 0.068(3) 0.053(2) 0.066(3) 0.002(2) 0.012(2) 0.025(2) O6 0.0551(15) 0.0485(15) 0.0606(16) 0.0203(13) 0.0056(13) 0.0096(12) N6 0.0373(14) 0.0405(15) 0.0568(17) 0.0019(13) 0.0147(12) 0.0154(12) C6 0.0327(16) 0.060(2) 0.0387(18) 0.0008(16) 0.0034(13) 0.0128(15) O7 0.160(4) 0.069(2) 0.117(3) 0.055(2) 0.012(3) 0.016(2) N7 0.096(3) 0.044(2) 0.070(2) 0.0048(17) 0.031(2) 0.012(2) C7 0.046(2) 0.074(3) 0.0382(18) 0.0044(18) 0.0126(15) 0.0168(18) O8 0.073(2) 0.0454(17) 0.118(3) 0.0184(18) 0.0245(19) 0.0058(15) N8 0.0483(16) 0.0443(16) 0.0427(16) 0.0082(13) 0.0034(13) 0.0103(13) C8 0.054(2) 0.072(3) 0.0395(19) 0.0150(18) 0.0128(16) 0.0162(19) O9 0.0771(18) 0.0695(18) 0.0677(17) 0.0099(14) 0.0359(14) 0.0383(15) N9 0.0430(15) 0.0408(15) 0.0407(15) 0.0091(12) 0.0108(12) 0.0098(12) C9 0.051(2) 0.060(2) 0.044(2) 0.0139(17) 0.0088(16) 0.0148(17) O10 0.085(2) 0.0647(18) 0.0549(17) -0.0007(14) -0.0107(14) 0.0322(16) N10 0.0435(15) 0.0449(16) 0.0413(15) 0.0066(13) 0.0162(12) 0.0033(12) C10 0.062(2) 0.056(2) 0.0396(19) 0.0098(17) 0.0160(16) 0.0227(18) O11 0.208(5) 0.110(3) 0.094(3) 0.046(2) 0.037(3) 0.107(3) N11 0.0463(16) 0.0405(15) 0.0499(16) 0.0148(13) 0.0205(13) 0.0095(12) C11 0.088(3) 0.062(3) 0.051(2) 0.0195(19) 0.020(2) 0.029(2) O12 0.256(6) 0.140(4) 0.100(3) 0.051(3) 0.084(4) 0.140(4) N12 0.0413(15) 0.0427(16) 0.069(2) 0.0221(15) 0.0101(14) 0.0090(13) C12 0.061(3) 0.056(2) 0.060(2) 0.004(2) 0.005(2) 0.014(2) O13 0.0614(19) 0.118(3) 0.072(2) -0.0146(19) 0.0022(16) 0.0179(19) N13 0.0420(15) 0.0404(15) 0.0543(17) 0.0131(13) 0.0083(13) 0.0073(12) C13 0.044(2) 0.052(2) 0.075(3) 0.005(2) 0.0138(18) 0.0082(17) O14 0.0442(14) 0.0554(16) 0.103(2) -0.0025(15) 0.0247(14) 0.0183(12) N14 0.071(2) 0.052(2) 0.105(3) 0.031(2) 0.025(2) 0.0165(19) C14 0.047(2) 0.073(3) 0.088(3) -0.004(2) 0.011(2) 0.005(2) O15 0.135(3) 0.0457(18) 0.150(4) -0.010(2) 0.071(3) 0.021(2) N15 0.0516(17) 0.0437(16) 0.0498(17) 0.0080(13) 0.0082(13) 0.0106(14) C15 0.045(2) 0.079(3) 0.114(4) -0.004(3) 0.023(2) 0.004(2) O16 0.086(2) 0.0503(18) 0.112(3) 0.0107(18) 0.002(2) -0.0030(17) N16 0.0455(15) 0.0454(16) 0.0409(15) 0.0086(12) 0.0143(12) 0.0180(13) C16 0.051(2) 0.081(3) 0.129(5) 0.008(3) 0.044(3) 0.008(2) N17 0.0582(18) 0.0491(17) 0.0609(19) 0.0091(15) 0.0299(15) 0.0214(14) C17 0.057(2) 0.058(2) 0.093(3) -0.002(2) 0.030(2) 0.011(2) N18 0.0664(19) 0.0488(17) 0.0565(18) 0.0090(14) 0.0319(15) 0.0229(15) C18 0.0372(18) 0.050(2) 0.075(3) 0.0067(19) 0.0157(17) 0.0088(16) N19 0.0509(17) 0.0493(17) 0.0415(15) 0.0067(13) 0.0061(13) 0.0146(14) C19 0.0414(19) 0.050(2) 0.053(2) 0.0028(17) 0.0133(15) 0.0137(16) N20 0.071(2) 0.0518(18) 0.0460(17) 0.0165(14) 0.0135(14) 0.0270(16) C20 0.0448(18) 0.0420(18) 0.0398(17) 0.0061(14) 0.0126(14) 0.0159(15) N21 0.126(4) 0.093(3) 0.082(3) 0.038(3) 0.040(3) 0.069(3) C21 0.0447(18) 0.0431(19) 0.0432(18) 0.0055(15) 0.0131(14) 0.0142(15) C22 0.0471(19) 0.049(2) 0.048(2) 0.0075(16) 0.0122(15) 0.0101(16) C23 0.072(3) 0.0391(19) 0.046(2) 0.0019(16) 0.0169(18) 0.0118(18) C24 0.069(2) 0.046(2) 0.059(2) 0.0078(18) 0.0220(19) 0.0265(19) C25 0.0474(19) 0.055(2) 0.055(2) 0.0063(17) 0.0144(16) 0.0229(17) C26 0.0485(19) 0.047(2) 0.0401(18) 0.0104(15) 0.0110(15) 0.0125(16) C27 0.046(2) 0.059(2) 0.050(2) 0.0105(18) 0.0062(16) 0.0123(17) C28 0.0409(19) 0.060(2) 0.058(2) 0.0154(19) 0.0028(17) 0.0093(17) C29 0.053(2) 0.048(2) 0.051(2) 0.0060(17) -0.0021(17) 0.0070(17) C30 0.058(2) 0.054(2) 0.047(2) 0.0029(17) 0.0027(17) 0.0169(18) C31 0.0412(18) 0.047(2) 0.0448(19) 0.0109(16) 0.0106(14) 0.0091(15) C32 0.0422(19) 0.062(2) 0.064(2) 0.0035(19) 0.0145(17) 0.0143(18) C33 0.049(2) 0.063(2) 0.064(2) 0.001(2) 0.0209(18) 0.0155(18) C34 0.0433(18) 0.0415(18) 0.0472(19) 0.0101(15) 0.0166(15) 0.0081(14) C35 0.0407(17) 0.0417(18) 0.0394(17) 0.0102(15) 0.0113(14) 0.0101(14) C36 0.0486(19) 0.0436(19) 0.0486(19) 0.0047(16) 0.0182(15) 0.0093(15) C37 0.0477(19) 0.0271(16) 0.0476(19) 0.0027(14) 0.0177(15) 0.0067(14) C38 0.0454(18) 0.0412(18) 0.052(2) 0.0108(16) 0.0198(15) 0.0162(15) C39 0.060(2) 0.044(2) 0.064(2) 0.0211(17) 0.0300(18) 0.0208(17) C40 0.058(2) 0.053(2) 0.080(3) 0.029(2) 0.030(2) 0.0285(19) C41 0.050(2) 0.068(3) 0.100(3) 0.042(2) 0.026(2) 0.031(2) C42 0.044(2) 0.057(2) 0.092(3) 0.034(2) 0.022(2) 0.0140(17) C43 0.0463(19) 0.0447(19) 0.062(2) 0.0208(17) 0.0205(16) 0.0169(15) C44 0.0390(18) 0.045(2) 0.060(2) 0.0211(17) 0.0189(17) 0.0115(15) C45 0.0404(17) 0.0427(19) 0.055(2) 0.0167(16) 0.0196(15) 0.0141(15) C46 0.0454(19) 0.048(2) 0.058(2) 0.0168(18) 0.0115(16) 0.0072(16) C47 0.045(2) 0.046(2) 0.073(3) 0.0155(19) 0.0128(18) 0.0077(16) C48 0.049(2) 0.041(2) 0.080(3) 0.020(2) 0.0237(19) 0.0103(16) C49 0.073(3) 0.058(2) 0.063(2) 0.027(2) 0.022(2) 0.024(2) C50 0.066(2) 0.046(2) 0.052(2) 0.0113(17) 0.0152(18) 0.0187(18) C51 0.058(2) 0.048(2) 0.0450(19) 0.0146(16) 0.0170(16) 0.0234(17) C52 0.068(2) 0.059(2) 0.059(2) 0.0216(19) 0.0147(19) 0.028(2) C53 0.092(3) 0.053(2) 0.071(3) 0.029(2) 0.018(2) 0.022(2) C54 0.081(3) 0.054(2) 0.075(3) 0.020(2) 0.012(2) 0.005(2) C55 0.057(2) 0.057(2) 0.071(3) 0.021(2) 0.0095(19) 0.0057(19) C56 0.0484(19) 0.048(2) 0.0429(18) 0.0112(15) 0.0158(15) 0.0222(16) C57 0.050(2) 0.062(2) 0.0435(19) 0.0152(17) 0.0107(16) 0.0241(18) C58 0.0419(19) 0.063(2) 0.0445(19) 0.0025(17) 0.0085(15) 0.0184(17) C59 0.0441(18) 0.0469(19) 0.0467(19) 0.0011(15) 0.0175(15) 0.0194(15) C60 0.0468(19) 0.0474(19) 0.0417(18) 0.0079(15) 0.0157(15) 0.0185(16) C61 0.0424(19) 0.055(2) 0.058(2) 0.0061(18) 0.0172(16) 0.0178(16) C62 0.050(2) 0.044(2) 0.062(2) 0.0070(17) 0.0239(17) 0.0142(16) C63 0.0460(19) 0.052(2) 0.053(2) 0.0048(17) 0.0171(16) 0.0114(16) C64 0.057(2) 0.055(2) 0.063(3) -0.0015(19) 0.0182(19) 0.0139(18) C65 0.069(3) 0.075(3) 0.058(3) -0.008(2) 0.015(2) 0.021(2) C66 0.077(3) 0.102(4) 0.038(2) 0.000(2) 0.0113(19) 0.029(3) C67 0.059(2) 0.075(3) 0.051(2) 0.015(2) 0.0083(18) 0.022(2) C68 0.0422(19) 0.058(2) 0.046(2) 0.0031(17) 0.0113(15) 0.0113(16) C69 0.050(2) 0.048(2) 0.048(2) 0.0119(17) 0.0068(16) 0.0114(16) C70 0.064(2) 0.059(2) 0.052(2) 0.0207(19) 0.0101(18) 0.0242(19) C71 0.095(3) 0.080(3) 0.057(2) 0.030(2) 0.028(2) 0.050(3) C72 0.103(3) 0.078(3) 0.055(2) 0.023(2) 0.025(2) 0.053(3) C73 0.086(3) 0.066(3) 0.070(3) 0.022(2) 0.026(2) 0.041(2) C74 0.141(5) 0.080(3) 0.062(3) 0.033(3) 0.021(3) 0.059(3) C75 0.139(5) 0.077(3) 0.055(3) 0.022(2) 0.022(3) 0.061(3) O1S 0.197(5) 0.120(4) 0.167(4) 0.071(4) 0.108(4) 0.083(4) N1S 0.0473(19) 0.109(3) 0.062(2) 0.016(2) 0.0076(16) 0.027(2) C1S 0.241(9) 0.080(4) 0.144(6) 0.038(4) 0.102(6) 0.088(5) O2S 0.096(3) 0.144(4) 0.169(5) -0.072(4) 0.012(3) -0.004(3) N2S 0.105(4) 0.167(6) 0.226(7) 0.133(6) 0.086(5) 0.080(4) C2S 0.206(8) 0.136(6) 0.157(7) 0.081(5) 0.108(6) 0.116(6) O3S 0.109(3) 0.143(4) 0.124(4) -0.003(3) 0.010(3) 0.018(3) C3S 0.110(6) 0.167(8) 0.183(9) -0.049(7) -0.015(6) 0.024(6) O4S 0.086(2) 0.130(3) 0.067(2) 0.019(2) -0.0076(18) 0.035(2) C4S 0.143(7) 0.148(8) 0.206(10) -0.066(7) 0.025(7) 0.040(6) O5S 0.066(2) 0.115(3) 0.103(3) 0.022(2) 0.0194(19) 0.0259(19) C5S 0.128(7) 0.127(7) 0.189(9) 0.050(6) 0.018(6) -0.006(5) C6S 0.108(5) 0.134(6) 0.111(5) -0.015(5) 0.032(4) -0.016(4) C7S 0.079(4) 0.157(6) 0.076(4) -0.006(4) 0.013(3) 0.043(4) C8S 0.086(4) 0.246(10) 0.138(6) 0.064(6) 0.038(4) 0.104(5) C9S 0.153(7) 0.125(6) 0.279(12) 0.027(7) 0.138(8) 0.009(5) C10S 0.105(5) 0.191(8) 0.101(5) 0.057(5) 0.053(4) 0.089(5) C11S 0.254(14) 0.120(8) 0.291(16) 0.049(9) -0.124(12) 0.005(8) C12S 0.201(9) 0.317(14) 0.190(9) 0.159(10) 0.134(8) 0.171(10) _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 Ni1 N2 2.079(3) . ? Ni1 N8 2.083(3) . ? Ni1 N1 2.084(3) . ? Ni1 N16 2.088(3) . ? Ni1 N15 2.090(3) . ? Ni1 N9 2.093(3) . ? S1 O4 1.447(3) . ? S1 O3 1.450(2) . ? S1 O2 1.474(3) . ? S1 O1 1.487(2) . ? N1 C5 1.331(5) . ? N1 C1 1.343(5) . ? C1 C2 1.389(5) . ? C1 C6 1.480(5) . ? N2 C10 1.342(5) . ? N2 C6 1.355(4) . ? C2 C3 1.383(6) . ? N3 C12 1.337(5) . ? N3 C11 1.445(5) . ? C3 C4 1.378(7) . ? N4 C12 1.377(5) . ? N4 C13 1.401(5) . ? C4 C5 1.389(6) . ? O5 C37 1.214(4) . ? N5 C19 1.360(5) . ? N5 C18 1.429(4) . ? O6 C44 1.212(4) . ? N6 C19 1.374(4) . ? N6 C20 1.398(4) . ? C6 C7 1.389(5) . ? O7 N14 1.231(5) . ? N7 O16 1.227(5) . ? N7 O15 1.234(5) . ? N7 C23 1.466(5) . ? C7 C8 1.371(6) . ? O8 N14 1.216(5) . ? N8 C30 1.341(4) . ? N8 C26 1.354(5) . ? C8 C9 1.389(5) . ? O9 C62 1.227(4) . ? N9 C31 1.342(4) . ? N9 C35 1.345(4) . ? C9 C10 1.377(5) . ? C9 C11 1.505(6) . ? O10 C69 1.222(4) . ? N10 C37 1.376(4) . ? N10 C36 1.439(4) . ? O11 N21 1.204(5) . ? N11 C37 1.373(4) . ? N11 C38 1.406(4) . ? O12 N21 1.220(5) . ? N12 C44 1.370(4) . ? N12 C43 1.421(4) . ? C12 O13 1.221(5) . ? N13 C44 1.382(4) . ? N13 C45 1.397(4) . ? C13 C18 1.388(6) . ? C13 C14 1.395(5) . ? O14 C19 1.225(4) . ? N14 C48 1.459(5) . ? C14 C15 1.369(7) . ? N15 C55 1.339(5) . ? N15 C51 1.360(4) . ? C15 C16 1.381(7) . ? N16 C60 1.341(4) . ? N16 C56 1.358(4) . ? C16 C17 1.411(6) . ? N17 C62 1.353(5) . ? N17 C61 1.451(5) . ? C17 C18 1.398(6) . ? N18 C62 1.376(5) . ? N18 C63 1.409(5) . ? N19 C69 1.348(5) . ? N19 C68 1.419(5) . ? N20 C69 1.375(5) . ? N20 C70 1.390(5) . ? C20 C25 1.399(5) . ? C20 C21 1.399(5) . ? N21 C73 1.452(6) . ? C21 C22 1.374(5) . ? C22 C23 1.376(5) . ? C23 C24 1.382(5) . ? C24 C25 1.381(5) . ? C26 C27 1.385(5) . ? C26 C31 1.471(5) . ? C27 C28 1.381(5) . ? C28 C29 1.362(6) . ? C29 C30 1.386(5) . ? C31 C32 1.395(5) . ? C32 C33 1.378(5) . ? C33 C34 1.386(5) . ? C34 C35 1.396(5) . ? C34 C36 1.502(5) . ? C38 C39 1.385(5) . ? C38 C43 1.402(5) . ? C39 C40 1.379(5) . ? C40 C41 1.383(6) . ? C41 C42 1.376(5) . ? C42 C43 1.404(5) . ? C45 C46 1.390(5) . ? C45 C50 1.396(5) . ? C46 C47 1.377(5) . ? C47 C48 1.362(5) . ? C48 C49 1.375(6) . ? C49 C50 1.372(5) . ? C51 C52 1.381(5) . ? C51 C56 1.472(5) . ? C52 C53 1.388(6) . ? C53 C54 1.379(6) . ? C54 C55 1.375(6) . ? C56 C57 1.375(5) . ? C57 C58 1.378(5) . ? C58 C59 1.384(5) . ? C59 C60 1.385(5) . ? C59 C61 1.509(5) . ? C63 C68 1.393(5) . ? C63 C64 1.406(5) . ? C64 C65 1.356(6) . ? C65 C66 1.368(7) . ? C66 C67 1.393(6) . ? C67 C68 1.392(5) . ? C70 C75 1.376(5) . ? C70 C71 1.382(6) . ? C71 C72 1.369(6) . ? C72 C73 1.350(6) . ? C73 C74 1.374(6) . ? C74 C75 1.376(7) . ? O1S C1S 1.447(8) . ? O1S C2S 1.451(7) . ? N1S C7S 1.318(7) . ? N1S C9S 1.409(8) . ? N1S C8S 1.420(7) . ? C1S C2S 1.386(9) 2_677 ? O2S C4S 1.426(10) . ? O2S C5S 1.457(9) . ? N2S C10S 1.207(8) . ? N2S C12S 1.413(10) . ? N2S C11S 1.533(13) . ? C2S C1S 1.386(9) 2_677 ? O3S C6S 1.407(8) . ? O3S C3S 1.425(9) . ? C3S C4S 1.336(10) . ? O4S C7S 1.187(6) . ? O5S C10S 1.188(7) . ? C5S C6S 1.437(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N8 92.63(11) . . ? N2 Ni1 N1 78.47(12) . . ? N8 Ni1 N1 95.70(11) . . ? N2 Ni1 N16 95.39(11) . . ? N8 Ni1 N16 168.62(11) . . ? N1 Ni1 N16 93.81(11) . . ? N2 Ni1 N15 171.44(12) . . ? N8 Ni1 N15 94.03(11) . . ? N1 Ni1 N15 95.52(12) . . ? N16 Ni1 N15 78.82(11) . . ? N2 Ni1 N9 96.97(11) . . ? N8 Ni1 N9 78.38(11) . . ? N1 Ni1 N9 172.44(11) . . ? N16 Ni1 N9 92.61(10) . . ? N15 Ni1 N9 89.64(11) . . ? O4 S1 O3 111.70(18) . . ? O4 S1 O2 109.9(2) . . ? O3 S1 O2 108.06(17) . . ? O4 S1 O1 109.62(15) . . ? O3 S1 O1 109.37(14) . . ? O2 S1 O1 108.06(15) . . ? C5 N1 C1 118.2(3) . . ? C5 N1 Ni1 126.2(3) . . ? C1 N1 Ni1 115.6(2) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 C6 115.3(3) . . ? C2 C1 C6 121.7(4) . . ? C10 N2 C6 118.0(3) . . ? C10 N2 Ni1 126.7(2) . . ? C6 N2 Ni1 115.3(2) . . ? C3 C2 C1 117.7(4) . . ? C12 N3 C11 120.6(3) . . ? C4 C3 C2 120.0(4) . . ? C12 N4 C13 129.0(3) . . ? C3 C4 C5 118.4(4) . . ? C19 N5 C18 123.2(3) . . ? N1 C5 C4 122.7(4) . . ? C19 N6 C20 127.4(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C1 115.2(3) . . ? C7 C6 C1 123.7(3) . . ? O16 N7 O15 124.4(4) . . ? O16 N7 C23 118.4(4) . . ? O15 N7 C23 117.3(4) . . ? C8 C7 C6 120.0(3) . . ? C30 N8 C26 118.0(3) . . ? C30 N8 Ni1 126.3(3) . . ? C26 N8 Ni1 115.4(2) . . ? C7 C8 C9 119.3(3) . . ? C31 N9 C35 118.8(3) . . ? C31 N9 Ni1 114.6(2) . . ? C35 N9 Ni1 126.5(2) . . ? C10 C9 C8 117.8(4) . . ? C10 C9 C11 122.9(3) . . ? C8 C9 C11 119.3(3) . . ? C37 N10 C36 121.6(3) . . ? N2 C10 C9 123.8(3) . . ? C37 N11 C38 126.2(3) . . ? N3 C11 C9 114.8(3) . . ? C44 N12 C43 125.8(3) . . ? O13 C12 N3 123.4(4) . . ? O13 C12 N4 123.1(4) . . ? N3 C12 N4 113.4(3) . . ? C44 N13 C45 127.5(3) . . ? C18 C13 C14 119.2(4) . . ? C18 C13 N4 118.2(3) . . ? C14 C13 N4 122.5(4) . . ? O8 N14 O7 122.6(4) . . ? O8 N14 C48 119.8(4) . . ? O7 N14 C48 117.6(4) . . ? C15 C14 C13 120.7(5) . . ? C55 N15 C51 117.9(3) . . ? C55 N15 Ni1 127.2(3) . . ? C51 N15 Ni1 114.7(2) . . ? C14 C15 C16 120.4(4) . . ? C60 N16 C56 118.8(3) . . ? C60 N16 Ni1 125.6(2) . . ? C56 N16 Ni1 114.3(2) . . ? C15 C16 C17 120.4(4) . . ? C62 N17 C61 121.8(3) . . ? C18 C17 C16 118.3(4) . . ? C62 N18 C63 125.7(3) . . ? C13 C18 C17 120.9(4) . . ? C13 C18 N5 119.9(3) . . ? C17 C18 N5 119.2(4) . . ? C69 N19 C68 126.6(3) . . ? O14 C19 N5 123.6(3) . . ? O14 C19 N6 124.1(3) . . ? N5 C19 N6 112.3(3) . . ? C69 N20 C70 128.4(3) . . ? N6 C20 C25 124.1(3) . . ? N6 C20 C21 117.0(3) . . ? C25 C20 C21 118.9(3) . . ? O11 N21 O12 121.3(4) . . ? O11 N21 C73 120.3(4) . . ? O12 N21 C73 118.4(4) . . ? C22 C21 C20 121.2(3) . . ? C21 C22 C23 118.5(3) . . ? C22 C23 C24 122.0(3) . . ? C22 C23 N7 119.1(4) . . ? C24 C23 N7 118.9(4) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C20 119.9(3) . . ? N8 C26 C27 121.5(3) . . ? N8 C26 C31 114.6(3) . . ? C27 C26 C31 123.9(3) . . ? C28 C27 C26 119.4(4) . . ? C29 C28 C27 119.3(3) . . ? C28 C29 C30 118.9(4) . . ? N8 C30 C29 122.8(4) . . ? N9 C31 C32 121.2(3) . . ? N9 C31 C26 116.6(3) . . ? C32 C31 C26 122.1(3) . . ? C33 C32 C31 119.1(3) . . ? C32 C33 C34 120.6(3) . . ? C33 C34 C35 116.7(3) . . ? C33 C34 C36 122.0(3) . . ? C35 C34 C36 121.2(3) . . ? N9 C35 C34 123.4(3) . . ? N10 C36 C34 113.2(3) . . ? O5 C37 N11 125.2(3) . . ? O5 C37 N10 123.4(3) . . ? N11 C37 N10 111.4(3) . . ? C39 C38 C43 119.8(3) . . ? C39 C38 N11 122.0(3) . . ? C43 C38 N11 118.1(3) . . ? C40 C39 C38 120.3(3) . . ? C39 C40 C41 120.3(3) . . ? C42 C41 C40 120.4(4) . . ? C41 C42 C43 120.1(3) . . ? C38 C43 C42 119.1(3) . . ? C38 C43 N12 119.6(3) . . ? C42 C43 N12 121.2(3) . . ? O6 C44 N12 125.4(3) . . ? O6 C44 N13 123.9(3) . . ? N12 C44 N13 110.7(3) . . ? C46 C45 C50 119.0(3) . . ? C46 C45 N13 124.3(3) . . ? C50 C45 N13 116.6(3) . . ? C47 C46 C45 119.9(3) . . ? C48 C47 C46 119.9(4) . . ? C47 C48 C49 121.5(3) . . ? C47 C48 N14 118.8(4) . . ? C49 C48 N14 119.6(4) . . ? C50 C49 C48 119.1(4) . . ? C49 C50 C45 120.5(4) . . ? N15 C51 C52 121.4(3) . . ? N15 C51 C56 115.2(3) . . ? C52 C51 C56 123.3(3) . . ? C51 C52 C53 119.6(4) . . ? C54 C53 C52 118.8(4) . . ? C55 C54 C53 118.7(4) . . ? N15 C55 C54 123.5(4) . . ? N16 C56 C57 121.0(3) . . ? N16 C56 C51 115.5(3) . . ? C57 C56 C51 123.4(3) . . ? C56 C57 C58 119.6(3) . . ? C57 C58 C59 120.0(3) . . ? C60 C59 C58 117.4(3) . . ? C60 C59 C61 121.2(3) . . ? C58 C59 C61 121.3(3) . . ? N16 C60 C59 123.0(3) . . ? N17 C61 C59 114.1(3) . . ? O9 C62 N17 122.9(3) . . ? O9 C62 N18 123.5(3) . . ? N17 C62 N18 113.6(3) . . ? C68 C63 C64 118.8(3) . . ? C68 C63 N18 119.2(3) . . ? C64 C63 N18 121.9(3) . . ? C65 C64 C63 121.2(4) . . ? C64 C65 C66 120.1(4) . . ? C65 C66 C67 120.6(4) . . ? C68 C67 C66 119.7(4) . . ? C67 C68 C63 119.5(4) . . ? C67 C68 N19 122.1(4) . . ? C63 C68 N19 118.4(3) . . ? O10 C69 N19 124.8(4) . . ? O10 C69 N20 123.2(4) . . ? N19 C69 N20 112.1(3) . . ? C75 C70 C71 118.3(4) . . ? C75 C70 N20 124.0(4) . . ? C71 C70 N20 117.7(3) . . ? C72 C71 C70 121.2(4) . . ? C73 C72 C71 119.5(4) . . ? C72 C73 C74 120.9(4) . . ? C72 C73 N21 119.3(4) . . ? C74 C73 N21 119.8(4) . . ? C73 C74 C75 119.4(4) . . ? C70 C75 C74 120.6(4) . . ? C1S O1S C2S 108.5(6) . . ? C7S N1S C9S 124.8(6) . . ? C7S N1S C8S 120.7(6) . . ? C9S N1S C8S 114.3(6) . . ? C2S C1S O1S 113.4(6) 2_677 . ? C4S O2S C5S 110.1(7) . . ? C10S N2S C12S 135.2(10) . . ? C10S N2S C11S 111.7(9) . . ? C12S N2S C11S 113.0(8) . . ? C1S C2S O1S 113.3(6) 2_677 . ? C6S O3S C3S 109.8(6) . . ? C4S C3S O3S 113.9(8) . . ? C3S C4S O2S 117.1(9) . . ? C6S C5S O2S 108.7(8) . . ? O3S C6S C5S 116.1(7) . . ? O4S C7S N1S 128.1(7) . . ? O5S C10S N2S 137.9(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.901 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.070 # Attachment '- H2a.cif' data_c:\x-ray_~1\474\474sq _database_code_depnum_ccdc_archive 'CCDC 879404' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H2A _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C183 H209 Fe2 N53 O46 S2' _chemical_formula_weight 4062.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.2186(16) _cell_length_b 19.1483(17) _cell_length_c 35.531(3) _cell_angle_alpha 85.896(2) _cell_angle_beta 88.045(2) _cell_angle_gamma 63.311(2) _cell_volume 11046.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4260 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9232 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 103522 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 38898 _reflns_number_gt 17827 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. Crystal diffracted poorly due to its high content of disordered solvent, with very few reflections observed at 2theta > 45 degrees. 11 DMF and 3 water solvent molecules could be located from the difference Fourier maps. The remaining electron density inside the crystal's pores, comprising 1801 Ang3 could not be assigned unambiguously, and was therefore treated with the SQUEEZE routine in PLATON. 