# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jonathan White' _publ_contact_author_email whitejm@unimelb.edu.au loop_ _publ_author_name 'Paul Donnelly' 'Brett Patterson' 'Jonathan White' data_jmwpd87 _database_code_depnum_ccdc_archive 'CCDC 745070' #TrackingRef 'jmwpd87.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H58 B Cl2 N8 Re S2' _chemical_formula_weight 1031.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.62030(10) _cell_length_b 20.2158(2) _cell_length_c 19.8643(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.6900(10) _cell_angle_gamma 90.00 _cell_volume 4624.43(8) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9683 _cell_measurement_theta_min 4.1733 _cell_measurement_theta_max 73.0960 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.2895 _exptl_crystal_size_mid 0.1520 _exptl_crystal_size_min 0.0140 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 7.356 _exptl_absorpt_correction_T_min 0.238 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini-S CCD-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16886 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 67.48 _reflns_number_total 8134 _reflns_number_gt 6606 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+71.5720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8134 _refine_ls_number_parameters 552 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.74808(3) 0.219080(18) 0.808424(18) 0.01791(11) Uani 1 1 d . . . S2 S 0.59098(17) 0.28866(10) 0.82122(11) 0.0229(4) Uani 1 1 d . . . S1 S 0.88687(18) 0.20681(10) 0.73448(10) 0.0231(4) Uani 1 1 d . . . N5 N 0.8638(7) 0.2107(4) 0.8877(3) 0.0281(17) Uani 1 1 d . . . N3 N 0.6559(6) 0.1988(3) 0.7106(3) 0.0212(15) Uani 1 1 d . . . C11 C 0.6490(7) 0.3646(4) 0.7962(4) 0.0200(18) Uani 1 1 d . . . N4 N 0.6570(6) 0.1434(3) 0.8226(4) 0.0263(17) Uani 1 1 d . . . N2 N 0.6870(6) 0.2208(4) 0.6490(3) 0.0206(14) Uani 1 1 d . . . N6 N 0.8177(6) 0.3161(4) 0.8246(4) 0.0240(16) Uani 1 1 d . . . C22 C 0.8599(8) 0.4007(4) 0.6339(5) 0.030(2) Uani 1 1 d . . . H22 H 0.7993 0.3958 0.6597 0.036 Uiso 1 1 calc R . . N7 N 0.7617(6) 0.3742(3) 0.7980(4) 0.0238(16) Uani 1 1 d . . . C4 C 0.5623(7) 0.1619(4) 0.7091(4) 0.0211(18) Uani 1 1 d . . . N8 N 0.5734(7) 0.4128(4) 0.7784(4) 0.0260(18) Uani 1 1 d . . . C37 C 1.2965(8) 0.3481(5) 0.7874(4) 0.028(2) Uani 1 1 d . . . H37 H 1.3218 0.3061 0.7770 0.033 Uiso 1 1 calc R . . N1 N 0.8567(6) 0.2353(4) 0.6031(4) 0.0223(16) Uani 1 1 d . . . C18 C 0.9725(8) 0.2803(6) 0.9771(4) 0.034(2) Uani 1 1 d . . . H18A H 0.9969 0.2423 1.0043 0.052 Uiso 1 1 calc R . . H18B H 0.8999 0.2962 0.9889 0.052 Uiso 1 1 calc R . . H18C H 1.0301 0.3145 0.9853 0.052 Uiso 1 1 calc R . . C30 C 1.4049(9) 0.4863(5) 0.5799(5) 0.036(2) Uani 1 1 d . . . H30 H 1.4031 0.5300 0.5654 0.043 Uiso 1 1 calc R . . C9 C 0.9574(7) 0.2611(5) 0.9015(4) 0.025(2) Uani 1 1 d . . . C10 C 0.9163(7) 0.3215(5) 0.8607(4) 0.0236(19) Uani 1 1 d . . . C3 C 0.7989(7) 0.2238(4) 0.6556(4) 0.0209(17) Uani 1 1 d . . . C6 C 0.6733(10) 0.1084(5) 0.8887(5) 0.043(3) Uani 1 1 d . . . H6A H 0.6394 0.1343 0.9221 0.052 Uiso 1 1 calc R . . H6B H 0.6333 0.0662 0.8840 0.052 Uiso 1 1 calc R . . C33 C 1.1954(7) 0.4475(4) 0.7564(4) 0.0230(19) Uani 1 1 d . . . H33 H 1.1498 0.4736 0.7248 0.028 Uiso 1 1 calc R . . C5 C 0.5545(7) 0.1244(4) 0.7742(5) 0.0249(19) Uani 1 1 d . . . C25 C 1.0408(8) 0.4144(4) 0.5590(5) 0.0257(19) Uani 1 1 d . . . H25 H 1.1008 0.4194 0.5328 0.031 Uiso 1 1 calc R . . C32 C 1.2258(7) 