161 residual electrons/unit cell were thus found, and their contribution was substracted from the hkl file. The protons on the water molecules could not be located and were not included in the final model. Some of the solvent molecules were significantly disordered and were therefore refined isotropically. ; _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^)+(0.1831P)^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 38898 _refine_ls_number_parameters 2300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.1014 _refine_ls_wR_factor_ref 0.3139 _refine_ls_wR_factor_gt 0.2794 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 Fe1 Fe 0.91797(5) 0.68991(5) 0.83104(2) 0.0403(2) Uani 1 1 d . . . S1 S 0.92407(9) 0.70898(10) 0.62573(4) 0.0456(4) Uani 1 1 d . . . O1 O 0.9267(3) 0.7061(2) 0.58472(11) 0.0535(11) Uani 1 1 d . . . N1 N 0.8742(3) 0.6244(3) 0.85906(13) 0.0457(12) Uani 1 1 d . . . C1 C 0.8067(3) 0.6265(3) 0.84346(17) 0.0441(15) Uani 1 1 d . . . Fe2 Fe 0.60647(5) 0.34855(5) 0.68027(2) 0.0417(2) Uani 1 1 d . . . S2 S 0.59357(9) 0.32407(9) 0.88802(4) 0.0417(4) Uani 1 1 d . . . O2 O 0.9464(2) 0.7684(2) 0.63783(11) 0.0517(11) Uani 1 1 d . . . N2 N 0.8271(3) 0.7113(3) 0.79702(13) 0.0443(12) Uani 1 1 d . . . C2 C 0.7669(4) 0.5856(4) 0.8600(2) 0.0580(17) Uani 1 1 d . . . H2 H 0.7196 0.5877 0.8485 0.070 Uiso 1 1 calc R . . O3 O 0.8408(2) 0.7252(3) 0.63954(13) 0.0652(13) Uani 1 1 d . . . N3 N 0.8469(3) 0.7847(3) 0.85700(13) 0.0425(12) Uani 1 1 d . . . C3 C 0.7961(4) 0.5418(4) 0.8932(2) 0.066(2) Uani 1 1 d . . . H3 H 0.7687 0.5140 0.9050 0.079 Uiso 1 1 calc R . . O4 O 0.9806(3) 0.6305(3) 0.64265(12) 0.0562(11) Uani 1 1 d . . . N4 N 0.9484(3) 0.7640(3) 0.80221(12) 0.0406(11) Uani 1 1 d . . . C4 C 0.8676(4) 0.5381(4) 0.90974(19) 0.0609(18) Uani 1 1 d . . . H4 H 0.8892 0.5085 0.9328 0.073 Uiso 1 1 calc R . . O5 O 0.5901(3) 0.3238(3) 0.92899(11) 0.0586(12) Uani 1 1 d . . . N5 N 1.0090(3) 0.6599(3) 0.86553(13) 0.0418(11) Uani 1 1 d . . . C5 C 0.9040(4) 0.5794(4) 0.89080(17) 0.0516(16) Uani 1 1 d . . . H5 H 0.9533 0.5759 0.9008 0.062 Uiso 1 1 calc R . . O6 O 0.5685(2) 0.2687(2) 0.87345(11) 0.0470(10) Uani 1 1 d . . . N6 N 0.9975(3) 0.5983(3) 0.80596(12) 0.0398(11) Uani 1 1 d . . . C6 C 0.7804(4) 0.6747(4) 0.80819(18) 0.0488(16) Uani 1 1 d . . . O7 O 0.6794(2) 0.3034(2) 0.87559(11) 0.0501(10) Uani 1 1 d . . . N7 N 0.7865(3) 0.8433(4) 0.69344(14) 0.0608(16) Uani 1 1 d . . . H7 H 0.8285 0.8059 0.6825 0.073 Uiso 1 1 calc R . . C7 C 0.7119(4) 0.6849(4) 0.7856(2) 0.065(2) Uani 1 1 d . . . H7A H 0.6800 0.6581 0.7926 0.078 Uiso 1 1 calc R . . O8 O 0.5400(2) 0.4038(2) 0.87190(11) 0.0464(10) Uani 1 1 d . . . N8 N 0.8526(3) 0.9208(4) 0.67732(15) 0.0661(17) Uani 1 1 d . . . H8 H 0.8860 0.8805 0.6647 0.079 Uiso 1 1 calc R . . C8 C 0.6939(4) 0.7344(4) 0.75380(19) 0.0576(18) Uani 1 1 d . . . H8A H 0.6474 0.7432 0.7393 0.069 Uiso 1 1 calc R . . O9 O 0.8741(3) 0.4787(3) 0.72157(12) 0.0589(12) Uani 1 1 d . . . N9 N 0.9676(4) 0.9237(3) 0.62521(15) 0.0635(15) Uani 1 1 d . . . H9 H 0.9403 0.9094 0.6101 0.076 Uiso 1 1 calc R . . C9 C 0.7402(4) 0.7716(4) 0.74204(19) 0.0579(18) Uani 1 1 d . . . O10 O 0.6706(3) 0.6575(3) 0.56653(11) 0.0602(12) Uani 1 1 d . . . N10 N 1.0870(3) 0.8255(3) 0.60287(14) 0.0565(14) Uani 1 1 d . . . H10 H 1.0538 0.8209 0.5869 0.068 Uiso 1 1 calc R . . C10 C 0.8063(3) 0.7587(4) 0.76489(16) 0.0464(15) Uani 1 1 d . . . H10A H 0.8389 0.7847 0.7575 0.056 Uiso 1 1 calc R . . O11 O 0.6822(5) 0.7834(4) 0.38450(16) 0.111(2) Uani 1 1 d . . . N11 N 1.4214(4) 0.6162(4) 0.5872(2) 0.0801(19) Uani 1 1 d . . . C11 C 0.7218(4) 0.8270(4) 0.70658(17) 0.065(2) Uani 1 1 d . . . H11A H 0.7060 0.8040 0.6861 0.077 Uiso 1 1 calc R . . H11B H 0.6738 0.8771 0.7118 0.077 Uiso 1 1 calc R . . O12 O 0.7527(5) 0.8455(5) 0.39279(17) 0.121(2) Uani 1 1 d . . . N12 N 1.0763(3) 0.7212(3) 0.69772(14) 0.0563(14) Uani 1 1 d . . . H12 H 1.0340 0.7292 0.6837 0.068 Uiso 1 1 calc R . . C12 C 0.7890(4) 0.9130(4) 0.6964(2) 0.0601(18) Uani 1 1 d . . . O13 O 1.2027(3) 0.6335(3) 0.71919(12) 0.0660(13) Uani 1 1 d . . . N13 N 1.1359(3) 0.5968(3) 0.67671(13) 0.0531(14) Uani 1 1 d . . . H13 H 1.0927 0.6162 0.6618 0.064 Uiso 1 1 calc R . . C13 C 0.8703(4) 0.9838(4) 0.6756(2) 0.0582(18) Uani 1 1 d . . . O14 O 1.2039(3) 0.4680(3) 0.56146(11) 0.0596(12) Uani 1 1 d . . . N14 N 1.1271(3) 0.5241(3) 0.61371(13) 0.0548(14) Uani 1 1 d . . . H14 H 1.0798 0.5614 0.6208 0.066 Uiso 1 1 calc R . . C14 C 0.8379(4) 1.0430(5) 0.70248(18) 0.072(2) Uani 1 1 d . . . H14A H 0.8028 1.0399 0.7222 0.086 Uiso 1 1 calc R . . O15 O 0.9354(3) 0.6224(3) 0.38988(13) 0.0763(15) Uani 1 1 d . . . N15 N 1.0695(3) 0.5631(3) 0.55495(13) 0.0493(13) Uani 1 1 d . . . H15 H 1.0285 0.5981 0.5674 0.059 Uiso 1 1 calc R . . C15 C 0.8580(5) 1.1037(5) 0.6993(2) 0.073(2) Uani 1 1 d . . . H15A H 0.8349 1.1438 0.7166 0.088 Uiso 1 1 calc R . . O16 O 1.0515(3) 0.5230(3) 0.38190(13) 0.0801(16) Uani 1 1 d . . . N16 N 1.0017(4) 0.5713(4) 0.40133(15) 0.0553(14) Uani 1 1 d . . . C16 C 0.9105(5) 1.1083(5) 0.6720(2) 0.074(2) Uani 1 1 d . . . H16 H 0.9239 1.1510 0.6703 0.089 Uiso 1 1 calc R . . O17 O 0.7362(3) 0.9628(3) 0.71492(15) 0.0845(16) Uani 1 1 d . . . N17 N 0.9578(3) 0.5333(3) 0.70201(13) 0.0448(12) Uani 1 1 d . . . H17 H 0.9616 0.5723 0.6888 0.054 Uiso 1 1 calc R . . C17 C 0.9432(5) 1.0510(5) 0.6474(2) 0.074(2) Uani 1 1 d . . . H17A H 0.9798 1.0542 0.6284 0.088 Uiso 1 1 calc R . . O18 O 1.0925(3) 0.8989(3) 0.64997(14) 0.0680(13) Uani 1 1 d . . . N18 N 0.8250(3) 0.5869(3) 0.68065(13) 0.0477(12) Uani 1 1 d . . . H18 H 0.8411 0.6159 0.6656 0.057 Uiso 1 1 calc R . . C18 C 0.9255(4) 0.9895(4) 0.64894(17) 0.0565(18) Uani 1 1 d . . . O19 O 1.4707(4) 0.6154(4) 0.6097(2) 0.107(2) Uani 1 1 d . . . N19 N 0.7362(3) 0.6709(3) 0.61724(12) 0.0477(13) Uani 1 1 d . . . H19 H 0.7756 0.6827 0.6232 0.057 Uiso 1 1 calc R . . C19 C 1.0522(4) 0.8849(4) 0.62750(19) 0.0548(17) Uani 1 1 d . . . O20 O 1.4418(4) 0.5738(4) 0.56013(18) 0.0991(19) Uani 1 1 d . . . N20 N 0.7665(3) 0.7043(3) 0.55797(12) 0.0425(12) Uani 1 1 d . . . H20 H 0.8062 0.7087 0.5694 0.051 Uiso 1 1 calc R . . C20 C 1.1699(4) 0.7723(4) 0.60105(18) 0.0571(17) Uani 1 1 d . . . O21 O 0.3191(2) 0.4192(3) 0.78969(12) 0.0622(13) Uani 1 1 d . . . N21 N 0.7238(5) 0.8026(5) 0.4037(2) 0.089(2) Uani 1 1 d . . . C21 C 1.1958(5) 0.7251(4) 0.5718(2) 0.072(2) Uani 1 1 d . . . H21 H 1.1561 0.7282 0.5543 0.086 Uiso 1 1 calc R . . O22 O 0.3143(2) 0.5649(3) 0.95235(11) 0.0569(12) Uani 1 1 d . . . N22 N 0.6671(3) 0.2552(3) 0.65148(13) 0.0481(13) Uani 1 1 d . . . C22 C 1.2761(4) 0.6733(4) 0.5662(2) 0.0643(19) Uani 1 1 d . . . H22 H 1.2925 0.6419 0.5451 0.077 Uiso 1 1 calc R . . O23 O 0.4176(3) 0.4039(3) 1.13395(12) 0.0775(15) Uani 1 1 d . . . N23 N 0.5648(3) 0.2808(3) 0.70751(12) 0.0398(11) Uani 1 1 d . . . C23 C 1.3321(4) 0.6687(4) 0.5924(2) 0.0641(19) Uani 1 1 d . . . O24 O 0.5448(3) 0.3276(4) 1.12482(13) 0.0851(17) Uani 1 1 d . . . N24 N 0.6601(3) 0.4066(3) 0.65440(13) 0.0465(12) Uani 1 1 d . . . C24 C 1.3093(4) 0.7106(4) 0.6235(2) 0.0664(19) Uani 1 1 d . . . H24 H 1.3491 0.7039 0.6418 0.080 Uiso 1 1 calc R . . O25 O 0.7619(3) 0.0770(3) 0.79215(13) 0.0654(13) Uani 1 1 d . . . N25 N 0.7006(3) 0.3160(3) 0.71465(12) 0.0412(11) Uani 1 1 d . . . C25 C 1.2271(4) 0.7636(4) 0.6284(2) 0.067(2) Uani 1 1 d . . . H25 H 1.2103 0.7934 0.6501 0.081 Uiso 1 1 calc R . . O26 O 0.3877(3) 0.1774(3) 0.86268(14) 0.0774(15) Uani 1 1 d . . . N26 N 0.5107(3) 0.3914(3) 0.64631(13) 0.0435(12) Uani 1 1 d . . . C26 C 0.8496(4) 0.8514(4) 0.84359(17) 0.0478(15) Uani 1 1 d . . . O27 O 0.1244(4) 0.4994(4) 0.9879(2) 0.104(2) Uani 1 1 d . . . N27 N 0.5349(3) 0.4401(3) 0.70764(12) 0.0382(11) Uani 1 1 d . . . C27 C 0.8036(4) 0.9211(4) 0.85860(18) 0.0566(17) Uani 1 1 d . . . H27 H 0.8068 0.9669 0.8483 0.068 Uiso 1 1 calc R . . O28 O 0.0580(4) 0.4766(4) 0.9443(2) 0.111(2) Uani 1 1 d . . . N28 N 0.7238(3) 0.1918(3) 0.81959(13) 0.0449(12) Uani 1 1 d . . . H28 H 0.6854 0.2290 0.8322 0.054 Uiso 1 1 calc R . . C28 C 0.7521(5) 0.9257(4) 0.8888(2) 0.068(2) Uani 1 1 d . . . H28A H 0.7199 0.9742 0.8997 0.082 Uiso 1 1 calc R . . O29 O 0.6828(2) 0.5254(3) 0.79374(11) 0.0523(11) Uani 1 1 d . . . N29 N 0.6474(3) 0.1249(3) 0.82994(14) 0.0540(14) Uani 1 1 d . . . H29 H 0.6175 0.1642 0.8439 0.065 Uiso 1 1 calc R . . C29 C 0.7487(4) 0.8595(4) 0.90259(18) 0.0593(18) Uani 1 1 d . . . H29A H 0.7140 0.8608 0.9233 0.071 Uiso 1 1 calc R . . O30 O 0.8800(4) 0.3075(4) 0.95318(15) 0.098(2) Uani 1 1 d . . . N30 N 0.5225(4) 0.1316(3) 0.87844(15) 0.0630(15) Uani 1 1 d . . . H30 H 0.5568 0.1375 0.8933 0.076 Uiso 1 1 calc R . . C30 C 0.7964(4) 0.7900(4) 0.88611(17) 0.0548(17) Uani 1 1 d . . . H30A H 0.7933 0.7439 0.8959 0.066 Uiso 1 1 calc R . . O31 O 0.8282(5) 0.1280(4) 1.11948(15) 0.104(2) Uani 1 1 d . . . N31 N 0.4246(3) 0.2310(3) 0.90991(15) 0.0583(14) Uani 1 1 d . . . H31 H 0.4671 0.2275 0.9225 0.070 Uiso 1 1 calc R . . C31 C 0.9065(4) 0.8394(4) 0.81102(17) 0.0461(15) Uani 1 1 d . . . O32 O 0.7229(5) 0.1160(6) 1.10405(19) 0.153(4) Uani 1 1 d . . . N32 N 0.1199(5) 0.4641(4) 0.9612(2) 0.084(2) Uani 1 1 d . . . C32 C 0.9152(4) 0.9000(4) 0.79025(18) 0.0555(17) Uani 1 1 d . . . H32 H 0.8841 0.9527 0.7967 0.067 Uiso 1 1 calc R . . N33 N 0.5937(3) 0.4772(3) 0.81339(12) 0.0451(12) Uani 1 1 d . . . H33 H 0.5882 0.4374 0.8247 0.054 Uiso 1 1 calc R . . C33 C 0.9687(4) 0.8829(4) 0.76062(18) 0.0558(17) Uani 1 1 d . . . H33A H 0.9752 0.9236 0.7462 0.067 Uiso 1 1 calc R . . N34 N 0.7261(3) 0.4150(3) 0.83391(13) 0.0472(12) Uani 1 1 d . . . H34 H 0.7100 0.3819 0.8454 0.057 Uiso 1 1 calc R . . C34 C 1.0140(4) 0.8049(4) 0.75168(16) 0.0474(16) Uani 1 1 d . . . N35 N 0.8015(3) 0.3377(3) 0.90132(13) 0.0553(14) Uani 1 1 d . . . H35 H 0.7539 0.3423 0.8938 0.066 Uiso 1 1 calc R . . C35 C 1.0034(3) 0.7470(4) 0.77275(15) 0.0460(15) Uani 1 1 d . . . H35A H 1.0348 0.6940 0.7668 0.055 Uiso 1 1 calc R . . N36 N 0.7643(3) 0.2893(3) 0.95487(13) 0.0548(14) Uani 1 1 d . . . H36 H 0.7191 0.3009 0.9423 0.066 Uiso 1 1 calc R . . C36 C 1.0739(4) 0.7852(4) 0.71831(17) 0.0528(16) Uani 1 1 d . . . H36A H 1.0577 0.8323 0.7008 0.063 Uiso 1 1 calc R . . H36B H 1.1297 0.7709 0.7277 0.063 Uiso 1 1 calc R . . N37 N 0.7739(5) 0.1389(4) 1.09655(19) 0.087(2) Uani 1 1 d . . . C37 C 1.1431(4) 0.6482(5) 0.69956(17) 0.0585(19) Uani 1 1 d . . . N38 N 0.4408(3) 0.3261(3) 0.81259(12) 0.0465(12) Uani 1 1 d . . . H38 H 0.4837 0.3156 0.8268 0.056 Uiso 1 1 calc R . . C38 C 1.1884(4) 0.5184(4) 0.67438(16) 0.0504(16) Uani 1 1 d . . . N39 N 0.3848(3) 0.4473(3) 0.83548(13) 0.0478(13) Uani 1 1 d . . . H39 H 0.4268 0.4255 0.8510 0.057 Uiso 1 1 calc R . . C39 C 1.2439(4) 0.4750(4) 0.70335(17) 0.0527(17) Uani 1 1 d . . . H39A H 1.2470 0.4995 0.7252 0.063 Uiso 1 1 calc R . . N40 N 0.3946(3) 0.5175(3) 0.89997(13) 0.0493(13) Uani 1 1 d . . . H40 H 0.4443 0.4852 0.8926 0.059 Uiso 1 1 calc R . . C40 C 1.2933(5) 0.3976(5) 0.69987(18) 0.064(2) Uani 1 1 d . . . H40A H 1.3310 0.3687 0.7195 0.077 Uiso 1 1 calc R . . N41 N 0.4449(3) 0.4630(3) 0.95849(13) 0.0466(12) Uani 1 1 d . . . H41 H 0.4885 0.4338 0.9454 0.056 Uiso 1 1 calc R . . C41 C 1.2906(4) 0.3580(4) 0.66780(19) 0.0631(19) Uani 1 1 d . . . H41A H 1.3258 0.3039 0.6657 0.076 Uiso 1 1 calc R . . N42 N 0.4789(4) 0.3761(4) 1.11337(15) 0.0601(15) Uani 1 1 d . . . C42 C 1.2349(4) 0.4016(4) 0.63994(18) 0.0611(18) Uani 1 1 d . . . H42 H 1.2311 0.3765 0.6185 0.073 Uiso 1 1 calc R . . C43 C 1.1850(4) 0.4798(4) 0.64212(15) 0.0488(16) Uani 1 1 d . . . C44 C 1.1398(4) 0.5130(4) 0.57608(17) 0.0489(15) Uani 1 1 d . . . C45 C 1.0581(3) 0.5631(3) 0.51666(15) 0.0401(14) Uani 1 1 d . . . C46 C 1.1085(4) 0.5039(4) 0.49423(18) 0.0579(18) Uani 1 1 d . . . H46 H 1.1561 0.4611 0.5047 0.069 Uiso 1 1 calc R . . C47 C 1.0898(4) 0.5069(4) 0.45639(17) 0.0561(17) Uani 1 1 d . . . H47 H 1.1248 0.4667 0.4408 0.067 Uiso 1 1 calc R . . C48 C 1.0199(4) 0.5685(4) 0.44179(16) 0.0437(14) Uani 1 1 d . . . C49 C 0.9686(4) 0.6281(4) 0.46336(18) 0.0575(18) Uani 1 1 d . . . H49 H 0.9207 0.6703 0.4527 0.069 Uiso 1 1 calc R . . C50 C 0.9878(4) 0.6257(4) 0.50061(17) 0.0537(17) Uani 1 1 d . . . H50 H 0.9530 0.6670 0.5158 0.064 Uiso 1 1 calc R . . C51 C 1.0773(4) 0.5932(4) 0.85828(15) 0.0445(15) Uani 1 1 d . . . C52 C 1.1462(4) 0.5616(4) 0.88181(18) 0.0543(17) Uani 1 1 d . . . H52 H 1.1929 0.5146 0.8761 0.065 Uiso 1 1 calc R . . C53 C 1.1451(4) 0.5999(5) 0.91327(18) 0.063(2) Uani 1 1 d . . . H53 H 1.1910 0.5794 0.9298 0.076 Uiso 1 1 calc R . . C54 C 1.0768(5) 0.6682(5) 0.92053(18) 0.0615(19) Uani 1 1 d . . . H54 H 1.0751 0.6951 0.9422 0.074 Uiso 1 1 calc R . . C55 C 1.0105(4) 0.6977(4) 0.89625(17) 0.0518(16) Uani 1 1 d . . . H55 H 0.9646 0.7459 0.9012 0.062 Uiso 1 1 calc R . . C56 C 1.0711(3) 0.5570(4) 0.82378(16) 0.0449(15) Uani 1 1 d . . . C57 C 1.1321(4) 0.4910(4) 0.81011(16) 0.0477(15) Uani 1 1 d . . . H57 H 1.1829 0.4637 0.8231 0.057 Uiso 1 1 calc R . . C58 C 1.1192(3) 0.4643(4) 0.77721(17) 0.0503(16) Uani 1 1 d . . . H58 H 1.1614 0.4182 0.7676 0.060 Uiso 1 1 calc R . . C59 C 1.0461(3) 0.5035(4) 0.75795(16) 0.0460(15) Uani 1 1 d . . . C60 C 0.9859(3) 0.5706(3) 0.77407(16) 0.0443(14) Uani 1 1 d . . . H60 H 0.9342 0.5978 0.7618 0.053 Uiso 1 1 calc R . . C61 C 1.0287(4) 0.4754(4) 0.72248(15) 0.0476(15) Uani 1 1 d . . . H61A H 1.0774 0.4595 0.7058 0.057 Uiso 1 1 calc R . . H61B H 1.0201 0.4285 0.7291 0.057 Uiso 1 1 calc R . . C62 C 0.8852(4) 0.5291(4) 0.70263(16) 0.0468(15) Uani 1 1 d . . . C63 C 0.7430(4) 0.6057(4) 0.67900(16) 0.0461(15) Uani 1 1 d . . . C64 C 0.7035(4) 0.5834(4) 0.70857(17) 0.0553(17) Uani 1 1 d . . . H64 H 0.7340 0.5533 0.7301 0.066 Uiso 1 1 calc R . . C65 C 0.6196(5) 0.6055(5) 0.7065(2) 0.068(2) Uani 1 1 d . . . H65 H 0.5933 0.5905 0.7268 0.082 Uiso 1 1 calc R . . C66 C 0.5743(5) 0.6487(5) 0.6756(2) 0.074(2) Uani 1 1 d . . . H66 H 0.5171 0.6638 0.6748 0.088 Uiso 1 1 calc R . . C67 C 0.6125(4) 0.6702(4) 0.6455(2) 0.0657(19) Uani 1 1 d . . . H67 H 0.5815 0.6992 0.6239 0.079 Uiso 1 1 calc R . . C68 C 0.6965(4) 0.6489(4) 0.64720(17) 0.0490(15) Uani 1 1 d . . . C69 C 0.7190(4) 0.6757(4) 0.57989(17) 0.0470(15) Uani 1 1 d . . . C70 C 0.7555(3) 0.7266(3) 0.51895(15) 0.0401(14) Uani 1 1 d . . . C71 C 0.7188(4) 0.6971(4) 0.49521(17) 0.0523(16) Uani 1 1 d . . . H71 H 0.6994 0.6609 0.5048 0.063 Uiso 1 1 calc R . . C72 C 0.7110(4) 0.7213(4) 0.45740(19) 0.0592(18) Uani 1 1 d . . . H72 H 0.6867 0.7013 0.4406 0.071 Uiso 1 1 calc R . . C73 C 0.7382(4) 0.7738(4) 0.44441(17) 0.0597(18) Uani 1 1 d . . . C74 C 0.7744(4) 0.8042(4) 0.46700(19) 0.0628(19) Uani 1 1 d . . . H74 H 0.7923 0.8413 0.4572 0.075 Uiso 1 1 calc R . . C75 C 0.7840(4) 0.7784(4) 0.50526(17) 0.0510(16) Uani 1 1 d . . . H75 H 0.8104 0.7970 0.5217 0.061 Uiso 1 1 calc R . . C76 C 0.7335(3) 0.3940(3) 0.66935(15) 0.0419(14) Uani 1 1 d . . . C77 C 0.7818(4) 0.4275(4) 0.65294(17) 0.0489(15) Uani 1 1 d . . . H77 H 0.8330 0.4170 0.6637 0.059 Uiso 1 1 calc R . . C78 C 0.7534(4) 0.4764(4) 0.62060(17) 0.0532(16) Uani 1 1 d . . . H78 H 0.7859 0.4986 0.6082 0.064 Uiso 1 1 calc R . . C79 C 0.6790(4) 0.4923(4) 0.60692(17) 0.0574(18) Uani 1 1 d . . . H79 H 0.6579 0.5279 0.5855 0.069 Uiso 1 1 calc R . . C80 C 0.6335(4) 0.4576(4) 0.62358(17) 0.0533(17) Uani 1 1 d . . . H80 H 0.5815 0.4698 0.6132 0.064 Uiso 1 1 calc R . . C81 C 0.7547(3) 0.3444(3) 0.70510(16) 0.0418(14) Uani 1 1 d . . . C82 C 0.8206(4) 0.3296(4) 0.72723(16) 0.0469(15) Uani 1 1 d . . . H82 H 0.8569 0.3515 0.7199 0.056 Uiso 1 1 calc R . . C83 C 0.8343(4) 0.2839(4) 0.75950(16) 0.0481(15) Uani 1 1 d . . . H83 H 0.8806 0.2729 0.7747 0.058 Uiso 1 1 calc R . . C84 C 0.7800(3) 0.2528(3) 0.77037(15) 0.0413(14) Uani 1 1 d . . . C85 C 0.7153(3) 0.2702(3) 0.74762(16) 0.0452(15) Uani 1 1 d . . . H85 H 0.6780 0.2495 0.7549 0.054 Uiso 1 1 calc R . . C86 C 0.7953(4) 0.1997(4) 0.80636(16) 0.0512(16) Uani 1 1 d . . . H86A H 0.8398 0.1472 0.8016 0.061 Uiso 1 1 calc R . . H86B H 0.8142 0.2212 0.8264 0.061 Uiso 1 1 calc R . . C87 C 0.7154(4) 0.1280(4) 0.81279(16) 0.0525(17) Uani 1 1 d . . . C88 C 0.6195(4) 0.0677(4) 0.82818(18) 0.0603(18) Uani 1 1 d . . . C89 C 0.6497(5) 0.0101(5) 0.8021(2) 0.070(2) Uani 1 1 d . . . H89 H 0.6921 0.0082 0.7851 0.084 Uiso 1 1 calc R . . C90 C 0.6201(6) -0.0432(5) 0.8003(2) 0.089(3) Uani 1 1 d . . . H90 H 0.6442 -0.0843 0.7836 0.107 Uiso 1 1 calc R . . C91 C 0.5530(7) -0.0368(6) 0.8235(3) 0.115(4) Uani 1 1 d . . . H91 H 0.5292 -0.0715 0.8213 0.138 Uiso 1 1 calc R . . C92 C 0.5233(6) 0.0182(6) 0.8487(2) 0.099(3) Uani 1 1 d . . . H92 H 0.4798 0.0207 0.8649 0.119 Uiso 1 1 calc R . . C93 C 0.5550(5) 0.0728(4) 0.85163(19) 0.068(2) Uani 1 1 d . . . C94 C 0.4402(5) 0.1790(4) 0.88187(19) 0.0590(18) Uani 1 1 d . . . C95 C 0.3459(5) 0.2895(4) 0.91996(18) 0.0569(18) Uani 1 1 d . . . C96 C 0.3446(5) 0.3363(4) 0.9490(2) 0.070(2) Uani 1 1 d . . . H96 H 0.3948 0.3294 0.9595 0.084 Uiso 1 1 calc R . . C97 C 0.2725(5) 0.3912(4) 0.9621(2) 0.075(2) Uani 1 1 d . . . H97 H 0.2730 0.4202 0.9826 0.090 Uiso 1 1 calc R . . C98 C 0.1994(5) 0.4055(5) 0.9467(3) 0.078(2) Uani 1 1 d . . . C99 C 0.1971(5) 0.3616(5) 0.9176(3) 0.085(2) Uani 1 1 d . . . H99 H 0.1462 0.3702 0.9071 0.102 Uiso 1 1 calc R . . C100 C 0.2717(5) 0.3042(5) 0.9042(2) 0.083(2) Uani 1 1 d . . . H100 H 0.2711 0.2748 0.8838 0.099 Uiso 1 1 calc R . . C101 C 0.6521(4) 0.1940(4) 0.66223(16) 0.0469(15) Uani 1 1 d . . . C102 C 0.6835(4) 0.1260(4) 0.64360(19) 0.0614(18) Uani 1 1 d . . . H102 H 0.6717 0.0837 0.6516 0.074 Uiso 1 1 calc R . . C103 C 0.7344(4) 0.1219(5) 0.6117(2) 0.075(2) Uani 1 1 d . . . H103 H 0.7582 0.0760 0.5980 0.089 Uiso 1 1 calc R . . C104 C 0.7489(4) 0.1844(5) 0.6008(2) 0.0633(19) Uani 1 1 d . . . H104 H 0.7813 0.1834 0.5791 0.076 Uiso 1 1 calc R . . C105 C 0.7162(4) 0.2478(4) 0.62160(17) 0.0539(17) Uani 1 1 d . . . H105 H 0.7289 0.2899 0.6145 0.065 Uiso 1 1 calc R . . C106 C 0.5976(4) 0.2064(4) 0.69539(16) 0.0460(15) Uani 1 1 d . . . C107 C 0.5812(5) 0.1489(4) 0.71403(19) 0.069(2) Uani 1 1 d . . . H107 H 0.6046 0.0974 0.7055 0.083 Uiso 1 1 calc R . . C108 C 0.5294(4) 0.1679(4) 0.74572(18) 0.0625(19) Uani 1 1 d . . . H108 H 0.5174 0.1294 0.7590 0.075 Uiso 1 1 calc R . . C109 C 0.4960(4) 0.2435(4) 0.75729(16) 0.0489(15) Uani 1 1 d . . . C110 C 0.5153(3) 0.2970(3) 0.73731(15) 0.0401(14) Uani 1 1 d . . . H110 H 0.4919 0.3490 0.7453 0.048 Uiso 1 1 calc R . . C111 C 0.4390(4) 0.2653(4) 0.79157(16) 0.0526(16) Uani 1 1 d . . . H11C H 0.3821 0.2824 0.7830 0.063 Uiso 1 1 calc R . . H11D H 0.4542 0.2178 0.8087 0.063 Uiso 1 1 calc R . . C112 C 0.3767(3) 0.4002(4) 0.81090(16) 0.0441(15) Uani 1 1 d . . . C113 C 0.3327(3) 0.5277(4) 0.83862(17) 0.0480(15) Uani 1 1 d . . . C114 C 0.2770(3) 0.5751(4) 0.81018(16) 0.0484(16) Uani 1 1 d . . . H114 H 0.2740 0.5531 0.7875 0.058 Uiso 1 1 calc R . . C115 C 0.2270(4) 0.6531(4) 0.81506(19) 0.0586(18) Uani 1 1 d . . . H115 H 0.1887 0.6837 0.7959 0.070 Uiso 1 1 calc R . . C116 C 0.2310(4) 0.6880(4) 0.8471(2) 0.0615(18) Uani 1 1 d . . . H116 H 0.1956 0.7417 0.8504 0.074 Uiso 1 1 calc R . . C117 C 0.2888(4) 0.6419(4) 0.87462(19) 0.0566(17) Uani 1 1 d . . . H117 H 0.2944 0.6659 0.8961 0.068 Uiso 1 1 calc R . . C118 C 0.3371(3) 0.5642(4) 0.87159(16) 0.0454(15) Uani 1 1 d . . . C119 C 0.3784(4) 0.5191(4) 0.93840(17) 0.0470(15) Uani 1 1 d . . . C120 C 0.4493(3) 0.4486(4) 0.99718(16) 0.0454(15) Uani 1 1 d . . . C121 C 0.5216(4) 0.3838(4) 1.01099(17) 0.0527(17) Uani 1 1 d . . . H121 H 0.5638 0.3555 0.9937 0.063 Uiso 1 1 calc R . . C122 C 0.5324(4) 0.3607(4) 1.04893(17) 0.0544(17) Uani 1 1 d . . . H122 H 0.5815 0.3173 1.0578 0.065 Uiso 1 1 calc R . . C123 C 0.4698(4) 0.4022(4) 1.07391(16) 0.0519(17) Uani 1 1 d . . . C124 C 0.3988(4) 0.4672(4) 1.06122(17) 0.0541(17) Uani 1 1 d . . . H124 H 0.3578 0.4965 1.0787 0.065 Uiso 1 1 calc R . . C125 C 0.3881(4) 0.4892(4) 1.02321(18) 0.0562(18) Uani 1 1 d . . . H125 H 0.3387 0.5323 1.0146 0.067 Uiso 1 1 calc R . . C126 C 0.4461(3) 0.4563(3) 0.65730(15) 0.0419(14) Uani 1 1 d . . . C127 C 0.3732(3) 0.4931(4) 0.63663(16) 0.0435(14) Uani 1 1 d . . . H127 H 0.3288 0.5390 0.6452 0.052 Uiso 1 1 calc R . . C128 C 0.3658(4) 0.4632(4) 0.60434(17) 0.0550(17) Uani 1 1 d . . . H128 H 0.3164 0.4879 0.5901 0.066 Uiso 1 1 calc R . . C129 C 0.4308(4) 0.3966(4) 0.59232(17) 0.0541(17) Uani 1 1 d . . . H129 H 0.4270 0.3749 0.5697 0.065 Uiso 1 1 calc R . . C130 C 0.5035(4) 0.3608(4) 0.61421(16) 0.0524(16) Uani 1 1 d . . . H130 H 0.5482 0.3144 0.6062 0.063 Uiso 1 1 calc R . . C131 C 0.4592(3) 0.4838(3) 0.69290(15) 0.0374(13) Uani 1 1 d . . . C132 C 0.4007(3) 0.5490(4) 0.71028(16) 0.0444(14) Uani 1 1 d . . . H132 H 0.3483 0.5799 0.6991 0.053 Uiso 1 1 calc R . . C133 C 0.4206(3) 0.5676(3) 0.74411(17) 0.0461(15) Uani 1 1 d . . . H133 H 0.3811 0.6110 0.7567 0.055 Uiso 1 1 calc R . . C134 C 0.4974(3) 0.5235(3) 0.75968(15) 0.0387(13) Uani 1 1 d . . . C135 C 0.5528(3) 0.4604(3) 0.74029(15) 0.0416(14) Uani 1 1 d . . . H135 H 0.6061 0.4300 0.7506 0.050 Uiso 1 1 calc R . . C136 C 0.5227(3) 0.5412(3) 0.79645(16) 0.0427(14) Uani 1 1 d . . . H13A H 0.5342 0.5870 0.7919 0.051 Uiso 1 1 calc R . . H13B H 0.4762 0.5557 0.8144 0.051 Uiso 1 1 calc R . . C137 C 0.6686(4) 0.4757(4) 0.81264(16) 0.0447(15) Uani 1 1 d . . . C138 C 0.8077(4) 0.3992(4) 0.83963(16) 0.0462(15) Uani 1 1 d . . . C139 C 0.8512(4) 0.4216(4) 0.8123(2) 0.0601(18) Uani 1 1 d . . . H139 H 0.8251 0.4471 0.7891 0.072 Uiso 1 1 calc R . . C140 C 0.9312(4) 0.4075(5) 0.8182(2) 0.070(2) Uani 1 1 d . . . H140 H 0.9599 0.4237 0.7995 0.085 Uiso 1 1 calc R . . C141 C 0.9698(5) 0.3684(5) 0.8527(2) 0.081(2) Uani 1 1 d . . . H141 H 1.0247 0.3587 0.8574 0.097 Uiso 1 1 calc R . . C142 C 0.9280(4) 0.3446(5) 0.8794(2) 0.071(2) Uani 1 1 d . . . H142 H 0.9550 0.3171 0.9021 0.085 Uiso 1 1 calc R . . C143 C 0.8480(4) 0.3600(4) 0.87369(17) 0.0518(16) Uani 1 1 d . . . C144 C 0.8220(4) 0.3110(4) 0.93685(19) 0.0596(18) Uani 1 1 d . . . C145 C 0.7717(4) 0.2512(4) 0.99074(17) 0.0518(16) Uani 1 1 d . . . C146 C 0.8266(5) 0.2449(5) 1.01765(19) 0.074(2) Uani 1 1 d . . . H146 H 0.8645 0.2659 1.0124 0.088 Uiso 1 1 calc R . . C147 C 0.8268(5) 0.2075(4) 1.05283(19) 0.073(2) Uani 1 1 d . . . H147 H 0.8637 0.2046 1.0718 0.088 Uiso 1 1 calc R . . C148 C 0.7746(5) 0.1753(4) 1.06022(18) 0.0634(19) Uani 1 1 d . . . C149 C 0.7203(5) 0.1802(5) 1.0335(2) 0.072(2) Uani 1 1 d . . . H149 H 0.6836 0.1578 1.0385 0.087 Uiso 1 1 calc R . . C150 C 0.7198(4) 0.2181(4) 0.99895(17) 0.0576(17) Uani 1 1 d . . . H150 H 0.6822 0.2214 0.9802 0.069 Uiso 1 1 calc R . . O1S O 0.9870(4) 0.8075(4) 0.55080(16) 0.0966(18) Uani 1 1 d . . . N1S N 1.4191(5) 0.7717(4) 0.5280(2) 0.093(2) Uiso 1 1 d . . . C1S C 1.4884(6) 0.7149(6) 0.5151(3) 0.102(3) Uiso 1 1 d . . . H1S H 1.5355 0.6924 0.5309 0.122 Uiso 1 1 calc R . . O2S O 0.6544(4) 0.1060(4) 0.92959(15) 0.0951(18) Uani 1 1 d . . . N2S N 1.3252(4) 0.5723(3) 0.48120(16) 0.0631(15) Uiso 1 1 d . . . C2S C 1.3419(7) 0.8098(7) 0.5091(3) 0.137(4) Uiso 1 1 d . . . H2S1 H 1.3021 0.8497 0.5249 0.206 Uiso 1 1 calc R . . H2S2 H 1.3223 0.7711 0.5045 0.206 Uiso 1 1 calc R . . H2S3 H 1.3483 0.8347 0.4850 0.206 Uiso 1 1 calc R . . O3S O 0.5382(4) 0.2149(4) 0.9672(2) 0.119(2) Uani 1 1 d . . . N3S N 1.3329(7) 0.0819(6) 0.4204(3) 0.145(3) Uiso 1 1 d . . . C3S C 1.4199(7) 0.8036(7) 0.5642(3) 0.129(4) Uiso 1 1 d . . . H3S1 H 1.3649 0.8447 0.5696 0.194 Uiso 1 1 calc R . . H3S2 H 1.4591 0.8257 0.5630 0.194 Uiso 1 1 calc R . . H3S3 H 1.4362 0.7616 0.5843 0.194 Uiso 1 1 calc R . . O4S O 1.2228(4) 0.6861(5) 0.4643(2) 0.126(2) Uiso 1 1 d . . . N4S N 1.1201(4) -0.0416(4) 0.50264(18) 0.0742(17) Uiso 1 1 d . . . C4S C 1.2455(7) 0.6138(7) 0.4782(3) 0.121(4) Uiso 1 1 d . . . H4S H 1.2076 0.5938 0.4855 0.146 Uiso 1 1 calc R . . O5S O 1.4934(5) 0.6903(5) 0.4830(2) 0.136(3) Uiso 1 1 d . . . N5S N 0.9895(4) 0.2175(4) 0.58105(19) 0.0798(18) Uiso 1 1 d . . . C5S C 1.3845(6) 0.6003(6) 0.4696(3) 0.120(3) Uiso 1 1 d . . . H5S1 H 1.4400 0.5594 0.4757 0.181 Uiso 1 1 calc R . . H5S2 H 1.3737 0.6470 0.4830 0.181 Uiso 1 1 calc R . . H5S3 H 1.3802 0.6134 0.4424 0.181 Uiso 1 1 calc R . . O6S O 1.3075(6) 0.0150(6) 0.4740(3) 0.176(4) Uiso 1 1 d . . . N6S N 0.4871(6) 0.1044(6) 0.5569(3) 0.129(3) Uiso 1 1 d . . . C6S C 1.3646(7) 0.4915(6) 0.4958(3) 0.123(4) Uiso 1 1 d . . . H6S1 H 1.4242 0.4731 0.4964 0.185 Uiso 1 1 calc R . . H6S2 H 1.3518 0.4593 0.4795 0.185 Uiso 1 1 calc R . . H6S3 H 1.3446 0.4874 0.5214 0.185 Uiso 1 1 calc R . . O7S O 1.1291(4) -0.0032(4) 0.4421(2) 0.115(2) Uiso 1 1 d . . . N7S N 0.3883(6) 0.0554(5) 0.9823(3) 0.123(3) Uiso 1 1 d . . . C7S C 1.3438(8) 0.0516(7) 0.4580(4) 0.141(4) Uiso 1 1 d . . . H7S H 1.3818 0.0594 0.4727 0.170 Uiso 1 1 calc R . . O8S O 1.0488(3) 0.1673(3) 0.52526(15) 0.0824(15) Uiso 1 1 d . . . N8S N 0.9116(6) -0.0660(6) 0.9902(3) 0.141(3) Uiso 1 1 d . . . C8S C 1.2610(8) 0.0784(8) 0.4029(4) 0.153(5) Uiso 1 1 d . . . H8S1 H 1.2545 0.1004 0.3767 0.229 Uiso 1 1 calc R . . H8S2 H 1.2110 0.1088 0.4172 0.229 Uiso 1 1 calc R . . H8S3 H 1.2704 0.0238 0.4033 0.229 Uiso 1 1 calc R . . O9S O 0.4288(7) 0.0264(7) 0.5584(3) 0.199(4) Uiso 1 1 d . . . N9S N 0.9231(5) 0.0833(5) 0.8861(2) 0.111(3) Uiso 1 1 d . . . C9S C 1.3846(8) 0.1166(8) 0.4028(4) 0.167(5) Uiso 1 1 d . . . H9S1 H 1.3675 0.1345 0.3766 0.250 Uiso 1 1 calc R . . H9S2 H 1.4423 0.0772 0.4034 0.250 Uiso 1 1 calc R . . H9S3 H 1.3785 0.1612 0.4168 0.250 Uiso 1 1 calc R . . O10S O 0.9595(4) -0.1616(4) 0.95056(19) 0.114(2) Uiso 1 1 d . . . N10S N 0.8821(4) 0.7118(4) 1.00248(19) 0.0824(19) Uiso 1 1 d . . . C10S C 1.1365(5) 0.0027(5) 0.4780(2) 0.078(2) Uiso 1 1 d . . . H10S H 1.1538 0.0392 0.4860 0.094 Uiso 1 1 calc R . . O11S O 0.8093(4) 0.0726(4) 0.90220(19) 0.114(2) Uiso 1 1 d . . . N11S N 0.5533(5) 0.7814(4) 0.9149(2) 0.092(2) Uiso 1 1 d . . . C11S C 1.1260(6) -0.0327(6) 0.5424(3) 0.110(3) Uiso 1 1 d . . . H11E H 1.1120 -0.0701 0.5573 0.165 Uiso 1 1 calc R . . H11F H 1.0878 0.0208 0.5484 0.165 Uiso 1 1 calc R . . H11G H 1.1822 -0.0428 0.5482 0.165 Uiso 1 1 calc R . . O12S O 0.3520(6) 0.0157(6) 1.0331(3) 0.180(4) Uiso 1 1 d . . . C12S C 1.0982(6) -0.1026(5) 0.4935(3) 0.103(3) Uiso 1 1 d . . . H12A H 1.0889 -0.1280 0.5168 0.155 Uiso 1 1 calc R . . H12B H 1.1429 -0.1415 0.4791 0.155 Uiso 1 1 calc R . . H12C H 1.0479 -0.0794 0.4783 0.155 Uiso 1 1 calc R . . O13S O 0.7992(5) 0.6980(4) 0.9633(2) 0.132(2) Uiso 1 1 d . . . C13S C 0.9894(5) 0.2113(4) 0.5436(2) 0.0645(19) Uiso 1 1 d . . . H13S H 0.9399 0.2432 0.5303 0.077 Uiso 1 1 calc R . . O14S O 0.4569(6) 0.8302(6) 0.9566(3) 0.173(3) Uiso 1 1 d . . . C14S C 1.0655(5) 0.1711(5) 0.6021(3) 0.096(3) Uiso 1 1 d . . . H14B H 1.0557 0.1808 0.6290 0.143 Uiso 1 1 calc R . . H14C H 1.1080 0.1861 0.5927 0.143 Uiso 1 1 calc R . . H14D H 1.0839 0.1153 0.5988 0.143 Uiso 1 1 calc R . . C15S C 0.9226(4) 0.2770(4) 0.5993(2) 0.073(2) Uiso 1 1 d . . . H15B H 0.9333 0.2716 0.6264 0.109 Uiso 1 1 calc R . . H15C H 0.8723 0.2720 0.5950 0.109 Uiso 1 1 calc R . . H15D H 0.9158 0.3284 0.5890 0.109 Uiso 1 1 calc R . . C16S C 0.4558(9) 0.0646(9) 0.5794(5) 0.165(5) Uiso 1 1 d . . . H16S H 0.4535 0.0640 0.6062 0.198 Uiso 1 1 calc R . . C17S C 0.5269(7) 0.1429(7) 0.5758(3) 0.144(4) Uiso 1 1 d . . . H17B H 0.5481 0.1692 0.5570 0.215 Uiso 1 1 calc R . . H17C H 0.5724 0.1039 0.5912 0.215 Uiso 1 1 calc R . . H17D H 0.4870 0.1817 0.5921 0.215 Uiso 1 1 calc R . . C18S C 0.4859(8) 0.1166(8) 0.5159(4) 0.159(5) Uiso 1 1 d . . . H18A H 0.5140 0.1487 0.5084 0.238 Uiso 1 1 calc R . . H18B H 0.4289 0.1434 0.5071 0.238 Uiso 1 1 calc R . . H18C H 0.5141 0.0658 0.5046 0.238 Uiso 1 1 calc R . . C19S C 0.3550(8) 0.0131(8) 0.9988(4) 0.140(4) Uiso 1 1 d . . . H19S H 0.3353 -0.0164 0.9856 0.168 Uiso 1 1 calc R . . C20S C 0.4130(8) 0.1099(8) 0.9982(4) 0.154(5) Uiso 1 1 d . . . H20A H 0.4381 0.1306 0.9784 0.231 Uiso 1 1 calc R . . H20B H 0.4529 0.0824 1.0185 0.231 Uiso 1 1 calc R . . H20C H 0.3646 0.1532 1.0084 0.231 Uiso 1 1 calc R . . C21S C 0.3971(10) 0.0535(10) 0.9417(5) 0.215(7) Uiso 1 1 d . . . H21A H 0.4257 0.0843 0.9326 0.323 Uiso 1 1 calc R . . H21B H 0.3426 0.0758 0.9300 0.323 Uiso 1 1 calc R . . H21C H 0.4289 -0.0008 0.9349 0.323 Uiso 1 1 calc R . . C22S C 0.9113(7) -0.0954(7) 0.9562(3) 0.124(4) Uiso 1 1 d . . . H22S H 0.8732 -0.0636 0.9372 0.149 Uiso 1 1 calc R . . C23S C 0.8473(8) 0.0149(8) 0.9966(4) 0.160(5) Uiso 1 1 d . . . H23A H 0.8551 0.0294 1.0215 0.240 Uiso 1 1 calc R . . H23B H 0.7928 0.0168 0.9953 0.240 Uiso 1 1 calc R . . H23C H 0.8519 0.0518 0.9772 0.240 Uiso 1 1 calc R . . C24S C 0.9777(11) -0.1037(10) 1.0200(5) 0.217(7) Uiso 1 1 d . . . H24A H 0.9639 -0.0700 1.0413 0.326 Uiso 1 1 calc R . . H24B H 1.0306 -0.1106 1.0092 0.326 Uiso 1 1 calc R . . H24C H 0.9814 -0.1548 1.0289 0.326 Uiso 1 1 calc R . . C25S C 0.8471(6) 0.1098(6) 0.8983(3) 0.096(3) Uiso 1 1 d . . . H25S H 0.8200 0.1630 0.9045 0.115 Uiso 1 1 calc R . . C26S C 0.9660(10) -0.0040(10) 0.8773(5) 0.208(7) Uiso 1 1 d . . . H26A H 1.0218 -0.0177 0.8680 0.312 Uiso 1 1 calc R . . H26B H 0.9348 -0.0132 0.8579 0.312 Uiso 1 1 calc R . . H26C H 0.9686 -0.0365 0.9003 0.312 Uiso 1 1 calc R . . C27S C 0.9666(7) 0.1368(7) 0.8772(3) 0.131(4) Uiso 1 1 d . . . H27A H 1.0225 0.1052 0.8680 0.197 Uiso 1 1 calc R . . H27B H 0.9691 0.1611 0.9001 0.197 Uiso 1 1 calc R . . H27C H 0.9356 0.1778 0.8578 0.197 Uiso 1 1 calc R . . C28S C 0.4798(8) 0.8334(8) 0.9205(4) 0.149(5) Uiso 1 1 d . . . H28S H 0.4457 0.8698 0.9014 0.179 Uiso 1 1 calc R . . C29S C 0.6166(7) 0.7287(7) 0.9420(3) 0.137(4) Uiso 1 1 d . . . H29B H 0.6664 0.6956 0.9283 0.205 Uiso 1 1 calc R . . H29C H 0.5963 0.6957 0.9567 0.205 Uiso 1 1 calc R . . H29D H 0.6293 0.7598 0.9590 0.205 Uiso 1 1 calc R . . C30S C 0.5878(7) 0.7774(7) 0.8763(3) 0.129(4) Uiso 1 1 d . . . H30B H 0.6440 0.7350 0.8760 0.193 Uiso 1 1 calc R . . H30C H 0.5884 0.8273 0.8685 0.193 Uiso 1 1 calc R . . H30D H 0.5537 0.7672 0.8588 0.193 Uiso 1 1 calc R . . C31S C 0.8706(6) 0.6729(6) 0.9772(3) 0.093(3) Uiso 1 1 d . . . H31S H 0.9146 0.6262 0.9691 0.112 Uiso 1 1 calc R . . C32S C 0.8175(7) 0.7865(7) 1.0133(3) 0.133(4) Uiso 1 1 d . . . H32A H 0.8383 0.8071 1.0326 0.200 Uiso 1 1 calc R . . H32B H 0.7706 0.7792 1.0234 0.200 Uiso 1 1 calc R . . H32C H 0.8002 0.8237 0.9911 0.200 Uiso 1 1 calc R . . C33S C 0.9634(6) 0.6793(6) 1.0179(3) 0.119(3) Uiso 1 1 d . . . H33B H 0.9654 0.7133 1.0368 0.179 Uiso 1 1 calc R . . H33C H 1.0027 0.6754 0.9976 0.179 Uiso 1 1 calc R . . H33D H 0.9777 0.6270 1.0297 0.179 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 Fe1 0.0362(5) 0.0565(6) 0.0331(4) -0.0084(4) -0.0002(3) -0.0243(4) S1 0.0379(8) 0.0634(11) 0.0412(8) -0.0141(8) 0.0031(7) -0.0263(8) O1 0.062(3) 0.063(3) 0.042(2) -0.014(2) -0.001(2) -0.033(2) N1 0.047(3) 0.063(3) 0.040(3) -0.010(3) 0.006(2) -0.035(3) C1 0.033(3) 0.045(4) 0.059(4) -0.018(3) 0.012(3) -0.021(3) Fe2 0.0353(5) 0.0530(5) 0.0321(4) -0.0041(4) -0.0028(3) -0.0154(4) S2 0.0393(8) 0.0531(9) 0.0325(8) -0.0055(7) -0.0027(6) -0.0201(7) O2 0.046(2) 0.064(3) 0.053(3) -0.017(2) -0.002(2) -0.030(2) N2 0.033(3) 0.062(3) 0.046(3) -0.025(3) 0.006(2) -0.025(2) C2 0.063(4) 0.070(5) 0.058(4) -0.011(4) 0.002(3) -0.044(4) O3 0.036(2) 0.087(3) 0.079(3) -0.033(3) 0.012(2) -0.030(2) N3 0.042(3) 0.057(3) 0.038(3) -0.009(2) 0.001(2) -0.029(2) C3 0.063(5) 0.062(5) 0.095(6) -0.026(4) 0.027(4) -0.046(4) O4 0.054(3) 0.067(3) 0.052(3) -0.007(2) 0.004(2) -0.031(2) N4 0.035(3) 0.057(3) 0.032(3) -0.004(2) -0.009(2) -0.022(2) C4 0.073(5) 0.063(5) 0.055(4) -0.007(3) 0.011(4) -0.038(4) O5 0.056(3) 0.068(3) 0.039(2) -0.008(2) -0.001(2) -0.015(2) N5 0.038(3) 0.057(3) 0.036(3) 0.000(2) -0.002(2) -0.027(3) C5 0.054(4) 0.069(4) 0.047(4) -0.009(3) 0.011(3) -0.041(4) O6 0.046(2) 0.056(3) 0.047(2) -0.013(2) 0.0045(19) -0.030(2) N6 0.034(3) 0.053(3) 0.033(3) 0.002(2) -0.007(2) -0.020(2) C6 0.040(3) 0.048(4) 0.054(4) -0.022(3) -0.003(3) -0.013(3) O7 0.038(2) 0.061(3) 0.053(3) -0.015(2) -0.0004(19) -0.023(2) N7 0.051(3) 0.081(5) 0.034(3) -0.007(3) 0.001(2) -0.015(3) C7 0.040(4) 0.070(5) 0.093(6) -0.029(4) 0.007(4) -0.029(3) O8 0.043(2) 0.050(3) 0.047(2) -0.0016(19) -0.0017(19) -0.022(2) N8 0.043(3) 0.084(5) 0.046(3) -0.024(3) 0.010(3) -0.004(3) C8 0.051(4) 0.055(4) 0.058(4) -0.015(4) -0.013(3) -0.014(3) O9 0.072(3) 0.065(3) 0.050(3) 0.011(2) -0.011(2) -0.042(3) N9 0.065(4) 0.059(4) 0.051(3) -0.010(3) 0.000(3) -0.013(3) C9 0.045(4) 0.062(4) 0.063(4) -0.031(4) 0.003(3) -0.017(3) O10 0.076(3) 0.084(3) 0.044(2) 0.007(2) -0.016(2) -0.057(3) N10 0.058(3) 0.060(4) 0.050(3) -0.013(3) -0.002(3) -0.024(3) C10 0.034(3) 0.061(4) 0.036(3) -0.009(3) -0.009(3) -0.012(3) O11 0.164(6) 0.127(5) 0.056(3) 0.003(3) -0.028(4) -0.078(5) N11 0.071(5) 0.071(5) 0.078(5) 0.000(4) 0.000(4) -0.014(4) C11 0.063(5) 0.071(5) 0.038(4) -0.014(3) -0.012(3) -0.008(4) O12 0.180(7) 0.126(6) 0.066(4) 0.004(4) 0.005(4) -0.078(6) N12 0.044(3) 0.089(4) 0.041(3) -0.020(3) 0.005(2) -0.033(3) C12 0.054(4) 0.049(4) 0.057(4) -0.008(3) -0.012(4) -0.005(4) O13 0.039(2) 0.099(4) 0.058(3) -0.025(3) -0.010(2) -0.026(2) N13 0.037(3) 0.085(4) 0.038(3) -0.020(3) -0.003(2) -0.026(3) C13 0.051(4) 0.046(4) 0.066(5) -0.011(3) -0.013(3) -0.009(3) O14 0.042(3) 0.087(3) 0.041(2) -0.012(2) -0.006(2) -0.020(2) N14 0.052(3) 0.076(4) 0.038(3) -0.019(3) -0.002(2) -0.028(3) C14 0.039(4) 0.100(6) 0.041(4) -0.024(4) -0.007(3) 0.003(4) O15 0.082(4) 0.090(4) 0.050(3) 0.002(3) -0.026(3) -0.031(3) N15 0.037(3) 0.073(4) 0.038(3) -0.019(3) 0.001(2) -0.023(3) C15 0.058(5) 0.059(5) 0.099(6) -0.036(4) -0.017(4) -0.017(4) O16 0.094(4) 0.096(4) 0.040(3) -0.024(3) -0.002(3) -0.030(3) N16 0.070(4) 0.063(4) 0.037(3) -0.003(3) -0.006(3) -0.033(3) C16 0.073(5) 0.067(5) 0.072(5) -0.015(4) -0.009(4) -0.019(4) O17 0.064(3) 0.083(4) 0.084(4) -0.036(3) 0.026(3) -0.011(3) N17 0.048(3) 0.052(3) 0.040(3) -0.005(2) -0.002(2) -0.028(3) C17 0.080(5) 0.061(5) 0.071(5) -0.017(4) -0.004(4) -0.022(4) O18 0.070(3) 0.058(3) 0.070(3) -0.019(2) -0.014(3) -0.020(2) N18 0.053(3) 0.063(3) 0.033(3) 0.000(2) 0.001(2) -0.031(3) C18 0.049(4) 0.072(5) 0.034(3) -0.016(3) 0.008(3) -0.013(4) O19 0.065(4) 0.106(5) 0.133(6) -0.025(4) -0.032(4) -0.018(3) N19 0.047(3) 0.070(4) 0.034(3) 0.003(2) -0.009(2) -0.034(3) C19 0.065(5) 0.051(4) 0.051(4) -0.001(3) -0.008(3) -0.028(4) O20 0.090(4) 0.095(4) 0.087(4) -0.018(4) 0.017(3) -0.018(3) N20 0.037(3) 0.055(3) 0.037(3) 0.003(2) -0.007(2) -0.022(2) C20 0.053(4) 0.068(5) 0.048(4) 0.002(3) -0.002(3) -0.025(4) O21 0.039(2) 0.085(3) 0.056(3) -0.022(2) -0.013(2) -0.018(2) N21 0.125(6) 0.096(6) 0.057(4) 0.013(4) -0.009(4) -0.062(5) C21 0.065(5) 0.079(5) 0.062(5) -0.024(4) 0.001(4) -0.021(4) O22 0.032(2) 0.082(3) 0.051(3) -0.020(2) -0.0024(19) -0.018(2) N22 0.041(3) 0.058(3) 0.035(3) -0.009(2) -0.006(2) -0.012(3) C22 0.056(4) 0.059(4) 0.063(5) -0.010(4) -0.002(4) -0.010(4) O23 0.075(3) 0.131(5) 0.041(3) -0.030(3) 0.017(2) -0.056(3) N23 0.034(3) 0.048(3) 0.031(3) -0.004(2) -0.007(2) -0.012(2) C23 0.053(4) 0.057(4) 0.068(5) -0.008(4) 0.004(4) -0.012(3) O24 0.073(4) 0.147(5) 0.042(3) -0.009(3) -0.002(3) -0.054(4) N24 0.046(3) 0.057(3) 0.031(3) -0.004(2) -0.003(2) -0.018(2) C24 0.053(4) 0.064(5) 0.070(5) -0.001(4) -0.007(4) -0.015(4) O25 0.074(3) 0.070(3) 0.056(3) -0.015(2) 0.018(2) -0.035(3) N25 0.042(3) 0.045(3) 0.033(3) 0.000(2) -0.002(2) -0.016(2) C25 0.065(5) 0.066(5) 0.061(4) -0.010(4) -0.007(4) -0.018(4) O26 0.094(4) 0.116(4) 0.053(3) -0.015(3) 0.008(3) -0.073(4) N26 0.041(3) 0.050(3) 0.035(3) -0.004(2) -0.004(2) -0.016(2) C26 0.042(3) 0.060(4) 0.043(3) -0.010(3) 0.000(3) -0.024(3) O27 0.103(5) 0.084(5) 0.098(5) -0.004(4) 0.031(4) -0.019(4) N27 0.037(3) 0.050(3) 0.031(2) 0.002(2) -0.002(2) -0.023(2) C27 0.063(4) 0.048(4) 0.055(4) -0.012(3) 0.011(3) -0.022(3) O28 0.062(4) 0.124(5) 0.138(6) 0.016(4) 0.011(4) -0.037(4) N28 0.045(3) 0.046(3) 0.037(3) -0.005(2) -0.001(2) -0.013(2) C28 0.078(5) 0.055(5) 0.062(5) -0.018(4) 0.021(4) -0.021(4) O29 0.054(3) 0.063(3) 