0.3839(4) 0.7371(4) 0.0213(18) Uani 1 1 d . . . C2 C 0.7972(7) 0.2496(5) 0.5353(4) 0.0247(19) Uani 1 1 d . . . H2A H 0.7500 0.2890 0.5367 0.030 Uiso 1 1 calc R . . H2B H 0.7463 0.2131 0.5198 0.030 Uiso 1 1 calc R . . C21 C 0.9723(7) 0.3831(4) 0.6612(4) 0.0207(18) Uani 1 1 d . . . H21 H 0.9849 0.3666 0.7053 0.025 Uiso 1 1 calc R . . C41 C 1.1535(8) 0.1450(4) 0.6080(5) 0.034(2) Uani 1 1 d . . . H41 H 1.1434 0.1005 0.5967 0.040 Uiso 1 1 calc R . . C20 C 1.0664(7) 0.3893(4) 0.6252(4) 0.0183(17) Uani 1 1 d . . . C13 C 0.5079(8) 0.5253(4) 0.7548(5) 0.034(2) Uani 1 1 d . . . H13A H 0.5317 0.5684 0.7417 0.050 Uiso 1 1 calc R . . H13B H 0.4829 0.5278 0.7989 0.050 Uiso 1 1 calc R . . H13C H 0.4450 0.5099 0.7223 0.050 Uiso 1 1 calc R . . C40 C 1.1506(8) 0.1656(4) 0.6730(5) 0.034(2) Uani 1 1 d . . . H40 H 1.1381 0.1350 0.7063 0.040 Uiso 1 1 calc R . . C14 C 0.4785(8) 0.1516(5) 0.6463(5) 0.032(2) Uani 1 1 d . . . H14A H 0.4975 0.1807 0.6113 0.048 Uiso 1 1 calc R . . H14B H 0.4013 0.1609 0.6557 0.048 Uiso 1 1 calc R . . H14C H 0.4829 0.1066 0.6316 0.048 Uiso 1 1 calc R . . C38 C 1.1868(7) 0.2812(4) 0.6431(4) 0.0243(18) Uani 1 1 d . . . C39 C 1.1662(8) 0.2329(4) 0.6902(5) 0.028(2) Uani 1 1 d . . . H39 H 1.1627 0.2457 0.7349 0.034 Uiso 1 1 calc R . . C24 C 0.9287(9) 0.4321(4) 0.5313(5) 0.036(2) Uani 1 1 d . . . H24 H 0.9151 0.4486 0.4873 0.043 Uiso 1 1 calc R . . C17 C 1.0731(8) 0.2340(5) 0.8831(5) 0.037(2) Uani 1 1 d . . . H17A H 1.0948 0.1952 0.9097 0.055 Uiso 1 1 calc R . . H17B H 1.1323 0.2671 0.8924 0.055 Uiso 1 1 calc R . . H17C H 1.0641 0.2228 0.8357 0.055 Uiso 1 1 calc R . . C28 C 1.5060(8) 0.3848(6) 0.6013(5) 0.035(2) Uani 1 1 d . . . H28 H 1.5732 0.3597 0.6019 0.043 Uiso 1 1 calc R . . C29 C 1.5040(9) 0.4495(6) 0.5795(5) 0.040(3) Uani 1 1 d . . . H29 H 1.5693 0.4680 0.5645 0.049 Uiso 1 1 calc R . . C26 C 1.3039(7) 0.3927(4) 0.6227(4) 0.0218(18) Uani 1 1 d . . . C27 C 1.4080(8) 0.3572(5) 0.6225(4) 0.026(2) Uani 1 1 d . . . H27 H 1.4110 0.3135 0.6371 0.032 Uiso 1 1 calc R . . C31 C 1.3081(8) 0.4587(5) 0.6019(4) 0.028(2) Uani 1 1 d . . . H31 H 1.2427 0.4850 0.6029 0.033 Uiso 1 1 calc R . . C1 C 0.8840(8) 0.2600(5) 0.4866(5) 0.031(2) Uani 1 1 d . . . H1A H 0.8438 0.2684 0.4420 0.047 Uiso 1 1 calc R . . H1B H 0.9311 0.2211 0.4855 0.047 Uiso 1 1 calc R . . H1C H 0.9325 0.2971 0.5011 0.047 Uiso 1 1 calc R . . C8 C 0.8722(9) 0.1540(5) 0.9336(5) 0.036(2) Uani 1 1 d . . . H8A H 0.8550 0.1690 0.9776 0.044 Uiso 1 1 calc R . . H8B H 0.9519 0.1385 0.9396 0.044 Uiso 1 1 calc R . . C19 C 0.9847(9) 0.3849(5) 0.8681(5) 0.039(2) Uani 1 1 d . . . H19A H 0.9464 0.4177 0.8381 0.058 Uiso 1 1 calc R . . H19B H 1.0613 0.3772 0.8567 0.058 Uiso 1 1 calc R . . H19C H 0.9899 0.4002 0.9142 0.058 Uiso 1 1 calc R . . C16 C 0.5653(8) 0.0505(5) 0.7550(5) 0.035(2) Uani 1 1 d . . . H16A H 0.5607 0.0235 0.7943 0.053 Uiso 1 1 calc R . . H16B H 0.6386 0.0433 0.7389 0.053 Uiso 1 1 calc R . . H16C H 0.5034 0.0391 0.7200 0.053 Uiso 1 1 calc R . . C43 C 1.1880(7) 0.2573(4) 0.5767(5) 0.026(2) Uani 1 1 d . . . H43 H 1.2003 0.2874 0.5430 0.032 Uiso 1 1 calc R . . C12 C 0.6083(8) 0.4782(4) 0.7572(5) 0.026(2) Uani 1 1 d . . . H12A H 0.6334 0.4753 0.7126 0.031 Uiso 1 1 calc R . . H12B H 0.6729 0.4944 0.7889 0.031 Uiso 1 1 calc R . . C36 C 1.3294(8) 0.3733(5) 0.8518(5) 0.031(2) Uani 1 1 d . . . H36 H 1.3739 0.3475 0.8841 0.038 Uiso 1 1 calc R . . C35 C 1.2975(9) 0.4362(5) 0.8689(5) 0.034(2) Uani 1 1 d . . . H35 H 1.3208 0.4532 0.9121 0.041 Uiso 1 1 calc R . . C42 C 1.1719(8) 0.1911(5) 0.5587(5) 0.032(2) Uani 1 1 d . . . H42 H 1.1734 0.1778 0.5140 0.039 Uiso 1 1 calc R . . C7 C 0.7959(9) 0.0974(5) 0.9123(5) 0.041(3) Uani 1 1 d . . . H7A H 0.8286 0.0748 0.8762 0.049 Uiso 1 1 calc R . . H7B H 0.8006 0.0670 0.9503 0.049 Uiso 1 1 calc R . . C23 C 0.8379(8) 0.4253(4) 0.5687(5) 0.033(2) Uani 1 1 d . . . H23 H 0.7629 0.4370 0.5503 0.040 Uiso 1 1 calc R . . C34 C 1.2302(8) 0.4732(5) 0.8205(5) 0.030(2) Uani 1 1 d . . . H34 H 1.2080 0.5158 0.8310 0.036 Uiso 1 1 calc R . . C15 C 0.4404(8) 0.1366(5) 0.8029(5) 0.035(2) Uani 1 1 d . . . H15A H 0.4393 0.1107 0.8434 0.052 Uiso 1 1 calc R . . H15B H 0.3762 0.1240 0.7698 0.052 Uiso 1 1 calc R . . H15C H 0.4341 0.1826 0.8137 0.052 Uiso 1 1 calc R . . B B 1.1958(8) 0.3611(5) 0.6575(5) 0.020(2) Uani 1 1 d . . . C44 C 0.7351(18) 0.4842(11) 0.9436(12) 0.069(9) Uani 0.486(8) 1 d PD A 1 H44A H 0.7488 0.4555 0.9064 0.082 Uiso 0.486(8) 1 calc PR A 1 H44B H 0.7732 0.4652 0.9856 0.082 Uiso 0.486(8) 1 calc PR A 1 Cl2 Cl 0.7912(12) 0.5641(6) 0.9317(9) 0.108(5) Uani 0.486(8) 1 d PD A 1 Cl1 Cl 0.5881(9) 0.4917(5) 0.9467(4) 0.102(4) Uani 0.486(8) 1 d PD A 1 C44' C 0.827(3) 0.537(3) 0.953(4) 0.29(6) Uiso 0.514(8) 1 d PD A 2 H44C H 0.8641 0.5295 0.9127 0.349 Uiso 0.514(8) 1 calc PR A 2 H44D H 0.8688 0.5726 0.9784 0.349 Uiso 0.514(8) 1 calc PR A 2 Cl1' Cl 0.6856(16) 0.5639(4) 0.9270(5) 0.153(8) Uani 0.514(8) 1 d PD A 2 Cl2' Cl 0.8415(9) 0.4660(4) 1.0023(4) 0.099(4) Uani 0.514(8) 1 d PD A 2 H H 0.515(9) 0.407(6) 0.774(6) 0.040 Uiso 1 1 d . . . H' H 0.918(9) 0.242(6) 0.608(6) 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01711(19) 0.01792(18) 0.01865(18) 0.00426(16) 0.00215(13) 0.00143(16) S2 0.0185(10) 0.0195(10) 0.0317(11) 0.0034(9) 0.0065(8) -0.0002(8) S1 0.0246(11) 0.0234(11) 0.0213(10) 0.0026(8) 0.0032(8) 0.0032(8) N5 0.039(5) 0.030(4) 0.015(3) 0.007(3) 0.003(3) 0.004(4) N3 0.032(4) 0.016(3) 0.016(3) 0.003(3) 0.003(3) 0.006(3) C11 0.024(5) 0.018(4) 0.019(4) -0.003(3) 0.005(3) 0.000(3) N4 0.029(4) 0.021(4) 0.029(4) 0.012(3) 0.002(3) 0.001(3) N2 0.013(3) 0.025(4) 0.023(3) 0.002(3) 0.002(3) -0.003(3) N6 0.026(4) 0.024(4) 0.022(4) 0.001(3) 0.005(3) -0.002(3) C22 0.025(5) 0.024(5) 0.044(6) -0.009(4) 0.009(4) -0.001(4) N7 0.027(4) 0.019(3) 0.025(4) 0.001(3) 0.005(3) -0.003(3) C4 0.018(4) 0.017(4) 0.028(4) 0.001(3) 0.001(3) -0.002(3) N8 0.023(4) 0.022(4) 0.033(4) 0.002(3) 0.004(4) -0.003(3) C37 0.031(5) 0.025(5) 0.029(5) 0.004(4) 0.011(4) 0.002(4) N1 0.009(3) 0.031(4) 0.026(4) -0.003(3) 0.001(3) -0.004(3) C18 0.028(5) 0.053(6) 0.022(5) 0.005(5) 0.001(4) 0.004(5) C30 0.048(7) 0.037(5) 0.023(5) 0.000(4) 0.003(4) -0.022(5) C9 0.012(4) 0.039(5) 0.023(4) 0.000(4) -0.004(3) -0.007(4) C10 0.008(4) 0.040(5) 0.022(4) -0.003(4) 0.001(3) -0.001(4) C3 0.034(5) 0.014(4) 0.014(4) 0.000(3) 0.002(3) 0.003(4) C6 0.049(7) 0.041(6) 0.038(6) 0.024(5) 0.004(5) -0.002(5) C33 0.013(4) 0.025(4) 0.030(5) -0.001(4) 0.001(4) 0.001(3) C5 0.012(4) 0.025(4) 0.037(5) 0.009(4) 0.000(4) 0.000(3) C25 0.025(5) 0.020(4) 0.032(5) 0.000(4) 0.002(4) -0.002(4) C32 0.024(5) 0.017(4) 0.024(4) 0.004(3) 0.010(4) -0.002(3) C2 0.008(4) 0.039(5) 0.026(5) 0.000(4) -0.006(3) -0.003(4) C21 0.010(4) 0.022(4) 0.029(5) -0.002(4) -0.001(3) -0.005(3) C41 0.019(5) 0.018(4) 0.062(7) -0.011(4) 0.000(4) -0.002(4) C20 0.015(4) 0.013(4) 0.025(4) -0.002(3) -0.004(3) -0.002(3) C13 0.036(6) 0.020(5) 0.044(6) 0.002(4) 0.005(5) 0.000(4) C40 0.029(5) 0.018(4) 0.055(6) 0.009(4) 