0.046(2) 0.007(2) -0.005(2) -0.034(2) N29 0.066(4) 0.053(3) 0.041(3) -0.011(2) 0.009(3) -0.025(3) C29 0.059(4) 0.077(5) 0.045(4) -0.028(4) 0.021(3) -0.031(4) O30 0.106(4) 0.160(6) 0.069(3) 0.038(4) -0.043(3) -0.098(4) N30 0.076(4) 0.073(4) 0.055(3) -0.018(3) 0.014(3) -0.046(3) C30 0.059(4) 0.078(5) 0.041(4) -0.009(3) 0.007(3) -0.043(4) O31 0.155(6) 0.101(5) 0.053(3) 0.029(3) -0.020(4) -0.058(4) N31 0.064(4) 0.069(4) 0.052(3) -0.009(3) 0.010(3) -0.038(3) C31 0.041(3) 0.051(4) 0.045(3) -0.013(3) -0.001(3) -0.018(3) O32 0.165(7) 0.262(10) 0.083(5) 0.074(6) -0.025(5) -0.151(8) N32 0.078(5) 0.063(5) 0.091(6) 0.017(4) 0.024(5) -0.019(4) C32 0.063(4) 0.060(4) 0.051(4) -0.010(3) 0.008(3) -0.033(4) N33 0.062(3) 0.050(3) 0.035(3) 0.002(2) -0.004(2) -0.035(3) C33 0.053(4) 0.071(5) 0.050(4) 0.007(3) 0.005(3) -0.036(4) N34 0.052(3) 0.054(3) 0.041(3) 0.001(2) -0.011(2) -0.029(3) C34 0.045(4) 0.076(5) 0.031(3) 0.001(3) -0.002(3) -0.036(4) N35 0.060(3) 0.083(4) 0.036(3) 0.014(3) -0.016(2) -0.046(3) C35 0.034(3) 0.076(5) 0.028(3) -0.012(3) -0.003(2) -0.023(3) N36 0.056(3) 0.068(4) 0.038(3) 0.007(3) -0.019(2) -0.026(3) C36 0.046(4) 0.073(5) 0.044(4) -0.018(3) 0.008(3) -0.029(3) N37 0.100(6) 0.110(6) 0.055(4) 0.019(4) -0.015(4) -0.053(5) C37 0.050(4) 0.100(6) 0.036(4) -0.028(4) 0.014(3) -0.042(4) N38 0.045(3) 0.067(4) 0.034(3) -0.007(2) -0.009(2) -0.029(3) C38 0.038(3) 0.087(5) 0.036(3) -0.011(3) 0.006(3) -0.035(4) N39 0.037(3) 0.073(4) 0.032(3) -0.007(3) -0.010(2) -0.022(3) C39 0.054(4) 0.082(5) 0.035(3) -0.007(3) 0.000(3) -0.041(4) N40 0.036(3) 0.068(4) 0.038(3) -0.014(2) -0.003(2) -0.016(2) C40 0.071(5) 0.104(6) 0.035(4) 0.010(4) -0.013(3) -0.056(5) N41 0.034(3) 0.063(3) 0.040(3) -0.015(2) -0.003(2) -0.018(2) C41 0.065(4) 0.069(5) 0.058(4) 0.008(4) -0.013(4) -0.033(4) N42 0.060(4) 0.095(5) 0.043(3) -0.019(3) 0.001(3) -0.049(4) C42 0.072(5) 0.076(5) 0.036(4) -0.004(3) -0.005(3) -0.033(4) C43 0.047(4) 0.081(5) 0.029(3) -0.009(3) 0.001(3) -0.038(4) C44 0.048(4) 0.064(4) 0.041(4) -0.011(3) -0.002(3) -0.029(3) C45 0.040(3) 0.054(4) 0.031(3) -0.009(3) -0.001(3) -0.025(3) C46 0.053(4) 0.048(4) 0.051(4) -0.018(3) -0.013(3) 0.000(3) C47 0.064(4) 0.051(4) 0.037(3) -0.018(3) 0.000(3) -0.009(3) C48 0.049(4) 0.053(4) 0.035(3) -0.006(3) -0.002(3) -0.027(3) C49 0.045(4) 0.070(5) 0.052(4) -0.013(4) -0.007(3) -0.019(3) C50 0.043(4) 0.061(4) 0.049(4) -0.020(3) -0.003(3) -0.015(3) C51 0.043(3) 0.074(4) 0.035(3) 0.004(3) -0.008(3) -0.043(3) C52 0.041(4) 0.071(5) 0.056(4) 0.012(3) 0.003(3) -0.032(3) C53 0.057(4) 0.111(6) 0.042(4) 0.002(4) -0.015(3) -0.056(5) C54 0.076(5) 0.092(6) 0.043(4) -0.006(4) -0.008(4) -0.060(5) C55 0.060(4) 0.067(4) 0.042(4) -0.001(3) -0.002(3) -0.041(4) C56 0.034(3) 0.065(4) 0.039(3) 0.009(3) -0.003(3) -0.026(3) C57 0.040(3) 0.065(4) 0.040(3) 0.003(3) -0.007(3) -0.025(3) C58 0.033(3) 0.052(4) 0.051(4) 0.003(3) 0.005(3) -0.007(3) C59 0.041(3) 0.053(4) 0.039(3) 0.000(3) 0.001(3) -0.017(3) C60 0.033(3) 0.050(4) 0.041(3) -0.007(3) -0.006(3) -0.010(3) C61 0.057(4) 0.047(4) 0.032(3) -0.009(3) 0.009(3) -0.018(3) C62 0.071(4) 0.042(4) 0.031(3) -0.005(3) -0.002(3) -0.027(3) C63 0.055(4) 0.053(4) 0.034(3) -0.006(3) 0.003(3) -0.028(3) C64 0.068(5) 0.076(5) 0.036(3) -0.011(3) 0.009(3) -0.044(4) C65 0.070(5) 0.098(6) 0.052(4) -0.007(4) 0.006(4) -0.050(4) C66 0.062(5) 0.102(6) 0.071(5) 0.001(5) 0.002(4) -0.050(5) C67 0.057(4) 0.087(5) 0.056(4) 0.003(4) -0.005(3) -0.035(4) C68 0.043(4) 0.066(4) 0.045(4) -0.004(3) -0.001(3) -0.031(3) C69 0.045(4) 0.056(4) 0.040(3) 0.001(3) -0.004(3) -0.022(3) C70 0.036(3) 0.036(3) 0.038(3) -0.003(3) 0.000(3) -0.007(3) C71 0.046(4) 0.063(4) 0.040(4) -0.011(3) -0.001(3) -0.017(3) C72 0.064(4) 0.053(4) 0.050(4) -0.007(3) -0.012(3) -0.015(4) C73 0.080(5) 0.051(4) 0.035(4) -0.005(3) -0.005(3) -0.018(4) C74 0.072(5) 0.056(4) 0.052(4) -0.001(3) 0.009(4) -0.022(4) C75 0.058(4) 0.056(4) 0.040(4) -0.012(3) 0.006(3) -0.026(3) C76 0.037(3) 0.047(4) 0.036(3) -0.010(3) 0.003(3) -0.014(3) C77 0.045(4) 0.059(4) 0.043(4) -0.008(3) 0.005(3) -0.023(3) C78 0.054(4) 0.061(4) 0.044(4) -0.007(3) 0.003(3) -0.025(3) C79 0.069(5) 0.059(4) 0.038(4) 0.004(3) 0.007(3) -0.025(4) C80 0.046(4) 0.070(5) 0.039(3) 0.001(3) -0.005(3) -0.022(3) C81 0.037(3) 0.044(4) 0.039(3) -0.010(3) 0.004(3) -0.013(3) C82 0.047(4) 0.053(4) 0.041(3) -0.005(3) -0.006(3) -0.022(3) C83 0.046(4) 0.058(4) 0.037(3) -0.007(3) -0.009(3) -0.018(3) C84 0.042(3) 0.044(3) 0.032(3) -0.006(3) -0.006(3) -0.013(3) C85 0.036(3) 0.050(4) 0.047(4) -0.001(3) -0.001(3) -0.016(3) C86 0.044(4) 0.062(4) 0.040(3) 0.002(3) -0.004(3) -0.017(3) C87 0.054(4) 0.051(4) 0.032(3) -0.003(3) 0.012(3) -0.006(3) C88 0.064(4) 0.064(5) 0.043(4) -0.015(3) 0.007(3) -0.020(4) C89 0.081(5) 0.080(6) 0.060(5) -0.012(4) 0.010(4) -0.045(5) C90 0.111(7) 0.096(7) 0.068(5) -0.034(5) 0.019(5) -0.050(6) C91 0.189(11) 0.114(8) 0.100(7) -0.048(6) 0.049(7) -0.118(8) C92 0.130(8) 0.109(7) 0.087(6) -0.050(6) 0.055(6) -0.075(6) C93 0.106(6) 0.067(5) 0.053(4) -0.009(4) 0.015(4) -0.058(5) C94 0.080(5) 0.064(5) 0.047(4) -0.004(4) 0.017(4) -0.046(4) C95 0.075(5) 0.059(4) 0.044(4) 0.005(3) 0.011(3) -0.039(4) C96 0.071(5) 0.066(5) 0.068(5) -0.013(4) 0.000(4) -0.024(4) C97 0.093(6) 0.068(5) 0.055(4) -0.016(4) 0.006(4) -0.028(5) C98 0.069(5) 0.075(6) 0.087(6) 0.015(5) 0.004(5) -0.032(5) C99 0.058(5) 0.102(7) 0.099(7) -0.015(6) 0.008(5) -0.037(5) C100 0.079(6) 0.098(6) 0.090(6) -0.024(5) 0.005(5) -0.055(5) C101 0.057(4) 0.040(4) 0.035(3) -0.010(3) -0.009(3) -0.012(3) C102 0.062(4) 0.060(5) 0.053(4) 0.001(4) -0.012(3) -0.019(4) C103 0.060(5) 0.081(6) 0.050(4) -0.034(4) -0.008(4) 0.002(4) C104 0.050(4) 0.067(5) 0.063(5) -0.006(4) -0.007(3) -0.017(4) C105 0.042(3) 0.071(5) 0.040(4) -0.017(3) 0.005(3) -0.016(3) C106 0.054(4) 0.046(4) 0.035(3) -0.003(3) 0.001(3) -0.021(3) C107 0.105(6) 0.054(4) 0.048(4) -0.016(3) 0.007(4) -0.033(4) C108 0.089(5) 0.070(5) 0.039(4) -0.007(3) -0.002(4) -0.044(4) C109 0.050(4) 0.059(4) 0.038(3) -0.006(3) -0.011(3) -0.023(3) C110 0.035(3) 0.046(4) 0.035(3) -0.004(3) -0.006(3) -0.014(3) C111 0.053(4) 0.068(4) 0.038(3) 0.001(3) -0.002(3) -0.027(3) C112 0.031(3) 0.068(4) 0.032(3) -0.002(3) 0.003(3) -0.021(3) C113 0.030(3) 0.067(4) 0.047(4) -0.002(3) -0.002(3) -0.021(3) C114 0.039(3) 0.074(5) 0.038(3) -0.004(3) 0.001(3) -0.030(3) C115 0.047(4) 0.074(5) 0.060(4) 0.011(4) -0.014(3) -0.033(4) C116 0.050(4) 0.062(5) 0.070(5) 0.000(4) 0.000(4) -0.024(3) C117 0.047(4) 0.074(5) 0.058(4) -0.002(4) -0.011(3) -0.034(4) C118 0.030(3) 0.062(4) 0.043(3) -0.003(3) -0.010(3) -0.018(3) C119 0.040(4) 0.054(4) 0.048(4) -0.012(3) -0.009(3) -0.020(3) C120 0.037(3) 0.061(4) 0.040(3) -0.018(3) -0.003(3) -0.023(3) C121 0.049(4) 0.067(4) 0.037(3) -0.020(3) 0.004(3) -0.020(3) C122 0.050(4) 0.080(5) 0.042(4) -0.018(3) 0.005(3) -0.035(4) C123 0.059(4) 0.084(5) 0.037(3) -0.019(3) 0.006(3) -0.050(4) C124 0.043(4) 0.086(5) 0.042(4) -0.023(3) 0.009(3) -0.035(4) C125 0.036(3) 0.077(5) 0.055(4) -0.030(4) -0.003(3) -0.021(3) C126 0.040(3) 0.051(4) 0.036(3) 0.003(3) 0.003(3) -0.023(3) C127 0.029(3) 0.060(4) 0.038(3) 0.003(3) -0.008(2) -0.016(3) C128 0.040(4) 0.078(5) 0.040(4) 0.005(3) -0.008(3) -0.021(3) C129 0.070(5) 0.067(5) 0.034(3) -0.003(3) -0.013(3) -0.038(4) C130 0.046(4) 0.068(4) 0.036(3) -0.005(3) -0.007(3) -0.019(3) C131 0.028(3) 0.049(4) 0.036(3) -0.001(3) -0.002(2) -0.018(3) C132 0.035(3) 0.055(4) 0.038(3) 0.000(3) -0.003(3) -0.016(3) C133 0.035(3) 0.044(4) 0.053(4) -0.002(3) 0.003(3) -0.013(3) C134 0.041(3) 0.047(4) 0.036(3) 0.000(3) 0.003(3) -0.028(3) C135 0.035(3) 0.058(4) 0.037(3) 0.005(3) 0.000(3) -0.026(3) C136 0.044(3) 0.045(4) 0.040(3) 0.000(3) -0.008(3) -0.020(3) C137 0.056(4) 0.055(4) 0.029(3) -0.010(3) -0.004(3) -0.029(3) C138 0.052(4) 0.053(4) 0.036(3) -0.001(3) -0.002(3) -0.026(3) C139 0.056(4) 0.057(4) 0.064(4) -0.003(3) -0.002(3) -0.023(3) C140 0.048(4) 0.089(6) 0.071(5) 0.003(4) -0.003(4) -0.030(4) C141 0.056(5) 0.120(7) 0.072(5) 0.008(5) -0.009(4) -0.045(5) C142 0.049(4) 0.097(6) 0.072(5) 0.017(4) -0.021(4) -0.039(4) C143 0.049(4) 0.068(4) 0.042(4) -0.005(3) -0.009(3) -0.029(3) C144 0.068(5) 0.069(5) 0.054(4) 0.008(4) -0.023(4) -0.042(4) C145 0.060(4) 0.053(4) 0.043(4) -0.003(3) -0.006(3) -0.026(3) C146 0.095(6) 0.099(6) 0.044(4) 0.002(4) -0.018(4) -0.059(5) C147 0.115(7) 0.078(5) 0.043(4) 0.014(4) -0.023(4) -0.058(5) C148 0.070(5) 0.065(5) 0.038(4) 0.005(3) 0.001(3) -0.016(4) C149 0.077(5) 0.089(6) 0.051(4) -0.001(4) 0.006(4) -0.038(4) C150 0.057(4) 0.070(5) 0.039(4) 0.001(3) -0.005(3) -0.022(4) O1S 0.114(5) 0.116(5) 0.088(4) 0.014(3) -0.037(3) -0.077(4) O2S 0.105(4) 0.107(4) 0.071(4) 0.013(3) -0.013(3) -0.047(4) O3S 0.106(5) 0.110(5) 0.149(6) 0.005(4) -0.041(4) -0.053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 1.941(5) . ? Fe1 N6 1.956(5) . ? Fe1 N2 1.956(5) . ? Fe1 N4 1.956(5) . ? Fe1 N1 1.966(5) . ? Fe1 N3 1.967(5) . ? S1 O1 1.460(4) . ? S1 O2 1.463(4) . ? S1 O3 1.479(4) . ? S1 O4 1.484(5) . ? N1 C5 1.339(8) . ? N1 C1 1.349(7) . ? C1 C2 1.379(8) . ? C1 C6 1.459(9) . ? Fe2 N24 1.950(5) . ? Fe2 N27 1.956(5) . ? Fe2 N23 1.963(5) . ? Fe2 N22 1.968(5) . ? Fe2 N26 1.973(5) . ? Fe2 N25 1.974(5) . ? S2 O5 1.455(4) . ? S2 O6 1.460(4) . ? S2 O8 1.479(4) . ? S2 O7 1.489(4) . ? N2 C10 1.358(7) . ? N2 C6 1.358(8) . ? C2 C3 1.369(10) . ? N3 C30 1.338(7) . ? N3 C26 1.352(8) . ? C3 C4 1.417(10) . ? N4 C31 1.351(7) . ? N4 C35 1.375(7) . ? C4 C5 1.373(8) . ? N5 C51 1.358(8) . ? N5 C55 1.360(7) . ? N6 C60 1.346(7) . ? N6 C56 1.363(7) . ? C6 C7 1.436(9) . ? N7 C12 1.366(9) . ? N7 C11 1.406(9) . ? C7 C8 1.371(10) . ? N8 C13 1.378(9) . ? N8 C12 1.382(9) . ? C8 C9 1.366(10) . ? O9 C62 1.225(7) . ? N9 C19 1.381(8) . ? N9 C18 1.458(8) . ? C9 C10 1.393(8) . ? C9 C11 1.530(10) . ? O10 C69 1.206(7) . ? N10 C19 1.385(8) . ? N10 C20 1.394(8) . ? O11 N21 1.224(9) . ? N11 O19 1.216(8) . ? N11 O20 1.241(8) . ? N11 C23 1.492(9) . ? O12 N21 1.196(9) . ? N12 C37 1.379(9) . ? N12 C36 1.455(8) . ? C12 O17 1.222(8) . ? O13 C37 1.221(7) . ? N13 C37 1.373(8) . ? N13 C38 1.378(8) . ? C13 C18 1.393(9) . ? C13 C14 1.436(9) . ? O14 C44 1.222(7) . ? N14 C44 1.364(7) . ? N14 C43 1.413(8) . ? C14 C15 1.364(11) . ? O15 N16 1.224(7) . ? N15 C45 1.383(7) . ? N15 C44 1.408(8) . ? C15 C16 1.366(11) . ? O16 N16 1.204(7) . ? N16 C48 1.479(7) . ? C16 C17 1.356(10) . ? N17 C62 1.359(8) . ? N17 C61 1.446(7) . ? C17 C18 1.351(10) . ? O18 C19 1.223(7) . ? N18 C62 1.372(8) . ? N18 C63 1.373(7) . ? N19 C69 1.361(7) . ? N19 C68 1.411(7) . ? N20 C69 1.405(7) . ? N20 C70 1.415(7) . ? C20 C21 1.356(9) . ? C20 C25 1.397(9) . ? O21 C112 1.214(7) . ? N21 C73 1.500(9) . ? C21 C22 1.366(9) . ? O22 C119 1.217(7) . ? N22 C105 1.338(7) . ? N22 C101 1.346(8) . ? C22 C23 1.374(10) . ? O23 N42 1.237(6) . ? N23 C110 1.327(7) . ? N23 C106 1.370(7) . ? C23 C24 1.353(10) . ? O24 N42 1.204(7) . ? N24 C80 1.359(7) . ? N24 C76 1.368(7) . ? C24 C25 1.396(9) . ? O25 C87 1.235(7) . ? N25 C81 1.347(7) . ? N25 C85 1.370(7) . ? O26 C94 1.206(8) . ? N26 C126 1.344(7) . ? N26 C130 1.355(7) . ? C26 C27 1.354(8) . ? C26 C31 1.487(8) . ? O27 N32 1.230(9) . ? N27 C135 1.344(7) . ? N27 C131 1.353(6) . ? C27 C28 1.383(9) . ? O28 N32 1.213(9) . ? N28 C87 1.336(8) . ? N28 C86 1.438(7) . ? C28 C29 1.352(9) . ? O29 C137 1.242(7) . ? N29 C87 1.386(8) . ? N29 C88 1.404(9) . ? C29 C30 1.381(9) . ? O30 C144 1.196(7) . ? N30 C94 1.367(9) . ? N30 C93 1.429(9) . ? O31 N37 1.238(8) . ? N31 C94 1.391(8) . ? N31 C95 1.420(8) . ? C31 C32 1.396(9) . ? O32 N37 1.206(9) . ? N32 C98 1.481(10) . ? C32 C33 1.363(8) . ? N33 C137 1.352(7) . ? N33 C136 1.436(7) . ? C33 C34 1.399(9) . ? N34 C137 1.361(7) . ? N34 C138 1.398(7) . ? C34 C35 1.376(8) . ? C34 C36 1.532(8) . ? N35 C144 1.328(8) . ? N35 C143 1.440(8) . ? N36 C145 1.402(8) . ? N36 C144 1.413(8) . ? N37 C148 1.425(9) . ? N38 C112 1.373(7) . ? N38 C111 1.441(8) . ? C38 C39 1.403(9) . ? C38 C43 1.426(8) . ? N39 C112 1.355(8) . ? N39 C113 1.410(8) . ? C39 C40 1.357(9) . ? N40 C119 1.387(7) . ? N40 C118 1.420(7) . ? C40 C41 1.427(10) . ? N41 C120 1.381(7) . ? N41 C119 1.382(7) . ? C41 C42 1.377(9) . ? N42 C123 1.444(8) . ? C42 C43 1.364(9) . ? C45 C46 1.381(8) . ? C45 C50 1.406(8) . ? C46 C47 1.390(8) . ? C47 C48 1.375(8) . ? C48 C49 1.372(8) . ? C49 C50 1.373(8) . ? C51 C52 1.399(8) . ? C51 C56 1.483(8) . ? C52 C53 1.375(9) . ? C53 C54 1.375(10) . ? C54 C55 1.381(9) . ? C56 C57 1.363(8) . ? C57 C58 1.376(8) . ? C58 C59 1.377(8) . ? C59 C60 1.407(8) . ? C59 C61 1.502(8) . ? C63 C64 1.401(8) . ? C63 C68 1.408(8) . ? C64 C65 1.394(9) . ? C65 C66 1.374(10) . ? C66 C67 1.393(9) . ? C67 C68 1.398(8) . ? C70 C75 1.365(8) . ? C70 C71 1.387(8) . ? C71 C72 1.380(9) . ? C72 C73 1.355(10) . ? C73 C74 1.364(10) . ? C74 C75 1.402(9) . ? C76 C77 1.393(8) . ? C76 C81 1.482(8) . ? C77 C78 1.384(8) . ? C78 C79 1.349(9) . ? C79 C80 1.372(9) . ? C81 C82 1.366(8) . ? C82 C83 1.350(8) . ? C83 C84 1.397(8) . ? C84 C85 1.351(8) . ? C84 C86 1.526(8) . ? C88 C93 1.388(9) . ? C88 C89 1.395(9) . ? C89 C90 1.357(11) . ? C90 C91 1.416(12) . ? C91 C92 1.339(11) . ? C92 C93 1.414(11) . ? C95 C100 1.382(10) . ? C95 C96 1.408(10) . ? C96 C97 1.355(10) . ? C97 C98 1.358(11) . ? C98 C99 1.393(12) . ? C99 C100 1.404(11) . ? C101 C102 1.374(9) . ? C101 C106 1.476(8) . ? C102 C103 1.425(10) . ? C103 C104 1.364(11) . ? C104 C105 1.349(9) . ? C106 C107 1.384(9) . ? C107 C108 1.403(9) . ? C108 C109 1.382(9) . ? C109 C110 1.372(8) . ? C109 C111 1.527(8) . ? C113 C114 1.409(8) . ? C113 C118 1.430(8) . ? C114 C115 1.376(9) . ? C115 C116 1.381(9) . ? C116 C117 1.398(9) . ? C117 C118 1.356(9) . ? C120 C125 1.398(8) . ? C120 C121 1.416(8) . ? C121 C122 1.381(8) . ? C122 C123 1.393(8) . ? C123 C124 1.392(9) . ? C124 C125 1.379(9) . ? C126 C127 1.397(8) . ? C126 C131 1.471(8) . ? C127 C128 1.354(8) . ? C128 C129 1.378(9) . ? C129 C130 1.417(8) . ? C131 C132 1.394(8) . ? C132 C133 1.382(8) . ? C133 C134 1.379(8) . ? C134 C135 1.389(8) . ? C134 C136 1.509(8) . ? C138 C139 1.395(9) . ? C138 C143 1.415(8) . ? C139 C140 1.379(9) . ? C140 C141 1.419(10) . ? C141 C142 1.373(10) . ? C142 C143 1.371(8) . ? C145 C150 1.367(9) . ? C145 C146 1.368(9) . ? C146 C147 1.395(9) . ? C147 C148 1.356(10) . ? C148 C149 1.364(10) . ? C149 C150 1.378(9) . ? N1S C1S 1.336(11) . ? N1S C2S 1.424(12) . ? N1S C3S 1.468(12) . ? C1S O5S 1.249(11) . ? N2S C4S 1.309(11) . ? N2S C5S 1.444(11) . ? N2S C6S 1.445(11) . ? N3S C7S 1.403(14) . ? N3S C9S 1.477(15) . ? N3S C8S 1.499(14) . ? O4S C4S 1.316(12) . ? N4S C10S 1.295(9) . ? N4S C11S 1.447(10) . ? N4S C12S 1.454(10) . ? N5S C13S 1.345(9) . ? N5S C15S 1.417(9) . ? N5S C14S 1.463(10) . ? O6S C7S 1.259(14) . ? N6S C16S 1.347(15) . ? N6S C17S 1.452(14) . ? N6S C18S 1.460(14) . ? O7S C10S 1.304(9) . ? N7S C19S 1.310(14) . ? N7S C21S 1.448(16) . ? N7S C20S 1.461(14) . ? O8S C13S 1.231(8) . ? N8S C22S 1.369(13) . ? N8S C23S 1.492(14) . ? N8S C24S 1.515(17) . ? O9S C16S 1.326(16) . ? N9S C25S 1.313(11) . ? N9S C26S 1.546(17) . ? N9S C27S 1.563(13) . ? O10S C22S 1.200(11) . ? N10S C31S 1.285(10) . ? N10S C33S 1.434(11) . ? N10S C32S 1.455(12) . ? O11S C25S 1.192(10) . ? N11S C28S 1.280(13) . ? N11S C29S 1.470(12) . ? N11S C30S 1.483(11) . ? O12S C19S 1.219(13) . ? O13S C31S 1.270(10) . ? O14S C28S 1.342(14) . ? 