0.010(5) -0.002(4) C14 0.026(5) 0.032(5) 0.037(5) 0.003(4) 0.000(4) -0.007(4) C38 0.019(4) 0.020(4) 0.034(5) 0.000(4) 0.006(4) 0.005(4) C39 0.025(5) 0.024(5) 0.038(5) 0.001(4) 0.013(4) -0.001(4) C24 0.047(6) 0.020(5) 0.035(5) 0.003(4) -0.010(5) -0.003(4) C17 0.032(5) 0.050(7) 0.028(5) 0.000(5) 0.004(4) -0.002(5) C28 0.023(5) 0.056(7) 0.029(5) -0.018(5) 0.009(4) -0.008(5) C29 0.030(6) 0.064(7) 0.029(5) -0.010(5) 0.010(4) -0.029(5) C26 0.022(5) 0.027(4) 0.017(4) -0.003(3) 0.003(3) -0.006(4) C27 0.030(5) 0.028(5) 0.022(4) -0.006(4) 0.008(4) -0.002(4) C31 0.033(5) 0.027(5) 0.023(4) -0.003(4) 0.004(4) -0.008(4) C1 0.021(5) 0.045(6) 0.027(5) -0.002(4) 0.000(4) -0.006(4) C8 0.029(5) 0.046(6) 0.033(5) 0.018(5) 0.002(4) 0.006(5) C19 0.033(6) 0.044(6) 0.037(6) -0.002(5) -0.007(4) -0.015(5) C16 0.025(5) 0.026(5) 0.054(6) 0.010(5) 0.005(5) -0.004(4) C43 0.020(5) 0.024(4) 0.034(5) 0.003(4) -0.002(4) -0.001(4) C12 0.036(5) 0.014(4) 0.028(5) 0.000(4) 0.005(4) -0.003(4) C36 0.023(5) 0.048(6) 0.024(5) 0.010(4) 0.003(4) 0.005(4) C35 0.034(6) 0.047(6) 0.022(5) -0.009(4) 0.009(4) -0.005(5) C42 0.020(5) 0.028(5) 0.049(6) -0.010(4) 0.001(4) 0.000(4) C7 0.043(6) 0.040(6) 0.036(6) 0.019(5) -0.007(5) -0.003(5) C23 0.023(5) 0.022(5) 0.051(6) -0.003(4) -0.004(4) 0.005(4) C34 0.032(5) 0.024(5) 0.036(5) -0.007(4) 0.011(4) 0.000(4) C15 0.036(6) 0.032(5) 0.037(6) 0.008(4) 0.007(4) 0.000(4) B 0.019(5) 0.019(5) 0.022(5) 0.003(4) 0.004(4) 0.002(4) C44 0.13(3) 0.041(14) 0.032(13) -0.012(11) -0.011(15) -0.001(16) Cl2 0.117(8) 0.066(6) 0.158(11) -0.037(6) 0.083(8) -0.045(6) Cl1 0.132(9) 0.109(7) 0.057(5) -0.001(5) -0.010(5) -0.061(6) Cl1' 0.32(2) 0.050(5) 0.068(6) -0.005(4) -0.060(9) 0.016(9) Cl2' 0.149(9) 0.096(6) 0.057(4) -0.005(4) 0.028(5) 0.048(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 Re1 N4 1.902(7) . ? Re1 N5 1.936(7) . ? Re1 N6 2.129(7) . ? Re1 N3 2.129(7) . ? Re1 S1 2.335(2) . ? Re1 S2 2.345(2) . ? S2 C11 1.775(8) . ? S1 C3 1.786(8) . ? N5 C8 1.460(11) . ? N5 C9 1.489(11) . ? N3 C4 1.316(11) . ? N3 N2 1.393(9) . ? C11 N7 1.320(11) . ? C11 N8 1.327(11) . ? N4 C5 1.477(11) . ? N4 C6 1.483(11) . ? N2 C3 1.292(11) . ? N6 C10 1.273(11) . ? N6 N7 1.412(10) . ? C22 C23 1.378(14) . ? C22 C21 1.391(12) . ? C4 C14 1.490(12) . ? C4 C5 1.512(12) . ? N8 C12 1.462(11) . ? C37 C36 1.383(13) . ? C37 C32 1.406(12) . ? N1 C3 1.334(11) . ? N1 C2 1.458(11) . ? C18 C9 1.540(12) . ? C30 C29 1.372(15) . ? C30 C31 1.379(13) . ? C9 C10 1.507(12) . ? C9 C17 1.540(13) . ? C10 C19 1.505(13) . ? C6 C7 1.455(14) . ? C33 C34 1.385(12) . ? C33 C32 1.400(12) . ? C5 C15 1.533(13) . ? C5 C16 1.551(13) . ? C25 C24 1.391(13) . ? C25 C20 1.404(12) . ? C32 B 1.638(12) . ? C2 C1 1.503(12) . ? C21 C20 1.391(12) . ? C41 C40 1.362(14) . ? C41 C42 1.388(14) . ? C20 B 1.655(12) . ? C13 C12 1.502(12) . ? C40 C39 1.409(13) . ? C38 C39 1.396(12) . ? C38 C43 1.406(12) . ? C38 B 1.642(12) . ? C24 C23 1.377(14) . ? C28 C29 1.377(16) . ? C28 C27 1.383(13) . ? C26 C31 1.398(12) . ? C26 C27 1.407(12) . ? C26 B 1.642(12) . ? C8 C7 1.475(14) . ? C43 C42 1.393(12) . ? C36 C35 1.380(14) . ? C35 C34 1.376(14) . ? C44 Cl1 1.72(2) . ? C44 Cl2 1.768(18) . ? C44' Cl2' 1.74(2) . ? C44' Cl1' 1.74(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Re1 N5 98.6(3) . . ? N4 Re1 N6 157.8(3) . . ? N5 Re1 N6 75.5(3) . . ? N4 Re1 N3 76.0(3) . . ? N5 Re1 N3 159.2(3) . . ? N6 Re1 N3 116.7(3) . . ? N4 Re1 S1 116.9(2) . . ? N5 Re1 S1 92.2(2) . . ? N6 Re1 S1 85.0(2) . . ? N3 Re1 S1 73.2(2) . . ? N4 Re1 S2 90.5(2) . . ? N5 Re1 S2 115.5(2) . . ? N6 Re1 S2 73.6(2) . . ? N3 Re1 S2 84.87(19) . . ? S1 Re1 S2 138.16(7) . . ? C11 S2 Re1 99.1(3) . . ? C3 S1 Re1 99.7(3) . . ? C8 N5 C9 115.8(7) . . ? C8 N5 Re1 123.9(6) . . ? C9 N5 Re1 120.0(5) . . ? C4 N3 N2 118.1(7) . . ? C4 N3 Re1 116.3(5) . . ? N2 N3 Re1 125.6(5) . . ? N7 C11 N8 121.2(8) . . ? N7 C11 S2 122.2(6) . . ? N8 C11 S2 116.5(6) . . ? C5 N4 C6 116.6(7) . . ? C5 N4 Re1 121.9(5) . . ? C6 N4 Re1 120.5(6) . . ? C3 N2 N3 107.6(6) . . ? C10 N6 N7 118.3(7) . . ? C10 N6 Re1 117.4(6) . . ? N7 N6 Re1 124.3(5) . . ? C23 C22 C21 120.3(9) . . ? C11 N7 N6 107.1(7) . . ? N3 C4 C14 123.0(8) . . ? N3 C4 C5 114.1(7) . . ? C14 C4 C5 122.5(7) . . ? C11 N8 C12 122.7(8) . . ? C36 C37 C32 122.0(9) . . ? C3 N1 C2 122.0(7) . . ? C29 C30 C31 120.3(10) . . ? N5 C9 C10 106.5(6) . . ? N5 C9 C18 109.8(7) . . ? C10 C9 C18 107.8(8) . . ? N5 C9 C17 110.6(8) . . ? C10 C9 C17 112.6(7) . . ? C18 C9 C17 109.4(7) . . ? N6 C10 C19 123.5(9) . . ? N6 C10 C9 115.5(8) . . ? C19 C10 C9 120.8(7) . . ? N2 C3 N1 122.3(7) . . ? N2 C3 S1 122.0(6) . . ? N1 C3 S1 115.5(6) . . ? C7 C6 N4 111.2(8) . . ? C34 C33 C32 122.9(8) . . ? N4 C5 C4 106.9(7) . . ? N4 C5 C15 112.2(8) . . ? C4 C5 C15 113.1(7) . . ? N4 C5 C16 109.0(7) . . ? C4 C5 C16 104.9(8) . . ? C15 C5 C16 110.4(7) . . ? C24 C25 C20 122.3(9) . . ? C33 C32 C37 115.0(8) . . ? C33 C32 B 119.6(7) . . ? C37 C32 B 124.7(8) . . ? N1 C2 C1 110.2(7) . . ? C20 C21 C22 122.6(8) . . ? C40 C41 C42 119.3(8) . . ? C21 C20 C25 115.5(8) . . ? C21 C20 B 120.4(7) . . ? C25 C20 B 123.8(7) . . ? C41 C40 C39 120.4(9) . . ? C39 C38 C43 114.4(8) . . ? C39 C38 B 125.7(8) . . ? C43 C38 B 119.5(8) . . ? C38 C39 C40 122.7(9) . . ? C23 C24 C25 120.4(9) . . ? C29 C28 C27 120.0(10) . . ? C30 C29 C28 119.4(9) . . ? C31 C26 C27 114.9(8) . . ? C31 C26 B 123.7(8) . . ? C27 C26 B 120.6(8) . . ? C28 C27 C26 122.6(9) . . ? C30 C31 C26 122.8(9) . . ? N5 C8 C7 116.2(8) . . ? C42 C43 C38 123.5(9) . . ? N8 C12 C13 109.8(7) . . ? C35 C36 C37 121.2(9) . . ? C34 C35 C36 118.3(9) . . ? C41 C42 C43 119.5(9) . . ? C6 C7 C8 119.9(10) . . ? C24 C23 C22 118.9(9) . . ? C35 C34 C33 120.5(9) . . ? C32 B C38 116.5(7) . . ? C32 B C26 102.7(7) . . ? C38 B C26 110.1(7) . . ? C32 B C20 110.0(7) . . ? C38 B C20 103.7(7) . . ? C26 B C20 114.1(7) . . ? Cl1 C44 Cl2 108.0(16) . . ? Cl2' C44' Cl1' 116(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 67.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.071 _refine_diff_density_min -1.622 _refine_diff_density_rms 0.147 # Attachment 'jmwpd88.cif' data_jmwpd88 _database_code_depnum_ccdc_archive 'CCDC 745071' #TrackingRef 'jmwpd88.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H58 B Fe N8 S2' _chemical_formula_weight 817.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5945(5) _cell_length_b 19.6278(8) _cell_length_c 22.4474(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.472(4) _cell_angle_gamma 90.00 _cell_volume 4219.