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 N5 Fe1 N6 81.94(19) . . ? N5 Fe1 N2 175.2(2) . . ? N6 Fe1 N2 95.30(18) . . ? N5 Fe1 N4 91.59(18) . . ? N6 Fe1 N4 94.74(19) . . ? N2 Fe1 N4 92.5(2) . . ? N5 Fe1 N1 93.6(2) . . ? N6 Fe1 N1 90.03(19) . . ? N2 Fe1 N1 82.5(2) . . ? N4 Fe1 N1 173.4(2) . . ? N5 Fe1 N3 93.8(2) . . ? N6 Fe1 N3 174.38(19) . . ? N2 Fe1 N3 89.16(19) . . ? N4 Fe1 N3 81.6(2) . . ? N1 Fe1 N3 94.0(2) . . ? O1 S1 O2 111.9(3) . . ? O1 S1 O3 109.4(3) . . ? O2 S1 O3 109.9(2) . . ? O1 S1 O4 108.8(3) . . ? O2 S1 O4 110.3(3) . . ? O3 S1 O4 106.4(3) . . ? C5 N1 C1 118.5(5) . . ? C5 N1 Fe1 127.4(4) . . ? C1 N1 Fe1 114.1(4) . . ? N1 C1 C2 121.6(6) . . ? N1 C1 C6 114.7(5) . . ? C2 C1 C6 123.7(6) . . ? N24 Fe2 N27 90.95(19) . . ? N24 Fe2 N23 173.63(19) . . ? N27 Fe2 N23 93.31(18) . . ? N24 Fe2 N22 93.5(2) . . ? N27 Fe2 N22 173.5(2) . . ? N23 Fe2 N22 82.7(2) . . ? N24 Fe2 N26 94.9(2) . . ? N27 Fe2 N26 81.26(19) . . ? N23 Fe2 N26 90.41(19) . . ? N22 Fe2 N26 93.59(19) . . ? N24 Fe2 N25 81.51(19) . . ? N27 Fe2 N25 94.63(18) . . ? N23 Fe2 N25 93.41(18) . . ? N22 Fe2 N25 90.75(19) . . ? N26 Fe2 N25 174.6(2) . . ? O5 S2 O6 112.7(3) . . ? O5 S2 O8 109.2(2) . . ? O6 S2 O8 109.3(2) . . ? O5 S2 O7 108.7(2) . . ? O6 S2 O7 108.8(2) . . ? O8 S2 O7 108.0(2) . . ? C10 N2 C6 118.6(5) . . ? C10 N2 Fe1 127.1(4) . . ? C6 N2 Fe1 114.3(4) . . ? C3 C2 C1 119.5(6) . . ? C30 N3 C26 117.1(5) . . ? C30 N3 Fe1 127.1(5) . . ? C26 N3 Fe1 115.8(4) . . ? C2 C3 C4 119.7(6) . . ? C31 N4 C35 118.2(5) . . ? C31 N4 Fe1 115.5(4) . . ? C35 N4 Fe1 126.1(4) . . ? C5 C4 C3 116.6(7) . . ? C51 N5 C55 117.4(5) . . ? C51 N5 Fe1 115.8(4) . . ? C55 N5 Fe1 126.8(4) . . ? N1 C5 C4 124.0(6) . . ? C60 N6 C56 117.3(5) . . ? C60 N6 Fe1 126.9(4) . . ? C56 N6 Fe1 115.7(4) . . ? N2 C6 C7 120.0(6) . . ? N2 C6 C1 114.4(5) . . ? C7 C6 C1 125.5(6) . . ? C12 N7 C11 124.8(6) . . ? C8 C7 C6 118.1(7) . . ? C13 N8 C12 128.1(6) . . ? C9 C8 C7 122.7(7) . . ? C19 N9 C18 117.1(6) . . ? C8 C9 C10 116.4(7) . . ? C8 C9 C11 123.9(6) . . ? C10 C9 C11 119.7(7) . . ? C19 N10 C20 125.9(6) . . ? N2 C10 C9 124.0(6) . . ? O19 N11 O20 122.7(7) . . ? O19 N11 C23 119.6(7) . . ? O20 N11 C23 117.7(7) . . ? N7 C11 C9 115.6(6) . . ? C37 N12 C36 121.8(5) . . ? O17 C12 N7 118.9(7) . . ? O17 C12 N8 125.4(7) . . ? N7 C12 N8 115.7(6) . . ? C37 N13 C38 127.5(5) . . ? N8 C13 C18 120.7(6) . . ? N8 C13 C14 122.1(7) . . ? C18 C13 C14 117.0(7) . . ? C44 N14 C43 124.4(5) . . ? C15 C14 C13 119.3(7) . . ? C45 N15 C44 126.9(5) . . ? C14 C15 C16 121.7(7) . . ? O16 N16 O15 124.1(6) . . ? O16 N16 C48 118.8(6) . . ? O15 N16 C48 117.1(6) . . ? C17 C16 C15 118.9(8) . . ? C62 N17 C61 121.6(5) . . ? C18 C17 C16 122.2(8) . . ? C62 N18 C63 128.8(5) . . ? C17 C18 C13 120.7(7) . . ? C17 C18 N9 122.0(6) . . ? C13 C18 N9 117.1(7) . . ? C69 N19 C68 125.9(5) . . ? O18 C19 N9 123.9(6) . . ? O18 C19 N10 123.0(6) . . ? N9 C19 N10 113.0(6) . . ? C69 N20 C70 125.1(5) . . ? C21 C20 N10 118.3(6) . . ? C21 C20 C25 118.4(7) . . ? N10 C20 C25 123.3(6) . . ? O12 N21 O11 124.9(8) . . ? O12 N21 C73 115.9(8) . . ? O11 N21 C73 119.1(8) . . ? C20 C21 C22 123.4(7) . . ? C105 N22 C101 117.5(5) . . ? C105 N22 Fe2 127.9(5) . . ? C101 N22 Fe2 114.5(4) . . ? C21 C22 C23 117.2(7) . . ? C110 N23 C106 118.3(5) . . ? C110 N23 Fe2 127.6(4) . . ? C106 N23 Fe2 113.9(4) . . ? C24 C23 C22 122.2(7) . . ? C24 C23 N11 117.6(7) . . ? C22 C23 N11 120.2(7) . . ? C80 N24 C76 116.4(5) . . ? C80 N24 Fe2 128.1(4) . . ? C76 N24 Fe2 115.5(4) . . ? C23 C24 C25 119.6(7) . . ? C81 N25 C85 116.7(5) . . ? C81 N25 Fe2 116.0(4) . . ? C85 N25 Fe2 127.3(4) . . ? C24 C25 C20 119.0(7) . . ? C126 N26 C130 118.1(5) . . ? C126 N26 Fe2 115.4(4) . . ? C130 N26 Fe2 126.5(4) . . ? N3 C26 C27 122.2(6) . . ? N3 C26 C31 112.9(5) . . ? C27 C26 C31 124.8(6) . . ? C135 N27 C131 118.1(5) . . ? C135 N27 Fe2 126.0(4) . . ? C131 N27 Fe2 115.8(4) . . ? C26 C27 C28 120.0(7) . . ? C87 N28 C86 120.2(5) . . ? C29 C28 C27 118.5(6) . . ? C87 N29 C88 129.0(6) . . ? C28 C29 C30 119.2(6) . . ? C94 N30 C93 122.4(6) . . ? N3 C30 C29 122.9(6) . . ? C94 N31 C95 125.5(6) . . ? N4 C31 C32 122.0(5) . . ? N4 C31 C26 114.0(6) . . ? C32 C31 C26 124.0(6) . . ? O28 N32 O27 126.4(8) . . ? O28 N32 C98 117.9(9) . . ? O27 N32 C98 115.4(9) . . ? C33 C32 C31 119.5(6) . . ? C137 N33 C136 122.5(5) . . ? C32 C33 C34 119.2(6) . . ? C137 N34 C138 127.4(5) . . ? C35 C34 C33 119.5(5) . . ? C35 C34 C36 120.8(6) . . ? C33 C34 C36 119.6(6) . . ? C144 N35 C143 127.5(5) . . ? N4 C35 C34 121.5(6) . . ? C145 N36 C144 126.7(5) . . ? N12 C36 C34 112.8(5) . . ? O32 N37 O31 120.8(7) . . ? O32 N37 C148 120.0(8) . . ? O31 N37 C148 119.1(8) . . ? O13 C37 N13 125.0(7) . . ? O13 C37 N12 121.7(6) . . ? N13 C37 N12 113.3(6) . . ? C112 N38 C111 121.1(5) . . ? N13 C38 C39 121.7(6) . . ? N13 C38 C43 119.3(6) . . ? C39 C38 C43 119.0(6) . . ? C112 N39 C113 126.6(5) . . ? C40 C39 C38 119.2(6) . . ? C119 N40 C118 124.9(5) . . ? C39 C40 C41 122.5(6) . . ? C120 N41 C119 126.1(5) . . ? C42 C41 C40 117.2(7) . . ? O24 N42 O23 122.7(6) . . ? O24 N42 C123 119.2(6) . . ? O23 N42 C123 118.1(6) . . ? C43 C42 C41 122.2(6) . . ? C42 C43 N14 122.0(5) . . ? C42 C43 C38 119.9(6) . . ? N14 C43 C38 118.1(6) . . ? O14 C44 N14 126.0(6) . . ? O14 C44 N15 122.7(5) . . ? N14 C44 N15 111.3(5) . . ? C46 C45 N15 124.1(5) . . ? C46 C45 C50 118.9(5) . . ? N15 C45 C50 116.8(5) . . ? C45 C46 C47 120.2(6) . . ? C48 C47 C46 119.3(6) . . ? C49 C48 C47 121.9(5) . . ? C49 C48 N16 119.6(6) . . ? C47 C48 N16 118.5(5) . . ? C48 C49 C50 118.8(6) . . ? C49 C50 C45 120.9(6) . . ? N5 C51 C52 122.4(6) . . ? N5 C51 C56 113.8(5) . . ? C52 C51 C56 123.7(6) . . ? C53 C52 C51 118.9(6) . . ? C52 C53 C54 119.1(6) . . ? C53 C54 C55 120.0(6) . . ? N5 C55 C54 122.1(6) . . ? C57 C56 N6 122.5(5) . . ? C57 C56 C51 124.9(5) . . ? N6 C56 C51 112.6(5) . . ? C56 C57 C58 119.1(6) . . ? C57 C58 C59 121.0(6) . . ? C58 C59 C60 116.4(6) . . ? C58 C59 C61 122.8(5) . . ? C60 C59 C61 120.7(5) . . ? N6 C60 C59 123.5(5) . . ? N17 C61 C59 113.8(5) . . ? O9 C62 N17 122.9(6) . . ? O9 C62 N18 122.8(6) . . ? N17 C62 N18 114.3(5) . . ? N18 C63 C64 121.6(6) . . ? N18 C63 C68 119.9(5) . . ? C64 C63 C68 118.5(6) . . ? C65 C64 C63 120.1(6) . . ? C66 C65 C64 121.1(7) . . ? C65 C66 C67 119.9(7) . . ? C66 C67 C68 119.8(7) . . ? C67 C68 C63 120.6(6) . . ? C67 C68 N19 120.7(6) . . ? C63 C68 N19 118.7(5) . . ? O10 C69 N19 125.9(6) . . ? O10 C69 N20 123.2(5) . . ? N19 C69 N20 110.9(5) . . ? C75 C70 C71 120.8(6) . . ? C75 C70 N20 116.8(5) . . ? C71 C70 N20 122.4(6) . . ? C72 C71 C70 118.9(7) . . ? C73 C72 C71 119.5(7) . . ? C72 C73 C74 123.1(6) . . ? C72 C73 N21 117.9(7) . . ? C74 C73 N21 118.9(7) . . ? C73 C74 C75 117.5(7) . . ? C70 C75 C74 120.2(6) . . ? N24 C76 C77 122.6(5) . . ? N24 C76 C81 113.7(5) . . ? C77 C76 C81 123.7(5) . . ? C78 C77 C76 118.5(6) . . ? C79 C78 C77 119.0(6) . . ? C78 C79 C80 120.8(6) . . ? N24 C80 C79 122.4(6) . . ? N25 C81 C82 122.1(5) . . ? N25 C81 C76 113.1(5) . . ? C82 C81 C76 124.7(6) . . ? C83 C82 C81 120.2(6) . . ? C82 C83 C84 119.6(6) . . ? C85 C84 C83 117.7(5) . . ? C85 C84 C86 121.9(6) . . ? C83 C84 C86 120.3(5) . . ? C84 C85 N25 123.7(6) . . ? N28 C86 C84 113.3(5) . . ? O25 C87 N28 123.9(6) . . ? O25 C87 N29 122.0(7) . . ? N28 C87 N29 114.0(5) . . ? C93 C88 C89 119.1(7) . . ? C93 C88 N29 118.1(6) . . ? C89 C88 N29 122.7(6) . . ? C90 C89 C88 121.5(7) . . ? C89 C90 C91 119.3(8) . . ? C92 C91 C90 119.6(8) . . ? C91 C92 C93 121.6(8) . . ? C88 C93 C92 118.6(7) . . ? C88 C93 N30 120.2(6) . . ? C92 C93 N30 121.2(6) . . ? O26 C94 N30 124.8(7) . . ? O26 C94 N31 124.0(7) . . ? N30 C94 N31 111.2(7) . . ? C100 C95 C96 117.7(7) . . ? C100 C95 N31 126.5(7) . . ? C96 C95 N31 115.8(7) . . ? C97 C96 C95 120.8(8) . . ? C96 C97 C98 121.5(8) . . ? C97 C98 C99 120.1(8) . . ? C97 C98 N32 122.4(9) . . ? C99 C98 N32 117.4(9) . . ? C98 C99 C100 118.4(8) . . ? C95 C100 C99 121.3(8) . . ? N22 C101 C102 123.0(6) . . ? N22 C101 C106 114.5(5) . . ? C102 C101 C106 122.5(6) . . ? C101 C102 C103 117.0(7) . . ? C104 C103 C102 119.6(7) . . ? C105 C104 C103 118.4(7) . . ? N22 C105 C104 124.4(7) . . ? N23 C106 C107 121.3(5) . . ? N23 C106 C101 114.1(5) . . ? C107 C106 C101 124.6(6) . . ? C106 C107 C108 119.0(6) . . ? C109 C108 C107 119.1(7) . . ? C110 C109 C108 118.4(6) . . ? C110 C109 C111 121.9(6) . . ? C108 C109 C111 119.7(6) . . ? N23 C110 C109 124.0(6) . . ? N38 C111 C109 114.8(5) . . ? O21 C112 N39 125.2(6) . . ? O21 C112 N38 121.9(6) . . ? N39 C112 N38 113.0(5) . . ? C114 C113 N39 123.1(6) . . ? C114 C113 C118 117.6(6) . . ? N39 C113 C118 119.3(5) . . ? C115 C114 C113 120.4(6) . . ? C114 C115 C116 121.7(6) . . ? C115 C116 C117 118.0(7) . . ? C118 C117 C116 122.1(6) . . ? C117 C118 N40 121.9(6) . . ? C117 C118 C113 120.0(6) . . ? N40 C118 C113 118.1(5) . . ? O22 C119 N41 124.9(6) . . ? O22 C119 N40 124.0(5) . . ? N41 C119 N40 111.1(5) . . ? N41 C120 C125 126.3(6) . . ? N41 C120 C121 115.7(5) . . ? C125 C120 C121 118.0(6) . . ? C122 C121 C120 121.7(6) . . ? C121 C122 C123 118.5(6) . . ? C124 C123 C122 121.0(6) . . ? C124 C123 N42 120.1(6) . . ? C122 C123 N42 118.9(6) . . ? C125 C124 C123 120.0(6) . . ? C124 C125 C120 120.8(6) . . ? N26 C126 C127 122.3(5) . . ? N26 C126 C131 113.9(5) . . ? C127 C126 C131 123.7(5) . . ? C128 C127 C126 119.9(6) . . ? C127 C128 C129 119.3(6) . . ? C128 C129 C130 119.1(6) . . ? N26 C130 C129 121.3(6) . . ? N27 C131 C132 121.9(5) . . ? N27 C131 C126 113.6(5) . . ? C132 C131 C126 124.5(5) . . ? C133 C132 C131 118.5(5) . . ? C134 C133 C132 120.4(5) . . ? C133 C134 C135 117.6(5) . . ? C133 C134 C136 122.7(5) . . ? C135 C134 C136 119.6(5) . . ? N27 C135 C134 123.4(5) . . ? N33 C136 C134 113.9(5) . . ? O29 C137 N33 122.1(6) . . ? O29 C137 N34 123.8(6) . . ? N33 C137 N34 114.1(5) . . ? C139 C138 N34 121.3(5) . . ? C139 C138 C143 118.6(6) . . ? N34 C138 C143 120.1(5) . . ? C140 C139 C138 121.4(7) . . ? C139 C140 C141 118.7(7) . . ? C142 C141 C140 120.2(7) . . ? C143 C142 C141 120.8(7) . . ? C142 C143 C138 120.3(6) . . ? C142 C143 N35 122.6(6) . . ? C138 C143 N35 117.2(5) . . ? O30 C144 N35 126.0(7) . . ? O30 C144 N36 122.0(6) . . ? N35 C144 N36 112.0(6) . . ? C150 C145 C146 118.4(6) . . ? C150 C145 N36 116.9(6) . . ? C146 C145 N36 124.7(6) . . ? C145 C146 C147 119.7(7) . . ? C148 C147 C146 120.6(7) . . ? C147 C148 C149 120.3(7) . . ? C147 C148 N37 120.2(7) . . ? C149 C148 N37 119.5(8) . . ? C148 C149 C150 118.7(7) . . ? C145 C150 C149 122.2(7) . . ? C1S N1S C2S 126.9(9) . . ? C1S N1S C3S 119.3(9) . . ? C2S N1S C3S 113.8(8) . . ? O5S C1S N1S 122.1(10) . . ? C4S N2S C5S 124.6(8) . . ? C4S N2S C6S 123.7(8) . . ? C5S N2S C6S 111.6(7) . . ? C7S N3S C9S 121.7(12) . . ? C7S N3S C8S 111.2(11) . . ? C9S N3S C8S 126.9(11) . . ? C10S N4S C11S 119.1(8) . . ? C10S N4S C12S 124.7(7) . . ? C11S N4S C12S 116.2(7) . . ? N2S C4S O4S 113.6(10) . . ? C13S N5S C15S 121.3(7) . . ? C13S N5S C14S 118.9(7) . . ? C15S N5S C14S 118.9(7) . . ? C16S N6S C17S 116.1(12) . . ? C16S N6S C18S 130.0(13) . . ? C17S N6S C18S 113.8(11) . . ? C19S N7S C21S 116.6(13) . . ? C19S N7S C20S 129.7(12) . . ? C21S N7S C20S 113.4(12) . . ? O6S C7S N3S 125.6(14) . . ? C22S N8S C23S 117.5(11) . . ? C22S N8S C24S 125.8(12) . . ? C23S N8S C24S 116.1(12) . . ? C25S N9S C26S 115.8(10) . . ? C25S N9S C27S 123.3(9) . . ? C26S N9S C27S 120.7(10) . . ? C31S N10S C33S 116.2(8) . . ? C31S N10S C32S 121.7(9) . . ? C33S N10S C32S 122.0(8) . . ? N4S C10S O7S 119.7(8) . . ? C28S N11S C29S 130.3(10) . . ? C28S N11S C30S 118.1(10) . . ? C29S N11S C30S 111.0(8) . . ? O8S C13S N5S 124.8(7) . . ? O9S C16S N6S 109.5(14) . . ? O12S C19S N7S 112.9(14) . . ? O10S C22S N8S 119.7(12) . . ? O11S C25S N9S 125.3(10) . . ? N11S C28S O14S 111.6(12) . . ? O13S C31S N10S 118.9(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.309 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.104 # Attachment '- M1a.cif' data_c:\frames\471\work\471sq _database_code_depnum_ccdc_archive 'CCDC 879405' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common M1a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H107 N21 Ni O12 S' _chemical_formula_weight 1825.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7602(16) _cell_length_b 14.4780(13) _cell_length_c 40.446(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.418(2) _cell_angle_gamma 90.00 _cell_volume 10259.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9269 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 95762 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18056 _reflns_number_gt 11678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Crystal diffracted poorly due to its high content of disordered solvent, with very few reflections observed at 2theta > 45 degrees. Two DMF and one CH3CN solvent molecules could be located from the difference Fourier maps. The remaining electron density inside the crystal's pores, comprising 1640 Ang3 could not be assigned unambiguously, and was therefore treated with the SQUEEZE routine in PLATON. 239 residual electrons/unit cell were thus found, and their contribution was substracted from the hkl file. ; _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^)+(0.1226P)^2^+0.9345P] 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 18056 _refine_ls_number_parameters 1185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1903 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ni1 Ni 0.21319(3) 0.96226(3) 0.412360(12) 0.04013(16) Uani 1 1 d . . . S1 S 0.31223(6) 0.67584(6) 0.56472(2) 0.0381(2) Uani 1 1 d . . . O1 O 0.32500(15) 0.76929(16) 0.57878(6) 0.0442(6) Uani 1 1 d . . . N1 N 0.28398(19) 1.0646(2) 0.39917(8) 0.0419(8) Uani 1 1 d . . . C1 C 0.3044(2) 1.1285(2) 0.42303(9) 0.0367(8) Uani 1 1 d . . . O2 O 0.35629(15) 0.66348(17) 0.53708(6) 0.0437(6) Uani 1 1 d . . . N2 N 0.24239(18) 1.0307(2) 0.45779(8) 0.0379(7) Uani 1 1 d . . . C2 C 0.3433(2) 1.2077(3) 0.41628(10) 0.0478(10) Uani 1 1 d . . . H2 H 0.3566 1.2532 0.4332 0.057 Uiso 1 1 calc R . . O3 O 0.23070(15) 0.66492(19) 0.55130(7) 0.0489(7) Uani 1 1 d . . . N3 N 0.2143(2) 0.9151(2) 0.55069(8) 0.0505(9) Uani 1 1 d . . . H3 H 0.2434 0.8658 0.5547 0.061 Uiso 1 1 calc R . . C3 C 0.3625(3) 1.2199(3) 0.38473(11) 0.0533(11) Uani 1 1 d . . . H3A H 0.3888 1.2740 0.3797 0.064 Uiso 1 1 calc R . . O4 O 0.33493(18) 0.60696(18) 0.59104(7) 0.0548(8) Uani 1 1 d . . . N4 N 0.1128(2) 0.8164(2) 0.54679(9) 0.0502(9) Uani 1 1 d . . . H4 H 0.1487 0.7742 0.5511 0.060 Uiso 1 1 calc R . . C4 C 0.3431(3) 1.1526(3) 0.36061(11) 0.0519(11) Uani 1 1 d . . . H4A H 0.3566 1.1585 0.3389 0.062 Uiso 1 1 calc R . . O5 O 0.53297(16) 0.94464(19) 0.53820(7) 0.0495(7) Uani 1 1 d . . . N5 N 0.0884(2) 0.6481(2) 0.57482(8) 0.0490(8) Uani 1 1 d . . . H5 H 0.1262 0.6355 0.5640 0.059 Uiso 1 1 calc R . . C5 C 0.3036(2) 1.0768(3) 0.36910(10) 0.0479(10) Uani 1 1 d . . . H5A H 0.2896 1.0306 0.3526 0.057 Uiso 1 1 calc R . . O6 O 0.53365(17) 0.76133(18) 0.67845(7) 0.0514(7) Uani 1 1 d . . . N6 N 0.1653(2) 0.5868(2) 0.62016(8) 0.0493(8) Uani 1 1 d . . . H6 H 0.2000 0.5884 0.6069 0.059 Uiso 1 1 calc R . . C6 C 0.2865(2) 1.1071(2) 0.45648(9) 0.0385(9) Uani 1 1 d . . . O7 O 0.18610(18) 0.5504(2) 0.43416(8) 0.0654(9) Uani 1 1 d . . . N7 N 0.20208(19) 0.8843(2) 0.36830(8) 0.0454(8) Uani 1 1 d . . . C7 C 0.3144(2) 1.1551(3) 0.48521(10) 0.0429(9) Uani 1 1 d . . . H7 H 0.3426 1.2104 0.4840 0.051 Uiso 1 1 calc R . . O8 O 0.38523(17) 0.31324(17) 0.52984(7) 0.0502(7) Uani 1 1 d . . . N8 N 0.30264(17) 0.8693(2) 0.42404(7) 0.0373(7) Uani 1 1 d . . . C8 C 0.3013(2) 1.1227(3) 0.51588(10) 0.0439(10) Uani 1 1 d . . . H8 H 0.3208 1.1555 0.5358 0.053 Uiso 1 1 calc R . . O9 O 0.09488(18) 0.9710(2) 0.53461(8) 0.0626(8) Uani 1 1 d . . . N9 N 0.44816(19) 0.8315(2) 0.51818(8) 0.0433(8) Uani 1 1 d . . . H9 H 0.4086 0.7985 0.5217 0.052 Uiso 1 1 calc R . . C9 C 0.2602(2) 1.0431(2) 0.51765(9) 0.0401(9) Uani 1 1 d . . . O10 O 0.04089(19) 0.6208(2) 0.62309(8) 0.0653(9) Uani 1 1 d . . . N10 N 0.45091(19) 0.8877(2) 0.57159(8) 0.0436(8) Uani 1 1 d . . . H10 H 0.4128 0.8489 0.5719 0.052 Uiso 1 1 calc R . . C10 C 0.2302(2) 1.0001(3) 0.48789(9) 0.0401(9) Uani 1 1 d . . . H10A H 0.1997 0.9466 0.4887 0.048 Uiso 1 1 calc R . . N11 N 0.4442(2) 0.8091(2) 0.63413(8) 0.0491(9) Uani 1 1 d . . . H11 H 0.4026 0.7928 0.6204 0.059 Uiso 1 1 calc R . . C11 C 0.2484(3) 1.0048(3) 0.55159(10) 0.0509(10) Uani 1 1 d . . . H11A H 0.2986 1.0022 0.5664 0.061 Uiso 1 1 calc R . . H11B H 0.2159 1.0484 0.5618 0.061 Uiso 1 1 calc R . . N12 N 0.44660(19) 0.6591(2) 0.65131(8) 0.0474(8) Uani 1 1 d . . . H12 H 0.4064 0.6534 0.6355 0.057 Uiso 1 1 calc R . . C12 C 0.1372(3) 0.9055(3) 0.54374(10) 0.0488(10) Uani 1 1 d . . . N13 N 0.1152(2) 1.0417(2) 0.39762(8) 0.0474(8) Uani 1 1 d . . . C13 C 0.0370(3) 0.7847(3) 0.54382(10) 0.0503(11) Uani 1 1 d . . . N14 N 0.12994(18) 0.8800(2) 0.42844(7) 0.0396(7) Uani 1 1 d . . . C14 C -0.0255(3) 0.8334(3) 0.52760(11) 0.0577(12) Uani 1 1 d . . . H14 H -0.0182 0.8910 0.5174 0.069 Uiso 1 1 calc R . . N15 N 0.17569(19) 0.6315(2) 0.48121(8) 0.0477(8) Uani 1 1 d . . . H15 H 0.1993 0.6516 0.5007 0.057 Uiso 1 1 calc R . . C15 C -0.0982(3) 0.7988(4) 0.52620(12) 0.0643(13) Uani 1 1 d . . . H15A H -0.1408 0.8339 0.5158 0.077 Uiso 1 1 calc R . . N16 N 0.28899(19) 0.5660(2) 0.47625(8) 0.0481(8) Uani 1 1 d . . . H16 H 0.3046 0.5947 0.4953 0.058 Uiso 1 1 calc R . . C16 C -0.1097(3) 0.7130(4) 0.53981(13) 0.0691(14) Uani 1 1 d . . . H16A H -0.1599 0.6887 0.5384 0.083 Uiso 1 1 calc R . . N17 N 0.39169(19) 0.4680(2) 0.52130(8) 0.0430(8) Uani 1 1 d . . . H17 H 0.3940 0.5230 0.5307 0.052 Uiso 1 1 calc R . . C17 C -0.0485(3) 0.6636(3) 0.55528(11) 0.0596(12) Uani 1 1 d . . . H17A H -0.0564 0.6047 0.5645 0.071 Uiso 1 1 calc R . . N18 N 0.3753(2) 0.4124(2) 0.57274(8) 0.0464(8) Uani 1 1 d . . . H18 H 0.3846 0.4692 0.5800 0.056 Uiso 1 1 calc R . . C18 C 0.0247(2) 0.6977(3) 0.55775(10) 0.0472(10) Uani 1 1 d . . . C19 C 0.0940(3) 0.6186(3) 0.60766(11) 0.0483(10) Uani 1 1 d . . . C20 C 0.1875(2) 0.5515(3) 0.65280(10) 0.0460(10) Uani 1 1 d . . . C21 C 0.1410(3) 0.5065(4) 0.67067(12) 0.0648(13) Uani 1 1 d . . . H21 H 0.0891 0.4970 0.6611 0.078 Uiso 1 1 calc R . . C22 C 0.1672(3) 0.4739(3) 0.70268(11) 0.0624(13) Uani 1 1 d . . . H22 H 0.1324 0.4438 0.7146 0.075 Uiso 1 1 calc R . . C23 C 0.2418(3) 0.4838(3) 0.71760(11) 0.0501(10) Uani 1 1 d . . . C24 C 0.2900(3) 0.5265(3) 0.69885(11) 0.0586(12) Uani 1 1 d . . . H24 H 0.3425 0.5330 0.7080 0.070 Uiso 1 1 calc R . . C25 C 0.2642(3) 0.5599(3) 0.66735(12) 0.0575(12) Uani 1 1 d . . . H25 H 0.2989 0.5893 0.6552 0.069 Uiso 1 1 calc R . . C26 C 0.2725(3) 0.4509(3) 0.75353(10) 0.0563(11) Uani 1 1 d . . . C27 C 0.3400(3) 0.3862(4) 0.75409(13) 0.0771(15) Uani 1 1 d . . . H27A H 0.3241 0.3319 0.7402 0.116 Uiso 1 1 calc R . . H27B H 0.3585 0.3666 0.7772 0.116 Uiso 1 1 calc R . . H27C H 0.3810 0.4183 0.7452 0.116 Uiso 1 1 calc R . . C28 C 0.2107(3) 0.4016(4) 0.76946(13) 0.0800(16) Uani 1 1 d . . . H28A H 0.1700 0.4454 0.7720 0.120 Uiso 1 1 calc R . . H28B H 0.2333 0.3775 0.7915 0.120 Uiso 1 1 calc R . . H28C H 0.1895 0.3504 0.7550 0.120 Uiso 1 1 calc R . . C29 C 0.2988(4) 0.5364(4) 0.77547(13) 0.0833(17) Uani 1 1 d . . . H29A H 0.3401 0.5678 0.7665 0.125 Uiso 1 1 calc R . . H29B H 0.3173 0.5165 0.7985 0.125 Uiso 1 1 calc R . . H29C H 0.2558 0.5789 0.7752 0.125 Uiso 1 1 calc R . . C30 C 0.2461(2) 0.8072(3) 0.37088(10) 0.0444(10) Uani 1 1 d . . . C31 C 0.2361(3) 0.7402(3) 0.34601(11) 0.0559(11) Uani 1 1 d . . . H31 H 0.2657 0.6852 0.3484 0.067 Uiso 1 1 calc R . . C32 C 0.1817(3) 0.7553(4) 0.31746(12) 0.0664(13) Uani 1 1 d . . . H32 H 0.1740 0.7104 0.3001 0.080 Uiso 1 1 calc R . . C33 C 0.1392(3) 0.8350(4) 0.31449(12) 0.0671(13) Uani 1 1 d . . . H33 H 0.1034 0.8473 0.2949 0.081 Uiso 1 1 calc R . . C34 C 0.1500(2) 0.8965(3) 0.34075(10) 0.0511(10) Uani 1 1 d . . . H34 H 0.1191 0.9504 0.3393 0.061 Uiso 1 1 calc R . . C35 C 0.3046(2) 0.8003(3) 0.40106(9) 0.0402(9) Uani 1 1 d . . . C36 C 0.3608(2) 0.7329(3) 0.40623(10) 0.0447(10) Uani 1 1 d . . . H36 H 0.3615 0.6845 0.3904 0.054 Uiso 1 1 calc R . . C37 C 0.4154(2) 0.7369(3) 0.43455(10) 0.0457(10) Uani 1 1 d . . . H37 H 0.4532 0.6899 0.4386 0.055 Uiso 1 1 calc R . . C38 C 0.4160(2) 0.8083(3) 0.45720(9) 0.0396(9) Uani 1 1 d . . . C39 C 0.3577(2) 0.8724(3) 0.45065(9) 0.0396(9) Uani 1 1 d . . . H39 