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2039 _cell_measurement_theta_min 4.5069 _cell_measurement_theta_max 73.2146 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.1488 _exptl_crystal_size_mid 0.0660 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 4.102 _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite #'Oxford Diffraction Gemini-S CCD-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18411 _diffrn_reflns_av_R_equivalents 0.1130 _diffrn_reflns_av_sigmaI/netI 0.2460 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.51 _diffrn_reflns_theta_max 73.43 _reflns_number_total 7921 _reflns_number_gt 3072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7921 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1323 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 0.623 _refine_ls_restrained_S_all 0.623 _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 C1 C -0.2988(5) 0.0784(3) 1.1074(2) 0.095(2) Uani 1 1 d . . . H1A H -0.3311 0.0901 1.1457 0.142 Uiso 1 1 calc R . . H1B H -0.3044 0.0299 1.1020 0.142 Uiso 1 1 calc R . . H1C H -0.3561 0.1006 1.0767 0.142 Uiso 1 1 calc R . . C2 C -0.1554(5) 0.1003(2) 1.10410(18) 0.0533(15) Uani 1 1 d . . . H2A H -0.0982 0.0782 1.1356 0.064 Uiso 1 1 calc R . . H2B H -0.1500 0.1491 1.1106 0.064 Uiso 1 1 calc R . . C3 C -0.0005(4) 0.1232(2) 1.02225(17) 0.0289(10) Uani 1 1 d . . . C4 C 0.1841(4) 0.26977(19) 1.03793(16) 0.0257(10) Uani 1 1 d . . . C5 C 0.2872(4) 0.3100(2) 1.00379(16) 0.0264(10) Uani 1 1 d . . . C6 C 0.3020(4) 0.31296(19) 0.88787(15) 0.0273(10) Uani 1 1 d . . . H6A H 0.3322 0.2841 0.8560 0.033 Uiso 1 1 calc R . . H6B H 0.3692 0.3497 0.8933 0.033 Uiso 1 1 calc R . . C7 C 0.1614(4) 0.34306(19) 0.86866(16) 0.0280(10) Uani 1 1 d . . . H7A H 0.1569 0.3491 0.8257 0.034 Uiso 1 1 calc R . . H7B H 0.1547 0.3878 0.8865 0.034 Uiso 1 1 calc R . . C8 C 0.0361(4) 0.30121(18) 0.88499(16) 0.0282(10) Uani 1 1 d . . . H8A H 0.0152 0.3128 0.9255 0.034 Uiso 1 1 calc R . . H8B H -0.0435 0.3149 0.8590 0.034 Uiso 1 1 calc R . . C9 C 0.0532(4) 0.1935(2) 0.81896(16) 0.0266(10) Uani 1 1 d . . . C10 C 0.1866(4) 0.1517(2) 0.81773(17) 0.0284(10) Uani 1 1 d . . . C11 C 0.4424(4) 0.0968(2) 0.91650(17) 0.0276(10) Uani 1 1 d . . . C12 C 0.6184(4) 0.0278(2) 0.86830(17) 0.0399(12) Uani 1 1 d . . . H12A H 0.6460 0.0632 0.8413 0.048 Uiso 1 1 calc R . . H12B H 0.5479 -0.0002 0.8474 0.048 Uiso 1 1 calc R . . C13 C 0.7443(4) -0.0158(2) 0.88728(16) 0.0393(12) Uani 1 1 d . . . H13A H 0.7813 -0.0361 0.8527 0.059 Uiso 1 1 calc R . . H13B H 0.7167 -0.0509 0.9139 0.059 Uiso 1 1 calc R . . H13C H 0.8146 0.0122 0.9073 0.059 Uiso 1 1 calc R . . C14 C 0.1425(4) 0.29616(19) 1.09755(15) 0.0322(11) Uani 1 1 d . . . H14A H 0.0767 0.2654 1.1137 0.048 Uiso 0.50 1 calc PR . . H14B H 0.1005 0.3403 1.0924 0.048 Uiso 0.50 1 calc PR . . H14C H 0.2238 0.2995 1.1245 0.048 Uiso 0.50 1 calc PR . . H14D H 0.1906 0.3381 1.1067 0.048 Uiso 0.50 1 calc PR . . H14E H 0.1668 0.2632 1.1280 0.048 Uiso 0.50 1 calc PR . . H14F H 0.0435 0.3040 1.0959 0.048 Uiso 0.50 1 calc PR . . C15 C 0.2383(4) 0.38530(18) 0.99753(16) 0.0374(12) Uani 1 1 d . . . H15A H 0.3042 0.4106 0.9758 0.056 Uiso 1 1 calc R . . H15B H 0.2322 0.4049 1.0365 0.056 Uiso 1 1 calc R . . H15C H 0.1483 0.3869 0.9764 0.056 Uiso 1 1 calc R . . C16 C 0.4312(4) 0.3097(2) 1.03742(15) 0.0366(11) Uani 1 1 d . . . H16A H 0.4956 0.3357 1.0155 0.055 Uiso 1 1 calc R . . H16B H 0.4641 0.2636 1.0417 0.055 Uiso 1 1 calc R . . H16C H 0.4242 0.3295 1.0762 0.055 Uiso 1 1 calc R . . C17 C 0.0518(4) 0.2463(2) 0.76658(15) 0.0364(12) Uani 1 1 d . . . H17A H -0.0315 0.2734 0.7667 0.055 Uiso 1 1 calc R . . H17B H 0.0540 0.2225 0.7293 0.055 Uiso 1 1 calc R . . H17C H 0.1322 0.2753 0.7717 0.055 Uiso 1 1 calc R . . C18 C -0.0767(4) 0.1483(2) 0.80898(16) 0.0377(11) Uani 1 1 d . . . H18A H -0.1591 0.1761 0.8085 0.057 Uiso 1 1 calc R . . H18B H -0.0790 0.1155 0.8407 0.057 Uiso 1 1 calc R . . H18C H -0.0734 0.1249 0.7715 0.057 Uiso 1 1 calc R . . C19 C 0.2227(4) 0.1178(2) 0.76074(15) 0.0398(12) Uani 1 1 d . . . H19A H 0.3092 0.0935 0.7672 0.060 Uiso 0.50 1 calc PR . . H19B H 0.2322 0.1517 0.7304 0.060 Uiso 0.50 1 calc PR . . H19C H 0.1499 0.0865 0.7481 0.060 Uiso 0.50 1 calc PR . . H19D H 0.1517 0.1277 0.7300 0.060 Uiso 0.50 1 calc PR . . H19E H 0.2286 0.0694 0.7667 0.060 Uiso 0.50 1 calc PR . . H19F H 0.3110 0.1347 0.7491 0.060 Uiso 0.50 1 calc PR . . C20 C -0.4462(4) 0.47180(19) 0.85167(17) 0.0250(10) Uani 1 1 d . . . C21 C -0.5112(4) 0.48200(19) 0.90599(16) 0.0250(10) Uani 1 1 d . . . H21 H -0.4943 0.4512 0.9371 0.030 Uiso 1 1 calc R . . C22 C -0.5989(4) 0.5364(2) 0.91388(17) 0.0313(11) Uani 1 1 d . . . H22 H -0.6391 0.5416 0.9503 0.038 Uiso 1 1 calc R . . C23 C -0.6286(4) 0.58363(19) 0.86893(17) 0.0298(11) Uani 1 1 d . . . H23 H -0.6899 0.6195 0.8743 0.036 Uiso 1 1 calc R . . C24 C -0.5637(4) 0.5756(2) 0.81545(17) 0.0344(11) Uani 1 1 d . . . H24 H -0.5794 0.6072 0.7849 0.041 Uiso 1 1 calc R . . C25 C -0.4767(4) 0.52106(19) 0.80773(17) 0.0279(10) Uani 1 1 d . . . H25 H -0.4360 0.5167 0.7714 0.033 Uiso 1 1 calc R . . C26 C -0.1948(4) 0.44166(19) 0.81842(16) 0.0242(10) Uani 1 1 d . . . C27 C -0.1235(4) 0.42474(19) 0.76745(16) 0.0279(10) Uani 1 1 d . . . H27 H -0.1644 0.3941 0.7401 0.033 Uiso 1 1 calc R . . C28 C 0.0060(4) 0.4524(2) 0.75665(18) 0.0371(12) Uani 1 1 d . . . H28 H 0.0499 0.4393 0.7227 0.044 Uiso 1 1 calc R . . C29 C 0.0708(4) 0.4988(2) 0.79501(18) 0.0353(11) Uani 1 1 d . . . H29 H 0.1585 0.5162 0.7879 0.042 Uiso 1 1 calc R . . C30 C 0.0015(4) 0.5190(2) 0.84459(17) 0.0332(11) Uani 1 1 d . . . H30 H 0.0419 0.5510 0.8710 0.040 Uiso 1 1 calc R . . C31 C -0.1277(4) 0.4916(2) 0.85466(17) 0.0327(11) Uani 1 1 d . . . H31 H -0.1731 0.5072 0.8875 0.039 Uiso 1 1 calc R . . C32 C -0.3093(4) 0.3573(2) 0.89513(17) 0.0273(10) Uani 1 1 d . . . C33 C -0.3362(4) 0.2872(2) 0.89563(19) 0.0333(11) Uani 1 1 d . . . H33 H -0.3838 0.2679 0.8625 0.040 Uiso 1 1 calc R . . C34 C -0.2946(5) 0.2446(2) 0.9438(2) 0.0457(13) Uani 1 1 d . . . H34 H -0.3119 0.1980 0.9418 0.055 Uiso 1 1 calc R . . C35 C -0.2270(5) 0.2730(3) 0.9947(2) 0.0501(15) Uani 1 1 d . . . H35 H -0.1970 0.2454 1.0266 0.060 Uiso 1 1 calc R . . C36 C -0.2054(4) 0.3419(2) 0.99712(19) 0.0435(13) Uani 1 1 d . . . H36 H -0.1632 0.3616 1.0313 0.052 Uiso 1 1 calc R . . C37 C -0.2465(4) 0.3827(2) 0.94831(17) 0.0338(11) Uani 1 1 d . . . H37 H -0.2313 0.4294 0.9513 0.041 Uiso 1 1 calc R . . C38 C -0.4189(4) 0.36264(19) 0.78143(17) 0.0258(10) Uani 1 1 d . . . C39 C -0.5552(4) 0.3744(2) 0.75603(17) 0.0354(11) Uani 1 1 d . . . H39 H -0.6066 0.4102 0.7707 0.043 Uiso 1 1 calc R . . C40 C -0.6158(5) 0.3347(2) 0.71004(18) 0.0431(13) Uani 1 1 d . . . H40 H -0.7064 0.3441 0.6952 0.052 Uiso 1 1 calc R . . C41 C -0.5433(5) 0.2818(2) 0.6863(2) 0.0545(15) Uani 1 1 d . . . H41 H -0.5829 0.2559 0.6550 0.065 Uiso 1 1 calc R . . C42 C -0.4098(5) 0.2682(2) 0.7103(2) 0.0526(15) Uani 1 1 d . . . H42 H -0.3592 0.2324 0.6950 0.063 Uiso 1 1 calc R . . C43 C -0.3509(4) 0.3069(2) 0.75644(17) 0.0361(11) Uani 1 1 d . . . H43 H -0.2616 0.2957 0.7718 0.043 Uiso 1 1 calc R . . N1 N -0.0998(4) 0.0840(2) 1.04598(16) 0.0381(10) Uani 1 1 d . . . N2 N 0.0414(3) 0.17863(16) 1.04871(13) 0.0256(8) Uani 1 1 d . . . N3 N 0.1345(3) 0.21449(15) 1.01497(13) 0.0246(8) Uani 1 1 d . . . N4 N 0.3036(3) 0.27197(15) 0.94423(13) 0.0264(8) Uani 1 1 d . . . H4 H 0.3940 0.2579 0.9482 0.032 Uiso 1 1 calc R . . N5 N 0.0502(3) 0.22589(15) 0.88120(13) 0.0250(8) Uani 