H 0.3569 0.9217 0.4661 0.047 Uiso 1 1 calc R . . C40 C 0.4776(2) 0.8218(3) 0.48714(10) 0.0430(9) Uani 1 1 d . . . H40A H 0.5127 0.7682 0.4890 0.052 Uiso 1 1 calc R . . H40B H 0.5074 0.8776 0.4836 0.052 Uiso 1 1 calc R . . C41 C 0.4821(2) 0.8926(3) 0.54240(9) 0.0415(9) Uani 1 1 d . . . C42 C 0.4753(2) 0.9395(3) 0.60065(10) 0.0415(9) Uani 1 1 d . . . C43 C 0.5027(3) 1.0296(3) 0.59897(11) 0.0509(10) Uani 1 1 d . . . H43 H 0.5044 1.0573 0.5778 0.061 Uiso 1 1 calc R . . C44 C 0.5274(3) 1.0785(3) 0.62817(11) 0.0549(11) Uani 1 1 d . . . H44 H 0.5473 1.1390 0.6268 0.066 Uiso 1 1 calc R . . C45 C 0.5235(3) 1.0408(3) 0.65908(11) 0.0563(11) Uani 1 1 d . . . H45 H 0.5402 1.0751 0.6790 0.068 Uiso 1 1 calc R . . C46 C 0.4952(3) 0.9527(3) 0.66076(10) 0.0511(11) Uani 1 1 d . . . H46 H 0.4914 0.9269 0.6820 0.061 Uiso 1 1 calc R . . C47 C 0.4722(2) 0.9009(3) 0.63204(9) 0.0422(9) Uani 1 1 d . . . C48 C 0.4794(2) 0.7450(3) 0.65661(10) 0.0423(9) Uani 1 1 d . . . C49 C 0.4738(2) 0.5788(3) 0.66981(10) 0.0454(10) Uani 1 1 d . . . C50 C 0.5010(2) 0.5793(3) 0.70332(10) 0.0465(10) Uani 1 1 d . . . H50 H 0.5027 0.6354 0.7156 0.056 Uiso 1 1 calc R . . C51 C 0.5263(3) 0.4975(3) 0.71956(10) 0.0515(11) Uani 1 1 d . . . H51 H 0.5452 0.4993 0.7429 0.062 Uiso 1 1 calc R . . C52 C 0.5249(3) 0.4143(3) 0.70315(10) 0.0498(10) Uani 1 1 d . . . C53 C 0.4946(3) 0.4157(3) 0.66912(11) 0.0566(11) Uani 1 1 d . . . H53 H 0.4908 0.3594 0.6569 0.068 Uiso 1 1 calc R . . C54 C 0.4700(3) 0.4960(3) 0.65255(11) 0.0564(11) Uani 1 1 d . . . H54 H 0.4505 0.4945 0.6293 0.068 Uiso 1 1 calc R . . C55 C 0.5551(3) 0.3225(3) 0.71941(12) 0.0619(13) Uani 1 1 d . . . C56 C 0.4909(4) 0.2495(3) 0.71449(15) 0.0820(16) Uani 1 1 d . . . H56A H 0.4725 0.2409 0.6905 0.123 Uiso 1 1 calc R . . H56B H 0.4487 0.2704 0.7255 0.123 Uiso 1 1 calc R . . H56C H 0.5107 0.1908 0.7244 0.123 Uiso 1 1 calc R . . C57 C 0.5799(4) 0.3330(4) 0.75694(14) 0.094(2) Uani 1 1 d . . . H57A H 0.5987 0.2736 0.7666 0.141 Uiso 1 1 calc R . . H57B H 0.5364 0.3531 0.7672 0.141 Uiso 1 1 calc R . . H57C H 0.6208 0.3791 0.7613 0.141 Uiso 1 1 calc R . . C58 C 0.6194(4) 0.2891(4) 0.70270(16) 0.0914(19) Uani 1 1 d . . . H58A H 0.6369 0.2288 0.7119 0.137 Uiso 1 1 calc R . . H58B H 0.6616 0.3334 0.7067 0.137 Uiso 1 1 calc R . . H58C H 0.6017 0.2834 0.6785 0.137 Uiso 1 1 calc R . . C59 C 0.0502(2) 1.0061(3) 0.40549(10) 0.0449(10) Uani 1 1 d . . . C60 C -0.0184(3) 1.0487(3) 0.39624(11) 0.0575(12) Uani 1 1 d . . . H60 H -0.0636 1.0210 0.4014 0.069 Uiso 1 1 calc R . . C61 C -0.0225(3) 1.1323(3) 0.37931(12) 0.0638(13) Uani 1 1 d . . . H61 H -0.0701 1.1624 0.3727 0.077 Uiso 1 1 calc R . . C62 C 0.0425(3) 1.1698(3) 0.37253(12) 0.0625(13) Uani 1 1 d . . . H62 H 0.0417 1.2282 0.3618 0.075 Uiso 1 1 calc R . . C63 C 0.1105(3) 1.1226(3) 0.38131(12) 0.0606(12) Uani 1 1 d . . . H63 H 0.1557 1.1487 0.3756 0.073 Uiso 1 1 calc R . . C64 C 0.0598(2) 0.9169(3) 0.42397(10) 0.0418(9) Uani 1 1 d . . . C65 C -0.0002(2) 0.8737(3) 0.43565(11) 0.0530(11) Uani 1 1 d . . . H65 H -0.0492 0.9015 0.4329 0.064 Uiso 1 1 calc R . . C66 C 0.0129(2) 0.7887(3) 0.45157(11) 0.0510(10) Uani 1 1 d . . . H66 H -0.0274 0.7583 0.4600 0.061 Uiso 1 1 calc R . . C67 C 0.0830(2) 0.7490(3) 0.45512(10) 0.0421(9) Uani 1 1 d . . . C68 C 0.1409(2) 0.7982(3) 0.44358(9) 0.0411(9) Uani 1 1 d . . . H68 H 0.1907 0.7721 0.4467 0.049 Uiso 1 1 calc R . . C69 C 0.0964(2) 0.6540(3) 0.47057(11) 0.0515(11) Uani 1 1 d . . . H69A H 0.0697 0.6500 0.4902 0.062 Uiso 1 1 calc R . . H69B H 0.0735 0.6074 0.4540 0.062 Uiso 1 1 calc R . . C70 C 0.2148(2) 0.5795(3) 0.46162(11) 0.0477(10) Uani 1 1 d . . . C71 C 0.3429(2) 0.5101(3) 0.46347(10) 0.0407(9) Uani 1 1 d . . . C72 C 0.3461(2) 0.5050(3) 0.42962(10) 0.0465(10) Uani 1 1 d . . . H72 H 0.3096 0.5372 0.4140 0.056 Uiso 1 1 calc R . . C73 C 0.4025(2) 0.4528(3) 0.41839(10) 0.0475(10) Uani 1 1 d . . . H73 H 0.4044 0.4491 0.3951 0.057 Uiso 1 1 calc R . . C74 C 0.4560(2) 0.4062(3) 0.44115(11) 0.0489(10) Uani 1 1 d . . . H74 H 0.4950 0.3711 0.4335 0.059 Uiso 1 1 calc R . . C75 C 0.4524(2) 0.4110(3) 0.47496(11) 0.0460(10) Uani 1 1 d . . . H75 H 0.4891 0.3787 0.4905 0.055 Uiso 1 1 calc R . . C76 C 0.3959(2) 0.4622(2) 0.48674(10) 0.0393(9) Uani 1 1 d . . . C77 C 0.3842(2) 0.3922(3) 0.54086(10) 0.0397(9) Uani 1 1 d . . . C78 C 0.3514(2) 0.3464(3) 0.59519(10) 0.0465(10) Uani 1 1 d . . . C79 C 0.3021(3) 0.3755(3) 0.61628(12) 0.0674(14) Uani 1 1 d . . . H79 H 0.2867 0.4384 0.6157 0.081 Uiso 1 1 calc R . . C80 C 0.2748(3) 0.3156(3) 0.63810(13) 0.0730(15) Uani 1 1 d . . . H80 H 0.2420 0.3383 0.6526 0.088 Uiso 1 1 calc R . . C81 C 0.2946(3) 0.2223(3) 0.63916(12) 0.0606(12) Uani 1 1 d . . . C82 C 0.3476(3) 0.1958(3) 0.61945(11) 0.0540(11) Uani 1 1 d . . . H82 H 0.3650 0.1336 0.6208 0.065 Uiso 1 1 calc R . . C83 C 0.3767(2) 0.2558(3) 0.59772(10) 0.0482(10) Uani 1 1 d . . . H83 H 0.4135 0.2348 0.5848 0.058 Uiso 1 1 calc R . . C84 C 0.2595(3) 0.1528(3) 0.66057(13) 0.0704(14) Uani 1 1 d . . . C85 C 0.2074(6) 0.0910(6) 0.63855(17) 0.153(4) Uani 1 1 d . . . H85A H 0.1661 0.1274 0.6258 0.230 Uiso 1 1 calc R . . H85B H 0.1858 0.0452 0.6522 0.230 Uiso 1 1 calc R . . H85C H 0.2357 0.0592 0.6230 0.230 Uiso 1 1 calc R . . C86 C 0.3224(5) 0.0978(6) 0.6826(2) 0.152(4) Uani 1 1 d . . . H86A H 0.3000 0.0616 0.6990 0.228 Uiso 1 1 calc R . . H86B H 0.3605 0.1405 0.6943 0.228 Uiso 1 1 calc R . . H86C H 0.3469 0.0561 0.6685 0.228 Uiso 1 1 calc R . . C87 C 0.2164(5) 0.1994(5) 0.68501(18) 0.130(3) Uani 1 1 d . . . H87A H 0.1848 0.2491 0.6736 0.195 Uiso 1 1 calc R . . H87B H 0.2527 0.2253 0.7036 0.195 Uiso 1 1 calc R . . H87C H 0.1837 0.1541 0.6938 0.195 Uiso 1 1 calc R . . O1S O 0.1752(6) 0.2101(7) 0.5653(2) 0.213(3) Uani 1 1 d . . . N1S N 0.1515(6) 0.3712(8) 0.5543(2) 0.179(4) Uani 1 1 d . . . C1S C 0.1717(5) 1.3918(6) 0.3799(2) 0.147(3) Uani 1 1 d . . . H1S1 H 0.1378 1.4449 0.3744 0.221 Uiso 1 1 calc R . . H1S2 H 0.2238 1.4137 0.3877 0.221 Uiso 1 1 calc R . . H1S3 H 0.1543 1.3555 0.3977 0.221 Uiso 1 1 calc R . . O2S O 0.2976(3) 0.5322(3) 0.34290(12) 0.1082(15) Uani 1 1 d . . . N2S N 0.2807(3) 0.4420(4) 0.29783(16) 0.1003(16) Uani 1 1 d . . . C2S C 0.1707(4) 1.3383(5) 0.35233(18) 0.095(2) Uani 1 1 d . . . N3S N 0.1696(5) 1.2914(5) 0.32991(19) 0.139(3) Uani 1 1 d . . . C3S C 0.3129(4) 0.4692(4) 0.32630(17) 0.0775(15) Uani 1 1 d . . . H3S H 0.3561 0.4339 0.3360 0.093 Uiso 1 1 calc R . . C4S C 0.3027(4) 0.3618(5) 0.28368(18) 0.103(2) Uani 1 1 d . . . H4S1 H 0.3496 0.3383 0.2972 0.154 Uiso 1 1 calc R . . H4S2 H 0.3120 0.3747 0.2609 0.154 Uiso 1 1 calc R . . H4S3 H 0.2622 0.3155 0.2828 0.154 Uiso 1 1 calc R . . C5S C 0.2122(6) 0.4915(7) 0.2805(3) 0.170(4) Uani 1 1 d . . . H5S1 H 0.1923 0.5322 0.2964 0.255 Uiso 1 1 calc R . . H5S2 H 0.1729 0.4465 0.2715 0.255 Uiso 1 1 calc R . . H5S3 H 0.2261 0.5284 0.2621 0.255 Uiso 1 1 calc R . . C6S C 0.1876(6) 0.2814(7) 0.5497(4) 0.182(5) Uani 1 1 d . . . H6S H 0.2220 0.2776 0.5341 0.218 Uiso 1 1 calc R . . C7S C 0.1722(6) 0.4369(5) 0.53439(19) 0.128(3) Uani 1 1 d . . . H7S1 H 0.2018 0.4092 0.5185 0.191 Uiso 1 1 calc R . . H7S2 H 0.2035 0.4830 0.5480 0.191 Uiso 1 1 calc R . . H7S3 H 0.1265 0.4666 0.5221 0.191 Uiso 1 1 calc R . . C8S C 0.0973(6) 0.3888(7) 0.5784(3) 0.164(4) Uani 1 1 d . . . H8S1 H 0.1227 0.4265 0.5971 0.246 Uiso 1 1 calc R . . H8S2 H 0.0816 0.3299 0.5870 0.246 Uiso 1 1 calc R . . H8S3 H 0.0523 0.4217 0.5669 0.246 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 Ni1 0.0449(3) 0.0322(3) 0.0422(3) -0.0020(2) 0.0040(2) -0.0010(2) S1 0.0451(6) 0.0293(5) 0.0401(5) 0.0003(4) 0.0074(4) 0.0005(4) O1 0.0538(17) 0.0291(13) 0.0486(15) -0.0046(11) 0.0051(13) 0.0033(12) N1 0.049(2) 0.0345(17) 0.0418(19) -0.0007(14) 0.0071(15) 0.0014(15) C1 0.039(2) 0.0305(19) 0.039(2) 0.0012(16) 0.0027(17) 0.0041(16) O2 0.0472(16) 0.0370(14) 0.0494(16) -0.0011(12) 0.0151(13) -0.0005(12) N2 0.0427(18) 0.0290(16) 0.0424(18) -0.0003(13) 0.0082(14) 0.0017(14) C2 0.061(3) 0.036(2) 0.047(2) -0.0035(17) 0.010(2) -0.0040(19) O3 0.0439(16) 0.0496(17) 0.0548(17) -0.0074(13) 0.0126(13) -0.0048(13) N3 0.066(3) 0.0340(18) 0.053(2) 0.0054(15) 0.0123(18) 0.0082(17) C3 0.064(3) 0.045(2) 0.053(3) 0.004(2) 0.013(2) -0.006(2) O4 0.085(2) 0.0333(15) 0.0425(15) 0.0058(12) 0.0004(15) 0.0016(14) N4 0.052(2) 0.0361(19) 0.063(2) 0.0084(16) 0.0105(18) 0.0127(16) C4 0.062(3) 0.050(3) 0.045(2) 0.0034(19) 0.013(2) -0.008(2) O5 0.0524(17) 0.0444(16) 0.0523(17) 0.0053(13) 0.0108(14) -0.0082(14) N5 0.056(2) 0.050(2) 0.0441(19) 0.0078(15) 0.0166(16) 0.0139(17) C5 0.059(3) 0.044(2) 0.041(2) -0.0005(18) 0.011(2) -0.007(2) O6 0.0597(19) 0.0429(16) 0.0479(16) 0.0075(13) -0.0025(15) -0.0074(14) N6 0.049(2) 0.053(2) 0.048(2) 0.0113(16) 0.0133(16) 0.0068(17) C6 0.037(2) 0.032(2) 0.045(2) -0.0037(16) 0.0049(17) 0.0036(16) O7 0.0561(19) 0.081(2) 0.0549(19) -0.0244(17) -0.0026(15) 0.0066(17) N7 0.048(2) 0.0419(19) 0.0455(19) -0.0036(15) 0.0069(16) -0.0055(16) C7 0.043(2) 0.035(2) 0.050(2) -0.0085(17) 0.0056(19) -0.0004(17) O8 0.0689(19) 0.0293(15) 0.0559(17) -0.0067(12) 0.0202(15) -0.0008(13) N8 0.0422(18) 0.0321(16) 0.0383(17) -0.0051(13) 0.0089(15) -0.0046(14) C8 0.046(2) 0.039(2) 0.045(2) -0.0114(17) 0.0021(19) 0.0031(18) O9 0.070(2) 0.0403(17) 0.081(2) 0.0132(15) 0.0225(17) 0.0235(15) N9 0.051(2) 0.0388(18) 0.0408(18) 0.0016(14) 0.0103(16) -0.0046(15) C9 0.049(2) 0.034(2) 0.038(2) -0.0027(16) 0.0080(17) 0.0080(18) O10 0.062(2) 0.075(2) 0.065(2) 0.0225(16) 0.0296(17) 0.0216(17) N10 0.049(2) 0.0438(19) 0.0391(18) 0.0029(14) 0.0102(15) -0.0065(15) C10 0.047(2) 0.0289(19) 0.046(2) -0.0008(17) 0.0131(18) 0.0062(17) N11 0.066(2) 0.0370(18) 0.0409(18) 0.0057(14) 0.0004(17) -0.0067(16) C11 0.067(3) 0.042(2) 0.044(2) -0.0023(18) 0.009(2) 0.006(2) N12 0.053(2) 0.0374(19) 0.050(2) 0.0068(15) 0.0004(16) -0.0062(16) C12 0.061(3) 0.045(2) 0.044(2) 0.0060(18) 0.019(2) 0.012(2) N13 0.054(2) 0.0346(18) 0.051(2) -0.0024(15) 0.0000(17) 0.0001(16) C13 0.059(3) 0.050(3) 0.043(2) -0.0039(19) 0.011(2) 0.014(2) N14 0.0438(19) 0.0341(17) 0.0401(17) -0.0060(14) 0.0047(14) 0.0003(14) C14 0.065(3) 0.050(3) 0.059(3) 0.001(2) 0.012(2) 0.021(2) N15 0.050(2) 0.0397(19) 0.052(2) -0.0049(15) 0.0049(17) 0.0032(16) C15 0.049(3) 0.077(4) 0.066(3) 0.002(3) 0.006(2) 0.023(3) N16 0.051(2) 0.047(2) 0.0440(19) -0.0078(15) 0.0016(16) 0.0115(16) C16 0.044(3) 0.081(4) 0.082(3) 0.000(3) 0.008(2) 0.010(3) N17 0.059(2) 0.0270(16) 0.0424(18) -0.0019(13) 0.0071(16) -0.0037(15) C17 0.059(3) 0.062(3) 0.061(3) 0.003(2) 0.021(2) 0.003(2) N18 0.065(2) 0.0306(17) 0.0446(19) -0.0040(14) 0.0110(17) -0.0043(16) C18 0.057(3) 0.044(2) 0.042(2) 0.0042(18) 0.012(2) 0.013(2) C19 0.054(3) 0.039(2) 0.054(3) 0.0040(19) 0.015(2) 0.0038(19) C20 0.052(3) 0.039(2) 0.048(2) 0.0051(18) 0.009(2) -0.0008(19) C21 0.047(3) 0.078(3) 0.066(3) 0.023(3) -0.001(2) -0.014(2) C22 0.060(3) 0.073(3) 0.054(3) 0.018(2) 0.010(2) -0.012(2) C23 0.058(3) 0.044(2) 0.050(2) -0.0018(19) 0.015(2) -0.001(2) C24 0.050(3) 0.081(3) 0.046(3) 0.004(2) 0.012(2) 0.000(2) C25 0.049(3) 0.062(3) 0.064(3) 0.010(2) 0.019(2) 0.004(2) C26 0.062(3) 0.061(3) 0.043(2) 0.002(2) 0.003(2) -0.003(2) C27 0.079(4) 0.079(4) 0.070(3) 0.010(3) 0.000(3) 0.013(3) C28 0.084(4) 0.099(4) 0.056(3) 0.025(3) 0.010(3) -0.017(3) C29 0.107(5) 0.081(4) 0.060(3) -0.009(3) 0.007(3) -0.016(3) C30 0.050(2) 0.041(2) 0.044(2) -0.0050(17) 0.0120(19) -0.0099(19) C31 0.063(3) 0.048(3) 0.056(3) -0.015(2) 0.011(2) -0.006(2) C32 0.072(3) 0.069(3) 0.057(3) -0.025(2) 0.008(3) -0.019(3) C33 0.066(3) 0.077(4) 0.054(3) -0.010(2) -0.001(2) -0.004(3) C34 0.054(3) 0.055(3) 0.042(2) -0.0046(19) 0.001(2) -0.004(2) C35 0.050(2) 0.033(2) 0.041(2) -0.0006(16) 0.0159(18) -0.0089(18) C36 0.061(3) 0.030(2) 0.046(2) -0.0041(16) 0.019(2) 0.0022(18) C37 0.059(3) 0.031(2) 0.049(2) 0.0026(17) 0.015(2) 0.0040(18) C38 0.045(2) 0.034(2) 0.042(2) 0.0036(16) 0.0126(18) 0.0016(17) C39 0.046(2) 0.032(2) 0.041(2) -0.0013(16) 0.0096(18) -0.0010(17) C40 0.045(2) 0.037(2) 0.048(2) 0.0019(17) 0.0096(19) 0.0053(17) C41 0.043(2) 0.038(2) 0.042(2) 0.0103(17) 0.0001(18) 0.0038(19) C42 0.042(2) 0.037(2) 0.047(2) 0.0005(17) 0.0114(18) 0.0022(17) C43 0.060(3) 0.038(2) 0.057(3) 0.0054(19) 0.014(2) -0.001(2) C44 0.062(3) 0.035(2) 0.068(3) 0.000(2) 0.011(2) -0.005(2) C45 0.071(3) 0.040(2) 0.057(3) -0.006(2) 0.008(2) -0.003(2) C46 0.068(3) 0.040(2) 0.044(2) 0.0008(18) 0.007(2) -0.006(2) C47 0.054(2) 0.031(2) 0.043(2) 0.0051(16) 0.0130(19) -0.0029(18) C48 0.055(3) 0.032(2) 0.041(2) 0.0069(17) 0.013(2) 0.0000(18) C49 0.053(3) 0.035(2) 0.050(2) 0.0053(18) 0.013(2) -0.0025(18) C50 0.063(3) 0.038(2) 0.042(2) -0.0014(17) 0.017(2) -0.0008(19) C51 0.074(3) 0.040(2) 0.041(2) 0.0005(18) 0.011(2) 0.002(2) C52 0.069(3) 0.035(2) 0.049(2) 0.0061(18) 0.020(2) 0.003(2) C53 0.076(3) 0.036(2) 0.059(3) -0.005(2) 0.017(2) 0.001(2) C54 0.070(3) 0.047(3) 0.050(3) -0.002(2) 0.002(2) -0.002(2) C55 0.081(3) 0.041(2) 0.069(3) 0.012(2) 0.027(3) 0.012(2) C56 0.113(5) 0.039(3) 0.099(4) 0.008(3) 0.034(4) 0.000(3) C57 0.154(6) 0.051(3) 0.074(4) 0.024(3) 0.012(4) 0.027(3) C58 0.119(5) 0.060(3) 0.107(4) 0.030(3) 0.053(4) 0.034(3) C59 0.055(3) 0.034(2) 0.043(2) -0.0060(17) 0.0034(19) 0.0068(19) C60 0.055(3) 0.057(3) 0.059(3) 0.000(2) 0.004(2) 0.015(2) C61 0.067(3) 0.055(3) 0.064(3) 0.000(2) -0.003(3) 0.019(3) C62 0.072(3) 0.042(3) 0.070(3) 0.008(2) 0.002(3) 0.008(2) C63 0.065(3) 0.045(3) 0.068(3) 0.005(2) -0.001(2) 0.003(2) C64 0.042(2) 0.038(2) 0.045(2) -0.0088(17) 0.0035(18) 0.0025(18) C65 0.043(2) 0.046(3) 0.070(3) -0.004(2) 0.011(2) 0.008(2) C66 0.045(3) 0.044(2) 0.068(3) -0.002(2) 0.019(2) -0.0019(19) C67 0.040(2) 0.038(2) 0.048(2) -0.0057(17) 0.0073(18) 0.0001(18) C68 0.039(2) 0.037(2) 0.046(2) -0.0072(17) 0.0057(18) 0.0048(17) C69 0.052(3) 0.037(2) 0.066(3) 0.0007(19) 0.013(2) -0.0013(19) C70 0.055(3) 0.035(2) 0.053(3) -0.0027(19) 0.009(2) 0.0023(19) C71 0.042(2) 0.034(2) 0.046(2) -0.0049(17) 0.0073(18) -0.0013(17) C72 0.053(3) 0.037(2) 0.048(2) 0.0004(18) 0.006(2) -0.0045(19) C73 0.057(3) 0.043(2) 0.046(2) -0.0048(18) 0.018(2) -0.008(2) C74 0.052(3) 0.042(2) 0.055(3) -0.0065(19) 0.013(2) -0.003(2) C75 0.045(2) 0.034(2) 0.058(3) -0.0022(18) 0.006(2) -0.0017(18) C76 0.043(2) 0.0272(19) 0.047(2) -0.0033(16) 0.0072(18) -0.0048(17) C77 0.035(2) 0.036(2) 0.048(2) -0.0048(17) 0.0078(17) -0.0042(16) C78 0.056(3) 0.036(2) 0.047(2) -0.0007(18) 0.010(2) -0.0052(19) C79 0.095(4) 0.045(3) 0.070(3) -0.002(2) 0.037(3) 0.015(3) C80 0.096(4) 0.055(3) 0.079(3) 0.005(2) 0.047(3) 0.012(3) C81 0.075(3) 0.051(3) 0.061(3) 0.000(2) 0.028(3) -0.004(2) C82 0.070(3) 0.035(2) 0.057(3) 0.0006(19) 0.010(2) -0.002(2) C83 0.055(3) 0.039(2) 0.051(2) -0.0023(18) 0.010(2) 0.0026(19) C84 0.093(4) 0.058(3) 0.066(3) 0.000(2) 0.029(3) -0.013(3) C85 0.235(10) 0.149(7) 0.082(5) -0.009(5) 0.042(5) -0.124(7) C86 0.135(7) 0.138(7) 0.198(9) 0.111(7) 0.072(6) 0.024(6) C87 0.215(9) 0.096(5) 0.104(5) 0.003(4) 0.102(6) -0.017(5) O1S 0.235(9) 0.176(8) 0.227(9) -0.012(7) 0.038(7) -0.015(7) N1S 0.207(10) 0.191(10) 0.128(6) 0.004(6) -0.001(6) -0.104(8) C1S 0.164(8) 0.149(8) 0.145(7) -0.061(6) 0.075(6) -0.058(6) O2S 0.143(4) 0.080(3) 0.111(3) 0.010(3) 0.048(3) 0.011(3) N2S 0.112(5) 0.085(4) 0.100(4) 0.020(3) 0.007(4) -0.004(3) C2S 0.124(6) 0.078(4) 0.093(5) -0.013(4) 0.047(4) -0.026(4) N3S 0.192(7) 0.106(5) 0.140(6) -0.011(4) 0.085(5) -0.038(5) C3S 0.087(4) 0.072(4) 0.077(4) 0.021(3) 0.024(3) 0.006(3) C4S 0.118(5) 0.081(4) 0.110(5) -0.011(4) 0.020(4) -0.003(4) C5S 0.156(9) 0.148(8) 0.187(10) 0.008(7) -0.026(7) 0.040(7) C6S 0.154(9) 0.077(6) 0.323(17) 0.033(8) 0.065(9) -0.005(6) C7S 0.204(9) 0.068(4) 0.108(5) 0.007(4) 0.016(6) -0.031(5) C8S 0.180(9) 0.145(8) 0.166(9) -0.076(7) 0.026(8) -0.085(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.068(3) . ? Ni1 N8 2.077(3) . ? Ni1 N2 2.077(3) . ? Ni1 N14 2.084(3) . ? Ni1 N13 2.089(3) . ? Ni1 N7 2.091(3) . ? S1 O4 1.466(3) . ? S1 O3 1.469(3) . ? S1 O1 1.471(3) . ? S1 O2 1.477(3) . ? N1 C5 1.331(5) . ? N1 C1 1.344(5) . ? C1 C2 1.388(5) . ? C1 C6 1.473(5) . ? N2 C10 1.345(5) . ? N2 C6 1.361(5) . ? C2 C3 1.386(6) . ? N3 C12 1.359(6) . ? N3 C11 1.431(5) . ? C3 C4 1.381(6) . ? N4 C12 1.373(5) . ? N4 C13 1.410(6) . ? C4 C5 1.376(6) . ? O5 C41 1.210(5) . ? N5 C19 1.383(5) . ? N5 C18 1.420(5) . ? O6 C48 1.219(5) . ? N6 C19 1.365(5) . ? N6 C20 1.411(5) . ? C6 C7 1.375(5) . ? O7 C70 1.220(5) . ? N7 C34 1.338(5) . ? N7 C30 1.356(5) . ? C7 C8 1.381(6) . ? O8 C77 1.228(4) . ? N8 C39 1.331(5) . ? N8 C35 1.368(5) . ? C8 C9 1.371(5) . ? O9 C12 1.228(5) . ? N9 C41 1.382(5) . ? N9 C40 1.444(5) . ? C9 C10 1.382(5) . ? C9 C11 1.527(5) . ? O10 C19 1.214(5) . ? N10 C41 1.385(5) . ? N10 C42 1.402(5) . ? N11 C48 1.376(5) . ? N11 C47 1.426(5) . ? N12 C48 1.376(5) . ? N12 C49 1.424(5) . ? N13 C63 1.341(5) . ? N13 C59 1.350(5) . ? C13 C14 1.386(6) . ? C13 C18 1.411(6) . ? N14 C68 1.333(5) . ? N14 C64 1.341(5) . ? C14 C15 1.377(7) . ? N15 C70 1.362(5) . ? N15 C69 1.441(5) . ? C15 C16 1.387(7) . ? N16 C70 1.367(5) . ? N16 C71 1.414(5) . ? C16 C17 1.365(7) . ? N17 C77 1.373(5) . ? N17 C76 1.414(5) . ? C17 C18 1.378(6) . ? N18 C77 1.357(5) . ? N18 C78 1.429(5) . ? C20 C21 1.351(6) . ? C20 C25 1.397(6) . ? C21 C22 1.385(6) . ? C22 C23 1.371(6) . ? C23 C24 1.379(6) . ? C23 C26 1.541(6) . ? C24 C25 1.370(6) . ? C26 C27 1.520(7) . ? C26 C28 1.536(7) . ? C26 C29 1.549(7) . ? C30 C31 1.388(5) . ? C30 C35 1.471(6) . ? C31 C32 1.397(7) . ? C32 C33 1.373(7) . ? C33 C34 1.376(6) . ? C35 C36 1.388(5) . ? C36 C37 1.376(6) . ? C37 C38 1.380(5) . ? C38 C39 1.384(5) . ? C38 C40 1.505(5) . ? C42 C47 1.397(5) . ? C42 C43 1.398(5) . ? C43 C44 1.385(6) . ? C44 C45 1.376(6) . ? C45 C46 1.377(6) . ? C46 C47 1.387(5) . ? C49 C50 1.362(5) . ? C49 C54 1.383(6) . ? C50 C51 1.392(6) . ? C51 C52 1.374(6) . ? C52 C53 1.393(6) . ? C52 C55 1.540(6) . ? C53 C54 1.376(6) . ? C55 C58 1.499(7) . ? C55 C57 1.518(7) . ? C55 C56 1.544(7) . ? C59 C60 1.362(6) . ? C59 C64 1.488(6) . ? C60 C61 1.387(6) . ? C61 C62 1.343(7) . ? C62 C63 1.383(6) . ? C64 C65 1.383(6) . ? C65 C66 1.390(6) . ? C66 C67 1.358(6) . ? C67 C68 1.393(6) . ? C67 C69 1.513(6) . ? C71 C72 1.382(5) . ? C71 C76 1.402(5) . ? C72 C73 1.389(6) . ? C73 C74 1.386(6) . ? C74 C75 1.381(6) . ? C75 C76 1.392(5) . ? C78 C79 1.384(6) . ? C78 C83 1.384(5) . ? C79 C80 1.381(7) . ? C80 C81 1.395(6) . ? C81 C82 1.384(6) . ? C81 C84 1.526(6) . ? C82 C83 1.394(6) . ? C84 C85 1.477(8) . ? C84 C87 1.505(8) . ? C84 C86 1.533(9) . ? O1S C6S 1.247(12) . ? N1S C7S 1.335(10) . ? N1S C6S 1.474(15) . ? N1S C8S 1.501(12) . ? C1S C2S 1.357(10) . ? O2S C3S 1.191(7) . ? N2S C3S 1.262(8) . ? N2S C4S 1.379(8) . ? N2S C5S 1.486(10) . ? C2S N3S 1.130(8) . ? 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 N1 Ni1 N8 92.77(12) . . ? N1 Ni1 N2 79.19(12) . . ? N8 Ni1 N2 92.13(12) . . ? N1 Ni1 N14 169.12(12) . . ? N8 Ni1 N14 96.53(12) . . ? N2 Ni1 N14 94.80(12) . . ? N1 Ni1 N13 92.59(13) . . ? N8 Ni1 N13 172.69(12) . . ? N2 Ni1 N13 93.75(12) . . ? N14 Ni1 N13 78.67(13) . . ? N1 Ni1 N7 98.24(12) . . ? N8 Ni1 N7 78.80(12) . . ? N2 Ni1 N7 170.49(13) . . ? N14 Ni1 N7 89.11(12) . . ? N13 Ni1 N7 95.51(13) . . ? O4 S1 O3 109.41(18) . . ? O4 S1 O1 109.76(16) . . ? O3 S1 O1 108.79(16) . . ? O4 S1 O2 110.51(17) . . ? O3 S1 O2 108.64(16) . . ? O1 S1 O2 109.69(16) . . ? C5 N1 C1 119.0(3) . . ? C5 N1 Ni1 126.3(3) . . ? C1 N1 Ni1 114.3(2) . . ? N1 C1 C2 120.8(3) . . ? N1 C1 C6 116.2(3) . . ? C2 C1 C6 122.9(3) . . ? C10 N2 C6 118.7(3) . . ? C10 N2 Ni1 126.1(2) . . ? C6 N2 Ni1 114.5(2) . . ? C3 C2 C1 119.5(4) . . ? C12 N3 C11 120.4(4) . . ? C4 C3 C2 119.3(4) . . ? C12 N4 C13 127.5(4) . . ? C5 C4 C3 117.7(4) . . ? C19 N5 C18 123.3(3) . . ? N1 C5 C4 123.7(4) . . ? C19 N6 C20 124.7(4) . . ? N2 C6 C7 120.5(4) . . ? N2 C6 C1 114.8(3) . . ? C7 C6 C1 124.6(4) . . ? C34 N7 C30 118.9(3) . . ? C34 N7 Ni1 126.4(3) . . ? C30 N7 Ni1 113.9(3) . . ? C6 C7 C8 119.8(4) . . ? C39 N8 C35 118.5(3) . . ? C39 N8 Ni1 126.5(2) . . ? C35 N8 Ni1 114.9(2) . . ? C9 C8 C7 120.1(4) . . ? C41 N9 C40 120.1(3) . . ? C8 C9 C10 117.7(4) . . ? C8 C9 C11 120.3(3) . . ? C10 C9 C11 122.0(4) . . ? C41 N10 C42 125.1(3) . . ? N2 C10 C9 123.0(4) . . ? C48 N11 C47 122.8(3) . . ? N3 C11 C9 115.3(3) . . ? C48 N12 C49 123.9(3) . . ? O9 C12 N3 122.0(4) . . ? O9 C12 N4 124.5(4) . . ? N3 C12 N4 113.5(4) . . ? C63 N13 C59 117.5(4) . . ? C63 N13 Ni1 127.1(3) . . ? C59 N13 Ni1 115.3(3) . . ? C14 C13 N4 123.7(4) . . ? C14 C13 C18 118.6(4) . . ? N4 C13 C18 117.7(4) . . ? C68 N14 C64 118.6(3) . . ? C68 N14 Ni1 126.4(3) . . ? C64 N14 Ni1 114.9(3) . . ? C15 C14 C13 120.5(5) . . ? C70 N15 C69 121.2(4) . . ? C14 C15 C16 120.5(4) . . ? C70 N16 C71 125.8(3) . . ? C17 C16 C15 119.5(5) . . ? C77 N17 C76 123.2(3) . . ? C16 C17 C18 121.1(5) . . ? C77 N18 C78 123.5(3) . . ? C17 C18 C13 119.8(4) . . ? C17 C18 N5 121.4(4) . . ? C13 C18 N5 118.8(4) . . ? O10 C19 N6 124.8(4) . . ? O10 C19 N5 123.1(4) . . ? N6 C19 N5 112.1(4) . . ? C21 C20 C25 117.1(4) . . ? C21 C20 N6 125.0(4) . . ? C25 C20 N6 117.8(4) . . ? C20 C21 C22 121.5(4) . . ? C23 C22 C21 121.9(4) . . ? C22 C23 C24 116.5(4) . . ? C22 C23 C26 123.3(4) . . ? C24 C23 C26 120.1(4) . . ? C25 C24 C23 121.8(4) . . ? C24 C25 C20 121.0(4) . . ? C27 C26 C28 108.8(4) . . ? C27 C26 C23 111.1(4) . . ? C28 C26 C23 111.9(4) . . ? C27 C26 C29 108.7(4) . . ? C28 C26 C29 107.5(4) . . ? C23 C26 C29 108.7(4) . . ? N7 C30 C31 121.1(4) . . ? N7 C30 C35 116.1(3) . . ? C31 C30 C35 122.9(4) . . ? C30 C31 C32 118.6(4) . . ? C33 C32 C31 120.0(4) . . ? C32 C33 C34 118.1(5) . . ? N7 C34 C33 123.2(4) . . ? N8 C35 C36 120.6(4) . . ? N8 C35 C30 114.9(3) . . ? C36 C35 C30 124.4(3) . . ? C37 C36 C35 119.2(4) . . ? C36 C37 C38 120.8(4) . . ? C37 C38 C39 116.8(4) . . ? C37 C38 C40 123.8(4) . . ? C39 C38 C40 119.3(3) . . ? N8 C39 C38 124.0(3) . . ? N9 C40 C38 113.2(3) . . ? O5 C41 N9 123.2(4) . . ? O5 C41 N10 124.3(4) . . ? N9 C41 N10 112.5(3) . . ? C47 C42 C43 118.9(4) . . ? C47 C42 N10 119.7(3) . . ? C43 C42 N10 121.4(4) . . ? C44 C43 C42 120.0(4) . . ? C45 C44 C43 121.1(4) . . ? C44 C45 C46 119.0(4) . . ? C45 C46 C47 121.3(4) . . ? C46 C47 C42 119.6(4) . . ? C46 C47 N11 120.8(3) . . ? C42 C47 N11 119.5(3) . . ? O6 C48 N12 123.5(3) . . ? O6 C48 N11 124.6(4) . . ? N12 C48 N11 111.8(4) . . ? C50 C49 C54 119.1(4) . . ? C50 C49 N12 123.6(4) . . ? C54 C49 N12 117.3(4) . . ? C49 C50 C51 119.9(4) . . ? C52 C51 C50 122.6(4) . . ? C51 C52 C53 116.0(4) . . ? C51 C52 C55 125.0(4) . . ? C53 C52 C55 119.0(4) . . ? C54 C53 C52 122.3(4) . . ? C53 C54 C49 120.0(4) . . ? C58 C55 C57 111.4(5) . . ? C58 C55 C52 108.9(4) . . ? C57 C55 C52 111.4(4) . . ? C58 C55 C56 108.8(4) . . ? C57 C55 C56 106.6(4) . . ? C52 C55 C56 109.7(4) . . ? N13 C59 C60 121.6(4) . . ? N13 C59 C64 114.7(3) . . ? C60 C59 C64 123.6(4) . . ? C59 C60 C61 120.1(5) . . ? C62 C61 C60 118.5(4) . . ? C61 C62 C63 119.4(4) . . ? N13 C63 C62 122.7(5) . . ? N14 C64 C65 121.6(4) . . ? N14 C64 C59 116.2(4) . . ? C65 C64 C59 122.2(4) . . ? C64 C65 C66 118.6(4) . . ? C67 C66 C65 120.3(4) . . ? C66 C67 C68 117.6(4) . . ? C66 C67 C69 120.5(4) . . ? C68 C67 C69 121.8(4) . . ? N14 C68 C67 123.2(4) . . ? N15 C69 C67 114.2(3) . . ? O7 C70 N15 122.9(4) . . ? O7 C70 N16 125.1(4) . . ? N15 C70 N16 112.0(4) . . ? C72 C71 C76 120.4(4) . . ? C72 C71 N16 122.2(4) . . ? C76 C71 N16 117.3(3) . . ? C71 C72 C73 120.2(4) . . ? C74 C73 C72 120.0(4) . . ? C75 C74 C73 119.7(4) . . ? C74 C75 C76 121.2(4) . . ? C75 C76 C71 118.4(4) . . ? C75 C76 N17 121.9(4) . . ? C71 C76 N17 119.7(3) . . ? O8 C77 N18 123.8(4) . . ? O8 C77 N17 121.8(4) . . ? N18 C77 N17 114.4(3) . . ? C79 C78 C83 118.3(4) . . ? C79 C78 N18 118.1(4) . . ? C83 C78 N18 123.6(4) . . ? C80 C79 C78 121.8(4) . . ? C79 C80 C81 121.0(4) . . ? C82 C81 C80 116.3(4) . . ? C82 C81 C84 121.5(4) . . ? C80 C81 C84 122.2(4) . . ? C81 C82 C83 123.2(4) . . ? C78 C83 C82 119.2(4) . . ? C85 C84 C87 109.4(6) . . ? C85 C84 C81 109.3(4) . . ? C87 C84 C81 112.1(5) . . ? C85 C84 C86 111.1(7) . . ? C87 C84 C86 104.6(6) . . ? C81 C84 C86 110.3(5) . . ? C7S N1S C6S 112.7(11) . . ? C7S N1S C8S 122.6(12) . . ? C6S N1S C8S 124.7(9) . . ? C3S N2S C4S 121.6(6) . . ? C3S N2S C5S 119.7(7) . . ? C4S N2S C5S 118.4(7) . . ? N3S C2S C1S 177.9(8) . . ? O2S C3S N2S 129.9(7) . . ? O1S C6S N1S 123.4(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.639 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.072 # Attachment '- M2a.cif' data_c:\frames\475\work\475sq _database_code_depnum_ccdc_archive 'CCDC 879406' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common M2a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H90 Fe N18 O10 S' _chemical_formula_weight 1635.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.318(2) _cell_length_b 18.423(3) _cell_length_c 19.119(3) _cell_angle_alpha 85.524(3) _cell_angle_beta 85.020(3) _cell_angle_gamma 78.522(3) _cell_volume 5257.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9637 _exptl_absorpt_correction_T_max 0.9742 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37150 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.1239 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18476 _reflns_number_gt 7737 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Crystal diffracted poorly due to its high content of disordered solvent, with very few reflections observed at 2theta > 40 degrees. There was significan residual electron density inside the crystal's pores, which could not be assigned unambiguously, and was therefore treated with the SQUEEZE routine in PLATON. 329 residual electrons/unit cell were thus found, and their contribution was substracted from the hkl file. There was significant disordered in some of the ligand atoms, resulting in unreasonable anisotropic displacement parameters. These atoms were therefore refined isotropically. ; _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^)+(0.1555P)^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 18476 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2709 _refine_ls_wR_factor_gt 0.2409 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.879 _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 Fe1 Fe 0.44211(4) 0.67532(4) 0.71521(4) 0.0534(3) Uani 1 1 d . . . S1 S 0.83305(8) 0.37509(7) 0.70473(7) 0.0530(4) Uani 1 1 d . . . O1 O 0.9158(2) 0.31790(19) 0.7026(2) 0.0705(11) Uani 1 1 d . . . N1 N 0.3536(3) 0.6897(2) 0.6462(3) 0.0636(12) Uani 1 1 d . . . C1 C 0.3130(3) 0.6310(3) 0.6410(3) 0.0655(16) Uani 1 1 d . . . O2 O 0.7555(2) 0.33978(18) 0.70264(18) 0.0592(9) Uani 1 1 d . . . N2 N 0.4249(3) 0.5733(2) 0.7157(2) 0.0562(11) Uani 1 1 d . . . C2 C 0.2417(3) 0.6350(4) 0.6011(4) 0.0772(18) Uani 1 1 d . . . H2 H 0.2138 0.5935 0.5998 0.093 Uiso 1 1 calc R . . O3 O 0.8365(2) 0.42931(17) 0.64475(17) 0.0539(9) Uani 1 1 d . . . N3 N 0.5989(3) 0.3886(2) 0.8029(3) 0.0725(14) Uani 1 1 d . . . H3 H 0.6464 0.3877 0.7734 0.087 Uiso 1 1 calc R . . C3 C 0.2111(4) 0.7007(4) 0.5630(4) 0.092(2) Uani 1 1 d . . . H3A H 0.1611 0.7053 0.5357 0.110 Uiso 1 1 calc R . . O4 O 0.8246(2) 0.41399(18) 0.76996(18) 0.0590(9) Uani 1 1 d . . . N4 N 0.6832(3) 0.4148(3) 0.8867(3) 0.0716(14) Uani 1 1 d . . . H4 H 0.7256 0.4096 0.8523 0.086 Uiso 1 1 calc R . . C4 C 0.2543(4) 0.7599(4) 0.5649(4) 0.088(2) Uani 1 1 d . . . H4A H 0.2354 0.8049 0.5379 0.105 Uiso 1 1 calc R . . O5 O 0.5730(2) 0.4169(2) 0.4988(2) 0.0714(11) Uani 1 1 d . . . N5 N 0.8595(3) 0.3775(3) 0.9153(3) 0.106(2) Uani 1 1 d D . . H5 H 0.8618 0.3983 0.8724 0.127 Uiso 1 1 calc R . . C5 C 0.3258(4) 0.7522(4) 0.6072(3) 0.0758(18) Uani 1 1 d . . . H5A H 0.3557 0.7926 0.6083 0.091 Uiso 1 1 calc R . . O6 O 0.8284(2) 0.1164(2) 0.5594(2) 0.0739(12) Uani 1 1 d . . . N6 N 0.9411(5) 0.2730(4) 0.8687(3) 0.147(3) Uani 1 1 d D . . H6 H 0.9270 0.2940 0.8272 0.176 Uiso 1 1 calc R . . C6 C 0.3566(3) 0.5628(3) 0.6815(3) 0.0627(15) Uani 1 1 d . . . O7 O 0.8359(3) 0.6805(2) 0.7253(2) 0.0834(12) Uani 1 1 d . . . N7 N 0.4642(3) 0.7770(2) 0.7082(2) 0.0552(11) Uani 1 1 d . . . C7 C 0.3339(4) 0.4929(4) 0.6809(4) 0.0819(19) Uani 1 1 d . . . H7 H 0.2830 0.4875 0.6582 0.098 Uiso 1 1 calc R . . O8 O 1.1657(3) 0.4554(2) 0.6095(2) 0.0787(12) Uani 1 1 d . . . N8 N 0.5396(2) 0.6636(2) 0.6418(2) 0.0465(10) Uani 1 1 d . . . C8 C 0.3849(4) 0.4331(3) 0.7128(4) 0.082(2) Uani 1 1 d . . . H8 H 0.3696 0.3856 0.7127 0.099 Uiso 1 1 calc R . . O9 O 0.5368(3) 0.4070(2) 0.9133(2) 0.0963(15) Uani 1 1 d . . . N9 N 0.6731(3) 0.4614(2) 0.5572(2) 0.0627(12) Uani 1 1 d . . . H9 H 0.7077 0.4534 0.5925 0.075 Uiso 1 1 calc R . . C9 C 0.4593(4) 0.4409(3) 0.7457(3) 0.0655(16) Uani 1 1 d . . . O10 O 0.9363(6) 0.2939(5) 0.9963(4) 0.226(4) Uani 1 1 d D . . N10 N 0.6411(3) 0.3471(2) 0.5903(3) 0.0693(13) Uani 1 1 d . . . H10 H 0.6732 0.3494 0.6257 0.083 Uiso 1 1 calc R . . C10 C 0.4747(3) 0.5115(3) 0.7478(3) 0.0601(15) Uani 1 1 d . . . H10A H 0.5230 0.5181 0.7730 0.072 Uiso 1 1 calc R . . N11 N 0.7533(3) 0.2125(3) 0.6244(3) 0.0796(16) Uani 1 1 d . . . H11 H 0.7587 0.2438 0.6555 0.095 Uiso 1 1 calc R . . C11 C 0.5201(4) 0.3744(3) 0.7791(4) 0.084(2) Uani 1 1 d . . . H11A H 0.4859 0.3535 0.8194 0.100 Uiso 1 1 calc R . . H11B H 0.5365 0.3360 0.7443 0.100 Uiso 1 1 calc R . . N12 N 0.9058(3) 0.1800(2) 0.6229(3) 0.0703(14) Uani 1 1 d . . . H12 H 0.8987 0.2168 0.6510 0.084 Uiso 1 1 calc R . . C12 C 0.7059(4) 0.4334(4) 0.9501(4) 0.083(2) Uani 1 1 d . . . N13 N 0.3491(3) 0.6945(2) 0.7937(3) 0.0713(14) Uani 1 1 d . . . C13 C 0.6462(5) 0.4709(4) 1.0002(4) 0.093(2) Uani 1 1 d . . . H13 H 0.5849 0.4835 0.9909 0.112 Uiso 1 1 calc R . . N14 N 0.5198(3) 0.6546(2) 0.7938(2) 0.0484(10) Uani 1 1 d . . . C14 C 0.6702(6) 0.4907(5) 1.0616(5) 0.121(3) Uani 1 1 d . . . H14 H 0.6261 0.5146 1.0947 0.146 Uiso 1 1 calc R . . N15 N 0.7942(3) 0.5727(3) 0.7722(3) 0.0638(12) Uani 1 1 d . . . H15 H 0.7897 0.5271 0.7648 0.077 Uiso 1 1 calc R . . C15 C 0.7618(6) 0.4756(5) 1.0763(4) 0.137(4) Uani 1 1 d . . . H15A H 0.7808 0.4908 1.1178 0.165 Uiso 1 1 calc R . . N16 N 0.8676(3) 0.5760(3) 0.6641(3) 0.0684(13) Uani 1 1 d . . . H16 H 0.8542 0.5320 0.6619 0.082 Uiso 1 1 calc R . . C16 C 0.8220(5) 0.4377(5) 1.0274(4) 0.135(4) Uani 1 1 d . . . H16A H 0.8831 0.4246 1.0371 0.162 Uiso 1 1 calc R . . N17 N 1.0133(3) 0.4771(2) 0.6127(2) 0.0578(11) Uani 1 1 d . . . H17 H 0.9663 0.4572 0.6258 0.069 Uiso 1 1 calc R . . C17 C 0.7971(5) 0.4179(4) 0.9650(4) 0.099(2) Uani 1 1 d . . . N18 N 1.0915(3) 0.3669(2) 0.6577(2) 0.0589(12) Uani 1 1 d . . . H18 H 1.0401 0.3520 0.6598 0.071 Uiso 1 1 calc R . . C18 C 0.9132(8) 0.3143(8) 0.9249(8) 0.179(4) Uiso 1 1 d D . . C19 C 0.9896(7) 0.2011(7) 0.8700(7) 0.155(4) Uiso 1 1 d D . . C20 C 1.0431(7) 0.1696(7) 0.9372(7) 0.188(5) Uiso 1 1 d D . . H20 H 1.0486 0.1945 0.9779 0.226 Uiso 1 1 calc R . . C21 C 1.0834(8) 0.0897(8) 0.9202(8) 0.196(5) Uiso 1 1 d D . . H21 H 1.1235 0.0628 0.9526 0.235 Uiso 1 1 calc R . . C22 C 1.0690(7) 0.0480(5) 0.8602(7) 0.166(5) Uani 1 1 d D . . C23 C 1.0440(5) 0.0898(5) 0.8023(6) 0.127(3) Uani 1 1 d D . . H23 H 1.0579 0.0716 0.7567 0.152 Uiso 1 1 calc R . . C24 C 0.9935(6) 0.1655(4) 0.8130(6) 0.130(4) Uani 1 1 d D . . H24 H 0.9611 0.1906 0.7752 0.156 Uiso 1 1 calc R . . C25 C 1.1155(8) -0.0364(5) 0.8527(7) 0.156(4) Uani 1 1 d . . . C26 C 1.0528(8) -0.0809(6) 0.8828(8) 0.215(7) Uani 1 1 d . . . H26A H 1.0033 -0.0755 0.8524 0.322 Uiso 1 1 calc R . . H26B H 1.0296 -0.0645 0.9295 0.322 Uiso 1 1 calc R . . H26C H 1.0828 -0.1331 0.8869 0.322 Uiso 1 1 calc R . . C27 C 1.1872(10) -0.0551(8) 0.9011(8) 0.222(6) Uiso 1 1 d . . . H27A H 1.1654 -0.0355 0.9469 0.333 Uiso 1 1 calc R . . H27B H 1.2382 -0.0331 0.8819 0.333 Uiso 1 1 calc R . . H27C H 1.2060 -0.1091 0.9067 0.333 Uiso 1 1 calc R . . C28 C 1.1605(9) -0.0521(7) 0.7865(8) 0.249(9) Uani 1 1 d . . . H28A H 1.1178 -0.0401 0.7500 0.374 Uiso 1 1 calc R . . H28B H 1.1880 -0.1049 0.7866 0.374 Uiso 1 1 calc R . . H28C H 1.2070 -0.0222 0.7767 0.374 Uiso 1 1 calc R . . C29 C 0.6027(4) 0.4039(3) 0.8722(4) 0.0768(19) Uani 1 1 d . . . C30 C 0.3813(4) 0.6875(3) 0.8578(4) 0.0706(17) Uani 1 1 d . . . C31 C 0.3240(6) 0.7035(4) 0.9177(4) 0.108(3) Uani 1 1 d . . . H31 H 0.3469 0.6983 0.9629 0.130 Uiso 1 1 calc R . . C32 C 0.2335(7) 0.7269(5) 0.9106(7) 0.132(4) Uani 1 1 d . . . H32 H 0.1941 0.7423 0.9502 0.159 Uiso 1 1 calc R . . C33 C 0.2023(6) 0.7278(5) 0.8482(7) 0.141(5) Uani 1 1 d . . . H33 H 0.1396 0.7376 0.8439 0.169 Uiso 1 1 calc R . . C34 C 0.2603(4) 0.7143(3) 0.7890(4) 0.093(2) Uani 1 1 d . . . H34 H 0.2370 0.7192 0.7440 0.112 Uiso 1 1 calc R . . C35 C 0.4779(4) 0.6639(3) 0.8593(3) 0.0627(15) Uani 1 1 d . . . C36 C 0.5243(5) 0.6520(3) 0.9184(3) 0.085(2) Uani 1 1 d . . . H36 H 0.4930 0.6574 0.9634 0.102 Uiso 1 1 calc R . . C37 C 0.6159(5) 0.6321(3) 0.9132(3) 0.0769(18) Uani 1 1 d . . . H37 H 0.6480 0.6251 0.9543 0.092 Uiso 1 1 calc R . . C38 C 0.6610(4) 0.6224(3) 0.8477(3) 0.0574(14) Uani 1 1 d . . . C39 C 0.6089(3) 0.6342(2) 0.7896(3) 0.0504(13) Uani 1 1 d . . . H39 H 0.6388 0.6273 0.7443 0.060 Uiso 1 1 calc R . . C40 C 0.7598(4) 0.6034(3) 0.8394(3) 0.0724(17) Uani 1 1 d . . . H40A H 0.7840 0.6487 0.8440 0.087 Uiso 1 1 calc R . . H40B H 0.7815 0.5670 0.8779 0.087 Uiso 1 1 calc R . . C41 C 0.8337(4) 0.6139(4) 0.7201(4) 0.0690(17) Uani 1 1 d . . . C42 C 0.9241(3) 0.6007(3) 0.6071(3) 0.0585(14) Uani 1 1 d . . . C43 C 0.9049(4) 0.6721(3) 0.5771(4) 0.0784(19) Uani 1 1 d . . . H43 H 0.8534 0.7055 0.5943 0.094 Uiso 1 1 calc R . . C44 C 0.9594(5) 0.6955(4) 0.5225(4) 0.0801(19) Uani 1 1 d . . . H44 H 0.9477 0.7454 0.5036 0.096 Uiso 1 1 calc R . . C45 C 1.0315(5) 0.6453(4) 0.4957(3) 0.0779(19) Uani 1 1 d . . . H45 H 1.0678 0.6607 0.4567 0.094 Uiso 1 1 calc R . . C46 C 1.0521(4) 0.5728(3) 0.5241(3) 0.0664(15) Uani 1 1 d . . . H46 H 1.1026 0.5393 0.5055 0.080 Uiso 1 1 calc R . . C47 C 0.9969(4) 0.5494(3) 0.5816(3) 0.0564(14) Uani 1 1 d . . . C48 C 1.0946(4) 0.4342(3) 0.6249(3) 0.0567(14) Uani 1 1 d . . . C49 C 1.1630(3) 0.3182(3) 0.6889(3) 0.0576(14) Uani 1 1 d . . . C50 C 1.1425(4) 0.2817(4) 0.7534(3) 0.0779(18) Uani 1 1 d . . . H50 H 1.0828 0.2902 0.7738 0.093 Uiso 1 1 calc R . . C51 C 1.2084(4) 0.2336(4) 0.7876(4) 0.087(2) Uani 1 1 d . . . H51 H 1.1927 0.2101 0.8316 0.104 Uiso 1 1 calc R . . C52 C 1.2970(4) 0.2180(3) 0.7602(3) 0.0646(15) Uani 1 1 d . . . C53 C 1.3137(4) 0.2545(3) 0.6956(3) 0.0653(15) Uani 1 1 d . . . H53 H 1.3728 0.2452 0.6741 0.078 Uiso 1 1 calc R . . C54 C 1.2492(3) 0.3036(3) 0.6611(3) 0.0595(14) Uani 1 1 d . . . H54 H 1.2650 0.3277 0.6174 0.071 Uiso 1 1 calc R . . C55 C 1.3667(4) 0.1656(4) 0.8012(4) 0.0836(19) Uani 1 1 d . . . C56 C 1.3858(7) 0.2067(6) 0.8654(5) 0.161(4) Uani 1 1 d . . . H56A H 1.3311 0.2184 0.8963 0.242 Uiso 1 1 calc R . . H56B H 1.4057 0.2527 0.8483 0.242 Uiso 1 1 calc R . . H56C H 1.4326 0.1746 0.8915 0.242 Uiso 1 1 calc R . . C57 C 1.4527(8) 0.1515(6) 0.7607(6) 0.176(4) Uiso 1 1 d . . . H57A H 1.4965 0.1183 0.7887 0.263 Uiso 1 1 calc R . . H57B H 1.4728 0.1985 0.7485 0.263 Uiso 1 1 calc R . . H57C H 1.4466 0.1281 0.7175 0.263 Uiso 1 1 calc R . . C58 C 1.3327(6) 0.1004(5) 0.8339(6) 0.172(5) Uani 1 1 d . . . H58A H 1.2735 0.1167 0.8575 0.258 Uiso 1 1 calc R . . H58B H 1.3736 0.0743 0.8683 0.258 Uiso 1 1 calc R . . H58C H 1.3285 0.0669 0.7974 0.258 Uiso 1 1 calc R . . C59 C 0.5376(4) 0.7872(3) 0.6689(3) 0.0564(14) Uani 1 1 d . . . C60 C 0.5690(4) 0.8530(3) 0.6643(3) 0.0794(18) Uani 1 1 d . . . H60 H 0.6215 0.8583 0.6357 0.095 Uiso 1 1 calc R . . C61 C 0.5220(6) 0.9106(4) 0.7023(4) 0.104(2) Uani 1 1 d . . . H61 H 0.5426 0.9560 0.7013 0.125 Uiso 1 1 calc R . . C62 C 0.4455(5) 0.9017(3) 0.7414(3) 0.0833(19) Uani 1 1 d . . . H62 H 0.4112 0.9412 0.7670 0.100 Uiso 1 1 calc R . . C63 C 0.4193(4) 0.8348(3) 0.7431(3) 0.0630(15) Uani 1 1 d . . . H63 H 0.3661 0.8291 0.7706 0.076 Uiso 1 1 calc R . . C64 C 0.5822(3) 0.7221(3) 0.6300(3) 0.0498(13) Uani 1 1 d . . . C65 C 0.6571(4) 0.7179(3) 0.5837(3) 0.0601(14) Uani 1 1 d . . . H65 H 0.6877 0.7583 0.5769 0.072 Uiso 1 1 calc R . . C66 C 0.6874(3) 0.6545(3) 0.5471(3) 0.0584(14) Uani 1 1 d . . . H66 H 0.7402 0.6509 0.5165 0.070 Uiso 1 1 calc R . . C67 C 0.6423(3) 0.5976(3) 0.5548(3) 0.0501(13) Uani 1 1 d . . . C68 C 0.5694(3) 0.6034(3) 0.6040(3) 0.0528(13) Uani 1 1 d . . . H68 H 0.5389 0.5630 0.6114 0.063 Uiso 1 1 calc R . . C69 C 0.6674(3) 0.5301(3) 0.5126(3) 0.0623(15) Uani 1 1 d . . . H69A H 0.6223 0.5318 0.4781 0.075 Uiso 1 1 calc R . . H69B H 0.7258 0.5306 0.4861 0.075 Uiso 1 1 calc R . . C70 C 0.6250(3) 0.4097(3) 0.5444(3) 0.0634(16) Uani 1 1 d . . . C71 C 0.6116(3) 0.2815(3) 0.5859(3) 0.0683(16) Uani 1 1 d . . . C72 C 0.5275(3) 0.2806(4) 0.5631(3) 0.0705(16) Uani 1 1 d . . . H72 H 0.4883 0.3263 0.5527 0.085 Uiso 1 1 calc R . . C73 C 0.5003(4) 0.2148(4) 0.5553(3) 0.0734(17) Uani 1 1 d . . . H73 H 0.4439 0.2152 0.5381 0.088 Uiso 1 1 calc R . . C74 C 0.5561(4) 0.1480(3) 0.5728(4) 0.0800(18) Uani 1 1 d . . . H74 H 0.5377 0.1024 0.5680 0.096 Uiso 1 1 calc R . . C75 C 0.6370(4) 0.1478(4) 0.5969(4) 0.085(2) Uani 1 1 d . . . H75 H 0.6737 0.1017 0.6101 0.102 Uiso 1 1 calc R . . C76 C 0.6676(3) 0.2132(3) 0.6028(4) 0.0739(18) Uani 1 1 d . . . C77 C 0.8298(4) 0.1647(3) 0.5992(4) 0.0709(17) Uani 1 1 d . . . C78 C 0.9947(3) 0.1425(3) 0.6068(3) 0.0579(14) Uani 1 1 d . . . C79 C 1.0176(4) 0.0795(4) 0.5692(4) 0.087(2) Uani 1 1 d . . . H79 H 0.9722 0.0591 0.5516 0.105 Uiso 1 1 calc R . . C80 C 1.1052(4) 0.0463(3) 0.5572(4) 0.091(2) Uani 1 1 d . . . H80 H 1.1186 0.0005 0.5351 0.109 Uiso 1 1 calc R . . C81 C 1.1754(3) 0.0765(3) 0.5757(3) 0.0559(14) Uani 1 1 d . . . C82 C 1.1507(3) 0.1394(3) 0.6114(3) 0.0643(15) Uani 1 1 d . . . H82 H 1.1959 0.1620 0.6264 0.077 Uiso 1 1 calc R . . C83 C 1.0619(3) 0.1716(3) 0.6267(3) 0.0703(17) Uani 1 1 d . . . H83 H 1.0481 0.2153 0.6520 0.084 Uiso 1 1 calc R . . C84 C 1.2719(3) 0.0392(3) 0.5557(3) 0.0688(16) Uani 1 1 d . . . C85 C 1.2889(6) 0.0423(5) 0.4783(5) 0.157(4) Uani 1 1 d . . . H85A H 1.3510 0.0189 0.4659 0.235 Uiso 1 1 calc R . . H85B H 1.2783 0.0942 0.4598 0.235 Uiso 1 1 calc R . . H85C H 1.2487 0.0158 0.4578 0.235 Uiso 1 1 calc R . . C86 C 1.2901(4) -0.0417(4) 0.5793(4) 0.102(2) Uani 1 1 d . . . H86A H 1.3526 -0.0634 0.5661 0.154 Uiso 1 1 calc R . . H86B H 1.2509 -0.0673 0.5566 0.154 Uiso 1 1 calc R . . H86C H 1.2788 -0.0473 0.6305 0.154 Uiso 1 1 calc R . . C87 C 1.3348(8) 0.0736(6) 0.5945(6) 0.174(4) Uiso 1 1 d . . . H87A H 1.3967 0.0500 0.5819 0.261 Uiso 1 1 calc R . . H87B H 1.3217 0.0662 0.6453 0.261 Uiso 1 1 calc R . . H87C H 1.3264 0.1269 0.5812 0.261 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 Fe1 0.0408(4) 0.0469(4) 0.0682(5) -0.0047(4) -0.0011(4) 0.0009(3) S1 0.0401(7) 0.0464(8) 0.0666(9) 0.0036(7) 0.0047(6) -0.0003(6) O1 0.043(2) 0.051(2) 0.109(3) 0.005(2) 0.009(2) 0.0034(16) N1 0.041(2) 0.054(3) 0.092(3) -0.016(3) -0.013(2) 0.010(2) C1 0.035(3) 0.069(4) 0.094(4) -0.028(3) -0.008(3) -0.005(3) O2 0.0440(19) 0.053(2) 0.076(2) 0.0006(18) 0.0051(17) -0.0042(16) N2 0.040(2) 0.051(3) 0.076(3) -0.009(2) 0.006(2) -0.007(2) C2 0.040(3) 0.078(4) 0.114(5) -0.038(4) -0.013(3) 0.002(3) O3 0.052(2) 0.049(2) 0.058(2) 0.0015(17) 0.0084(17) -0.0084(16) N3 0.057(3) 0.046(3) 0.102(4) 0.014(3) 0.023(3) -0.001(2) C3 0.056(4) 0.097(5) 0.123(6) -0.051(5) -0.033(4) 0.014(4) O4 0.055(2) 0.054(2) 0.063(2) 0.0075(18) -0.0012(18) -0.0068(17) N4 0.047(3) 0.076(3) 0.071(4) 0.023(3) 0.019(3) 0.016(2) C4 0.062(4) 0.081(5) 0.113(5) -0.024(4) -0.036(4) 0.026(3) O5 0.045(2) 0.067(3) 0.100(3) -0.017(2) -0.017(2) 0.0029(18) N5 0.066(3) 0.149(5) 0.059(3) 0.033(3) 0.008(3) 0.060(3) C5 0.055(3) 0.075(4) 0.093(5) -0.023(4) -0.020(3) 0.010(3) O6 0.051(2) 0.047(2) 0.124(3) -0.021(2) -0.019(2) 0.0006(18) N6 0.180(7) 0.097(5) 0.102(5) 0.033(4) 0.076(5) 0.068(5) C6 0.034(3) 0.063(4) 0.092(4) -0.034(3) 0.005(3) -0.004(3) O7 0.096(3) 0.065(3) 0.093(3) -0.005(2) -0.023(2) -0.019(2) N7 0.051(3) 0.046(3) 0.064(3) -0.002(2) -0.010(2) 0.005(2) C7 0.047(3) 0.086(5) 0.116(5) -0.040(4) 0.005(3) -0.016(3) O8 0.054(2) 0.080(3) 0.105(3) 0.015(2) -0.016(2) -0.022(2) N8 0.035(2) 0.049(2) 0.051(2) -0.001(2) -0.0084(19) 0.0039(19) C8 0.049(3) 0.053(4) 0.142(6) -0.017(4) 0.015(4) -0.008(3) O9 0.063(3) 0.090(3) 0.113(3) 0.025(3) 0.041(3) 0.009(2) N9 0.046(2) 0.059(3) 0.080(3) -0.013(3) -0.007(2) 0.005(2) C9 0.046(3) 0.046(3) 0.103(5) -0.010(3) 0.019(3) -0.014(3) O10 0.214(8) 0.243(9) 0.156(7) 0.035(6) 0.038(6) 0.073(7) N10 0.048(3) 0.050(3) 0.109(4) -0.009(3) -0.020(3) -0.001(2) C10 0.033(3) 0.058(4) 0.084(4) -0.001(3) 0.005(3) -0.002(2) N11 0.044(3) 0.059(3) 0.137(5) -0.020(3) -0.031(3) 0.005(2) C11 0.069(4) 0.043(3) 0.134(6) -0.011(4) 0.019(4) -0.006(3) N12 0.035(2) 0.048(3) 0.125(4) -0.013(3) -0.020(3) 0.008(2) C12 0.064(4) 0.097(5) 0.061(4) 0.031(4) 0.014(3) 0.027(3) N13 0.048(3) 0.057(3) 0.107(4) -0.016(3) 0.008(3) -0.007(2) C13 0.077(4) 0.091(5) 0.081(5) 0.023(4) 0.020(4) 0.034(4) N14 0.043(2) 0.043(2) 0.055(3) 0.0040(19) 0.001(2) -0.0030(18) C14 0.117(7) 0.127(7) 0.078(6) 0.018(5) 0.032(5) 0.049(5) N15 0.051(3) 0.052(3) 0.087(4) -0.002(3) -0.012(3) -0.006(2) C15 0.127(7) 0.186(9) 0.062(5) -0.016(5) 0.005(5) 0.056(6) N16 0.056(3) 0.060(3) 0.088(4) -0.005(3) 0.002(3) -0.011(2) C16 0.106(6) 0.203(10) 0.058(5) -0.003(5) -0.011(4) 0.060(6) N17 0.043(2) 0.059(3) 0.071(3) -0.002(2) 0.002(2) -0.014(2) C17 0.085(5) 0.121(6) 0.062(4) 0.012(4) 0.019(4) 0.035(4) N18 0.039(2) 0.067(3) 0.071(3) 0.002(2) -0.006(2) -0.011(2) C22 0.172(10) 0.104(7) 0.188(11) 0.071(8) 0.006(8) 0.019(7) C23 0.110(6) 0.094(6) 0.168(9) 0.034(6) -0.013(6) -0.014(5) C24 0.131(7) 0.072(5) 0.199(10) 0.057(6) -0.093(7) -0.037(5) C25 0.134(8) 0.097(7) 0.200(11) 0.036(7) 0.042(8) 0.026(6) C26 0.167(10) 0.109(8) 0.330(17) 0.004(9) 0.134(12) -0.007(7) C28 0.231(14) 0.169(11) 0.257(15) 0.061(11) 0.140(13) 0.086(10) C29 0.057(4) 0.051(4) 0.101(6) 0.027(4) 0.024(4) 0.017(3) C30 0.066(4) 0.053(4) 0.085(5) -0.008(3) 0.030(4) -0.007(3) C31 0.121(6) 0.074(5) 0.113(6) -0.012(4) 0.065(5) -0.008(4) C32 0.101(7) 0.096(6) 0.197(11) -0.061(7) 0.086(7) -0.030(5) C33 0.064(5) 0.111(7) 0.254(13) -0.111(9) 0.054(7) -0.025(5) C34 0.047(4) 0.071(4) 0.159(7) -0.042(4) 0.021(4) -0.003(3) C35 0.083(4) 0.049(3) 0.049(4) -0.002(3) 0.016(3) -0.005(3) C36 0.117(6) 0.068(4) 0.055(4) 0.003(3) 0.029(4) 0.003(4) C37 0.104(5) 0.077(4) 0.039(3) 0.002(3) -0.002(3) 0.007(4) C38 0.071(4) 0.048(3) 0.048(3) 0.006(2) -0.014(3) 0.004(3) C39 0.055(3) 0.038(3) 0.055(3) 0.000(2) 0.001(3) -0.005(2) C40 0.074(4) 0.070(4) 0.071(4) -0.007(3) -0.028(3) 0.001(3) C41 0.052(3) 0.054(4) 0.101(5) -0.009(4) -0.027(4) 0.000(3) C42 0.042(3) 0.059(4) 0.076(4) 0.003(3) -0.005(3) -0.015(3) C43 0.057(4) 0.062(4) 0.121(6) 0.022(4) -0.026(4) -0.025(3) C44 0.073(4) 0.068(4) 0.105(5) 0.018(4) -0.032(4) -0.025(4) C45 0.085(5) 0.087(5) 0.073(4) 0.015(4) -0.025(4) -0.044(4) C46 0.072(4) 0.078(4) 0.054(4) 0.000(3) -0.009(3) -0.026(3) C47 0.057(3) 0.053(3) 0.061(4) 0.004(3) -0.010(3) -0.017(3) C48 0.047(3) 0.064(4) 0.061(4) -0.001(3) -0.004(3) -0.017(3) C49 0.047(3) 0.058(3) 0.067(4) -0.005(3) 0.001(3) -0.011(3) C50 0.054(3) 0.091(5) 0.079(4) 0.015(4) 0.007(3) -0.004(3) C51 0.061(4) 0.098(5) 0.089(5) 0.026(4) 0.001(4) -0.001(4) C52 0.053(3) 0.063(4) 0.077(4) 0.003(3) -0.011(3) -0.009(3) C53 0.052(3) 0.054(3) 0.092(5) -0.006(3) -0.001(3) -0.014(3) C54 0.043(3) 0.063(4) 0.071(4) -0.001(3) -0.001(3) -0.010(3) C55 0.056(4) 0.077(4) 0.116(6) 0.011(4) -0.013(4) -0.014(3) C56 0.172(10) 0.142(9) 0.171(10) 0.005(7) -0.077(8) -0.011(7) C58 0.112(7) 0.123(8) 0.249(12) 0.089(8) 0.003(8) 0.007(6) C59 0.058(3) 0.043(3) 0.065(4) 0.005(3) -0.008(3) -0.004(3) C60 0.092(5) 0.049(4) 0.089(5) 0.006(3) 0.023(4) -0.012(3) C61 0.127(6) 0.053(4) 0.130(6) -0.003(4) 0.025(5) -0.027(4) C62 0.110(5) 0.044(4) 0.089(5) -0.006(3) 0.016(4) -0.009(3) C63 0.066(3) 0.054(4) 0.062(4) 0.000(3) -0.006(3) 0.005(3) C64 0.040(3) 0.046(3) 0.061(3) 0.009(3) -0.005(3) -0.006(2) C65 0.056(3) 0.045(3) 0.080(4) 0.005(3) -0.010(3) -0.012(3) C66 0.034(3) 0.073(4) 0.064(4) 0.000(3) -0.001(2) -0.004(3) C67 0.036(3) 0.053(3) 0.060(3) -0.006(3) -0.008(2) -0.002(2) C68 0.038(3) 0.052(3) 0.064(3) -0.006(3) -0.006(3) 0.001(2) C69 0.048(3) 0.062(4) 0.073(4) -0.008(3) -0.004(3) 0.001(3) C70 0.034(3) 0.058(4) 0.094(5) -0.021(3) -0.002(3) 0.007(3) C71 0.045(3) 0.059(4) 0.097(5) -0.016(3) -0.009(3) 0.003(3) C72 0.035(3) 0.078(4) 0.095(5) -0.008(3) -0.003(3) -0.003(3) C73 0.039(3) 0.077(4) 0.105(5) -0.009(4) -0.007(3) -0.011(3) C74 0.051(3) 0.065(4) 0.125(6) -0.011(4) 0.000(4) -0.014(3) C75 0.044(3) 0.066(4) 0.142(6) -0.013(4) -0.007(4) 0.003(3) C76 0.045(3) 0.053(4) 0.126(5) -0.027(3) -0.012(3) -0.005(3) C77 0.052(4) 0.045(3) 0.112(5) 0.008(3) -0.012(3) -0.004(3) C78 0.045(3) 0.039(3) 0.087(4) -0.001(3) -0.008(3) -0.002(2) C79 0.044(3) 0.075(4) 0.146(6) -0.036(4) -0.014(4) -0.005(3) C80 0.055(4) 0.063(4) 0.159(7) -0.047(4) -0.014(4) -0.004(3) C81 0.046(3) 0.048(3) 0.070(4) 0.005(3) -0.003(3) -0.005(2) C82 0.046(3) 0.055(3) 0.095(4) -0.017(3) -0.015(3) -0.006(3) C83 0.048(3) 0.062(4) 0.103(5) -0.028(3) -0.020(3) 0.000(3) C84 0.045(3) 0.058(4) 0.101(5) -0.011(3) 0.006(3) -0.007(3) C85 0.117(7) 0.154(8) 0.141(8) 0.055(6) 0.069(6) 0.053(6) C86 0.062(4) 0.085(5) 0.139(6) 0.021(4) 0.006(4) 0.021(3) _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 Fe1 N1 1.939(4) . ? Fe1 N8 1.949(4) . ? Fe1 N2 1.949(4) . ? Fe1 N7 1.961(4) . ? Fe1 N14 1.965(4) . ? Fe1 N13 1.980(5) . ? S1 O3 1.465(3) . ? S1 O2 1.469(4) . ? S1 O4 1.470(4) . ? S1 O1 1.478(3) . ? N1 C5 1.339(7) . ? N1 C1 1.365(7) . ? C1 C2 1.372(7) . ? C1 C6 1.493(8) . ? N2 C6 1.335(6) . ? N2 C10 1.370(6) . ? C2 C3 1.383(9) . ? N3 C29 1.385(8) . ? N3 C11 1.404(7) . ? C3 C4 1.387(9) . ? N4 C29 1.344(8) . ? N4 C12 1.376(8) . ? C4 C5 1.396(8) . ? O5 C70 1.213(6) . ? N5 C18 1.294(14) . ? N5 C17 1.428(8) . ? O6 C77 1.219(7) . ? N6 C18 1.356(14) . ? N6 C19 1.383(13) . ? C6 C7 1.399(8) . ? O7 C41 1.245(7) . ? N7 C59 1.334(6) . ? N7 C63 1.340(6) . ? C7 C8 1.354(8) . ? O8 C48 1.232(6) . ? N8 C68 1.352(6) . ? N8 C64 1.362(6) . ? C8 C9 1.385(8) . ? O9 C29 1.219(7) . ? N9 C70 1.363(7) . ? N9 C69 1.464(7) . ? C9 C10 1.372(7) . ? C9 C11 1.518(8) . ? O10 C18 1.442(14) . ? N10 C71 1.383(7) . ? N10 C70 1.387(7) . ? N11 C77 1.392(7) . ? N11 C76 1.407(6) . ? N12 C77 1.372(7) . ? N12 C78 1.419(6) . ? C12 C13 1.388(9) . ? C12 C17 1.419(9) . ? N13 C34 1.345(7) . ? N13 C30 1.347(8) . ? C13 C14 1.358(11) . ? N14 C39 1.339(6) . ? N14 C35 1.364(6) . ? C14 C15 1.423(11) . ? N15 C41 1.377(8) . ? N15 C40 1.459(7) . ? C15 C16 1.380(10) . ? N16 C41 1.334(7) . ? N16 C42 1.434(7) . ? C16 C17 1.379(10) . ? N17 C48 1.364(6) . ? N17 C47 1.401(6) . ? N18 C48 1.353(7) . ? N18 C49 1.414(6) . ? C19 C24 1.306(13) . ? C19 C20 1.592(15) . ? C20 C21 1.528(16) . ? C21 C22 1.484(16) . ? C22 C23 1.338(12) . ? C22 C25 1.589(13) . ? C23 C24 1.475(12) . ? C25 C28 1.410(14) . ? C25 C26 1.440(13) . ? C25 C27 1.469(15) . ? C30 C31 1.395(8) . ? C30 C35 1.459(8) . ? C31 C32 1.383(12) . ? C32 C33 1.322(13) . ? C33 C34 1.384(12) . ? C35 C36 1.366(8) . ? C36 C37 1.375(9) . ? C37 C38 1.382(8) . ? C38 C39 1.402(7) . ? C38 C40 1.481(8) . ? C42 C43 1.380(7) . ? C42 C47 1.391(7) . ? C43 C44 1.376(8) . ? C44 C45 1.381(9) . ? C45 C46 1.388(8) . ? C46 C47 1.421(7) . ? C49 C54 1.364(7) . ? C49 C50 1.398(7) . ? C50 C51 1.378(8) . ? C51 C52 1.394(8) . ? C52 C53 1.389(8) . ? C52 C55 1.515(8) . ? C53 C54 1.376(7) . ? C55 C57 1.457(12) . ? C55 C58 1.476(10) . ? C55 C56 1.568(11) . ? C59 C60 1.385(8) . ? C59 C64 1.478(7) . ? C60 C61 1.376(9) . ? C61 C62 1.366(9) . ? C62 C63 1.367(8) . ? C64 C65 1.381(7) . ? C65 C66 1.387(7) . ? C66 C67 1.360(7) . ? C67 C68 1.389(7) . ? C67 C69 1.502(7) . ? C71 C72 1.398(7) . ? C71 C76 1.406(7) . ? C72 C73 1.380(8) . ? C73 C74 1.386(8) . ? C74 C75 1.358(8) . ? C75 C76 1.394(8) . ? C78 C83 1.345(7) . ? C78 C79 1.384(8) . ? C79 C80 1.367(8) . ? C80 C81 1.388(7) . ? C81 C82 1.363(7) . ? C81 C84 1.530(7) . ? C82 C83 1.387(7) . ? C84 C85 1.480(10) . ? C84 C86 1.502(8) . ? C84 C87 1.523(12) . ? 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 N1 Fe1 N8 91.61(17) . . ? N1 Fe1 N2 81.46(19) . . ? N8 Fe1 N2 94.65(17) . . ? N1 Fe1 N7 97.44(18) . . ? N8 Fe1 N7 81.45(18) . . ? N2 Fe1 N7 175.93(19) . . ? N1 Fe1 N14 172.06(19) . . ? N8 Fe1 N14 95.20(16) . . ? N2 Fe1 N14 93.90(17) . . ? N7 Fe1 N14 87.63(16) . . ? N1 Fe1 N13 92.2(2) . . ? N8 Fe1 N13 174.21(19) . . ? N2 Fe1 N13 90.25(18) . . ? N7 Fe1 N13 93.71(19) . . ? N14 Fe1 N13 81.4(2) . . ? O3 S1 O2 110.0(2) . . ? O3 S1 O4 108.6(2) . . ? O2 S1 O4 109.2(2) . . ? O3 S1 O1 109.8(2) . . ? O2 S1 O1 109.6(2) . . ? O4 S1 O1 109.6(2) . . ? C5 N1 C1 118.1(5) . . ? C5 N1 Fe1 126.3(4) . . ? C1 N1 Fe1 115.5(4) . . ? N1 C1 C2 122.8(6) . . ? N1 C1 C6 112.4(4) . . ? C2 C1 C6 124.8(6) . . ? C6 N2 C10 116.7(5) . . ? C6 N2 Fe1 116.1(4) . . ? C10 N2 Fe1 127.2(4) . . ? C1 C2 C3 118.7(6) . . ? C29 N3 C11 120.8(5) . . ? C2 C3 C4 119.3(6) . . ? C29 N4 C12 126.3(6) . . ? C3 C4 C5 119.0(6) . . ? C18 N5 C17 128.8(8) . . ? N1 C5 C4 121.9(6) . . ? C18 N6 C19 126.4(10) . . ? N2 C6 C7 121.9(5) . . ? N2 C6 C1 113.1(5) . . ? C7 C6 C1 124.8(5) . . ? C59 N7 C63 116.8(5) . . ? C59 N7 Fe1 115.3(3) . . ? C63 N7 Fe1 127.6(4) . . ? C8 C7 C6 119.7(6) . . ? C68 N8 C64 118.2(4) . . ? C68 N8 Fe1 126.6(4) . . ? C64 N8 Fe1 115.1(3) . . ? C7 C8 C9 120.1(6) . . ? C70 N9 C69 120.3(5) . . ? C10 C9 C8 117.1(5) . . ? C10 C9 C11 121.5(5) . . ? C8 C9 C11 121.4(5) . . ? C71 N10 C70 126.5(5) . . ? N2 C10 C9 124.2(5) . . ? C77 N11 C76 123.4(5) . . ? N3 C11 C9 115.6(5) . . ? C77 N12 C78 126.5(5) . . ? N4 C12 C13 124.7(6) . . ? N4 C12 C17 118.9(6) . . ? C13 C12 C17 116.2(7) . . ? C34 N13 C30 118.7(6) . . ? C34 N13 Fe1 127.1(5) . . ? C30 N13 Fe1 114.2(4) . . ? C14 C13 C12 123.9(7) . . ? C39 N14 C35 117.1(5) . . ? C39 N14 Fe1 127.0(4) . . ? C35 N14 Fe1 115.9(4) . . ? C13 C14 C15 119.8(7) . . ? C41 N15 C40 121.1(5) . . ? C16 C15 C14 117.0(8) . . ? C41 N16 C42 125.6(5) . . ? C17 C16 C15 122.8(8) . . ? C48 N17 C47 126.8(5) . . ? C16 C17 C12 120.1(6) . . ? C16 C17 N5 122.4(6) . . ? C12 C17 N5 117.3(7) . . ? C48 N18 C49 126.1(4) . . ? N5 C18 N6 118.4(12) . . ? N5 C18 O10 115.7(12) . . ? N6 C18 O10 125.9(12) . . ? C24 C19 N6 116.8(11) . . ? C24 C19 C20 124.3(11) . . ? N6 C19 C20 118.8(11) . . ? C21 C20 C19 102.9(11) . . ? C22 C21 C20 129.2(12) . . ? C23 C22 C21 115.3(10) . . ? C23 C22 C25 118.6(12) . . ? C21 C22 C25 121.8(11) . . ? C22 C23 C24 116.3(10) . . ? C19 C24 C23 125.7(9) . . ? C28 C25 C26 119.5(13) . . ? C28 C25 C27 103.4(11) . . ? C26 C25 C27 102.3(11) . . ? C28 C25 C22 114.8(9) . . ? C26 C25 C22 107.2(8) . . ? C27 C25 C22 108.3(12) . . ? O9 C29 N4 126.3(8) . . ? O9 C29 N3 120.4(7) . . ? N4 C29 N3 113.3(6) . . ? N13 C30 C31 120.6(7) . . ? N13 C30 C35 115.8(5) . . ? C31 C30 C35 123.5(7) . . ? C32 C31 C30 119.1(9) . . ? C33 C32 C31 119.3(9) . . ? C32 C33 C34 120.4(9) . . ? N13 C34 C33 121.4(8) . . ? N14 C35 C36 121.7(5) . . ? N14 C35 C30 112.6(5) . . ? C36 C35 C30 125.6(6) . . ? C35 C36 C37 120.5(6) . . ? C36 C37 C38 119.6(6) . . ? C37 C38 C39 116.7(5) . . ? C37 C38 C40 121.4(5) . . ? C39 C38 C40 121.8(5) . . ? N14 C39 C38 124.3(5) . . ? N15 C40 C38 113.4(5) . . ? O7 C41 N16 124.1(7) . . ? O7 C41 N15 122.3(6) . . ? N16 C41 N15 113.5(6) . . ? C43 C42 C47 121.2(6) . . ? C43 C42 N16 121.1(5) . . ? C47 C42 N16 117.6(5) . . ? C44 C43 C42 120.8(6) . . ? C43 C44 C45 119.0(6) . . ? C44 C45 C46 121.6(6) . . ? C45 C46 C47 119.2(6) . . ? C42 C47 N17 119.5(5) . . ? C42 C47 C46 118.1(5) . . ? N17 C47 C46 122.3(5) . . ? O8 C48 N18 122.1(5) . . ? O8 C48 N17 123.2(5) . . ? N18 C48 N17 114.7(5) . . ? C54 C49 C50 117.9(5) . . ? C54 C49 N18 125.4(5) . . ? C50 C49 N18 116.7(5) . . ? C51 C50 C49 120.4(5) . . ? C50 C51 C52 122.8(6) . . ? C53 C52 C51 114.7(5) . . ? C53 C52 C55 125.2(5) . . ? C51 C52 C55 120.2(5) . . ? C54 C53 C52 123.5(5) . . ? C49 C54 C53 120.8(5) . . ? C57 C55 C58 117.0(8) . . ? C57 C55 C52 111.3(7) . . ? C58 C55 C52 112.0(6) . . ? C57 C55 C56 103.4(7) . . ? C58 C55 C56 104.0(8) . . ? C52 C55 C56 108.0(6) . . ? N7 C59 C60 123.2(5) . . ? N7 C59 C64 113.9(5) . . ? C60 C59 C64 122.9(5) . . ? C61 C60 C59 118.2(6) . . ? C62 C61 C60 119.4(6) . . ? C61 C62 C63 118.6(6) . . ? N7 C63 C62 123.8(6) . . ? N8 C64 C65 120.6(5) . . ? N8 C64 C59 113.0(4) . . ? C65 C64 C59 126.4(5) . . ? C64 C65 C66 119.7(5) . . ? C67 C66 C65 120.5(5) . . ? C66 C67 C68 117.4(5) . . ? C66 C67 C69 123.1(5) . . ? C68 C67 C69 119.5(5) . . ? N8 C68 C67 123.4(5) . . ? N9 C69 C67 111.9(4) . . ? O5 C70 N9 124.7(6) . . ? O5 C70 N10 123.0(6) . . ? N9 C70 N10 112.4(5) . . ? N10 C71 C72 121.7(5) . . ? N10 C71 C76 119.9(5) . . ? C72 C71 C76 118.3(5) . . ? C73 C72 C71 121.4(5) . . ? C72 C73 C74 119.5(5) . . ? C75 C74 C73 119.9(6) . . ? C74 C75 C76 121.9(6) . . ? C75 C76 C71 118.9(5) . . ? C75 C76 N11 121.6(5) . . ? C71 C76 N11 119.5(5) . . ? O6 C77 N12 124.8(5) . . ? O6 C77 N11 123.1(5) . . ? N12 C77 N11 112.0(6) . . ? C83 C78 C79 117.3(5) . . ? C83 C78 N12 118.2(5) . . ? C79 C78 N12 124.5(5) . . ? C80 C79 C78 120.4(5) . . ? C79 C80 C81 123.0(6) . . ? C82 C81 C80 115.0(5) . . ? C82 C81 C84 125.0(5) . . ? C80 C81 C84 120.1(5) . . ? C81 C82 C83 122.4(5) . . ? C78 C83 C82 121.8(5) . . ? C85 C84 C86 105.8(6) . . ? C85 C84 C87 114.8(7) . . ? C86 C84 C87 105.2(6) . . ? C85 C84 C81 109.9(5) . . ? C86 C84 C81 111.9(5) . . ? C87 C84 C81 109.1(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.143 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.078