1 1 d . . . H5 H -0.0320 0.2106 0.8944 0.030 Uiso 1 1 calc R . . N6 N 0.2605(3) 0.14568(15) 0.86646(13) 0.0251(8) Uani 1 1 d . . . N7 N 0.3817(3) 0.10654(16) 0.86396(13) 0.0273(8) Uani 1 1 d . . . N8 N 0.5606(4) 0.05871(18) 0.92081(16) 0.0352(10) Uani 1 1 d . . . S1 S 0.05590(11) 0.09351(5) 0.95328(4) 0.0327(3) Uani 1 1 d . . . S2 S 0.38538(11) 0.12965(5) 0.98383(4) 0.0315(3) Uani 1 1 d . . . Fe Fe 0.19807(7) 0.18155(3) 0.94032(3) 0.02487(16) Uani 1 1 d . . . B B -0.3454(5) 0.4075(2) 0.83624(19) 0.0239(11) Uani 1 1 d . . . H' H 0.597(4) 0.0499(18) 0.9576(14) 0.040(14) Uiso 1 1 d . . . H H -0.119(5) 0.039(2) 1.0295(18) 0.075(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(4) 0.150(6) 0.082(4) -0.061(4) 0.026(3) -0.040(4) C2 0.058(4) 0.073(4) 0.031(3) 0.009(3) 0.015(3) -0.016(3) C3 0.030(3) 0.029(2) 0.028(3) 0.012(2) 0.001(2) 0.005(2) C4 0.026(2) 0.026(2) 0.025(2) 0.0043(19) 0.003(2) 0.003(2) C5 0.036(3) 0.023(2) 0.021(2) -0.0038(19) 0.0065(19) -0.003(2) C6 0.031(2) 0.024(2) 0.027(2) 0.0018(19) 0.0065(19) -0.007(2) C7 0.034(3) 0.028(2) 0.023(2) 0.0049(18) 0.004(2) 0.005(2) C8 0.032(3) 0.022(2) 0.031(3) -0.0005(18) 0.007(2) 0.001(2) C9 0.033(3) 0.028(3) 0.019(2) -0.0024(19) 0.0017(19) -0.001(2) C10 0.026(3) 0.029(2) 0.031(3) -0.004(2) 0.003(2) -0.002(2) C11 0.030(3) 0.025(2) 0.028(3) -0.0014(19) 0.004(2) 0.000(2) C12 0.037(3) 0.042(3) 0.042(3) -0.005(2) 0.004(2) 0.006(2) C13 0.037(3) 0.037(3) 0.046(3) 0.002(2) 0.015(2) 0.006(2) C14 0.035(3) 0.037(3) 0.025(2) -0.003(2) 0.006(2) -0.001(2) C15 0.051(3) 0.026(3) 0.037(3) -0.004(2) 0.016(2) 0.000(2) C16 0.036(3) 0.053(3) 0.022(2) -0.005(2) 0.005(2) -0.010(3) C17 0.038(3) 0.039(3) 0.033(3) -0.001(2) 0.005(2) 0.002(2) C18 0.039(3) 0.039(3) 0.035(3) -0.005(2) -0.002(2) -0.002(2) C19 0.038(3) 0.051(3) 0.031(3) -0.011(2) 0.007(2) 0.009(2) C20 0.021(2) 0.021(2) 0.033(3) -0.0030(19) -0.0002(19) -0.0062(19) C21 0.026(2) 0.023(2) 0.025(2) 0.0031(18) -0.0010(19) -0.001(2) C22 0.032(3) 0.032(3) 0.031(3) -0.006(2) 0.006(2) -0.002(2) C23 0.027(3) 0.022(2) 0.039(3) -0.005(2) 0.000(2) -0.001(2) C24 0.035(3) 0.032(3) 0.036(3) 0.002(2) -0.001(2) -0.011(2) C25 0.030(3) 0.025(2) 0.029(3) -0.0005(19) 0.005(2) -0.002(2) C26 0.026(2) 0.022(2) 0.025(2) 0.0001(18) -0.0008(19) 0.001(2) C27 0.026(2) 0.033(3) 0.024(2) 0.0005(19) -0.0023(19) -0.002(2) C28 0.028(3) 0.046(3) 0.038(3) 0.008(2) 0.009(2) 0.003(2) C29 0.024(3) 0.032(3) 0.049(3) 0.013(2) -0.001(2) -0.009(2) C30 0.034(3) 0.032(3) 0.033(3) -0.001(2) -0.008(2) 0.000(2) C31 0.034(3) 0.030(3) 0.035(3) 0.005(2) 0.007(2) 0.000(2) C32 0.021(2) 0.033(3) 0.029(3) 0.002(2) 0.012(2) 0.003(2) C33 0.024(3) 0.034(3) 0.043(3) 0.006(2) 0.009(2) 0.003(2) C34 0.034(3) 0.040(3) 0.065(4) 0.022(3) 0.023(3) 0.012(3) C35 0.037(3) 0.065(4) 0.050(4) 0.028(3) 0.020(3) 0.027(3) C36 0.029(3) 0.065(4) 0.037(3) 0.005(3) 0.008(2) 0.019(3) C37 0.033(3) 0.037(3) 0.032(3) 0.009(2) 0.008(2) 0.010(2) C38 0.025(2) 0.020(2) 0.033(3) 0.0032(19) 0.009(2) -0.005(2) C39 0.041(3) 0.033(3) 0.033(3) 0.002(2) 0.009(2) -0.010(2) C40 0.042(3) 0.046(3) 0.039(3) -0.001(2) -0.007(2) -0.018(3) C41 0.060(4) 0.049(3) 0.056(4) -0.022(3) 0.007(3) -0.023(3) C42 0.063(4) 0.034(3) 0.062(4) -0.025(3) 0.017(3) -0.011(3) C43 0.034(3) 0.031(3) 0.044(3) -0.006(2) 0.008(2) -0.006(2) N1 0.041(2) 0.043(3) 0.031(2) 0.006(2) 0.0093(19) -0.014(2) N2 0.026(2) 0.0256(19) 0.026(2) 0.0005(16) 0.0070(15) -0.0056(17) N3 0.028(2) 0.0218(19) 0.024(2) -0.0007(15) 0.0019(16) 0.0038(17) N4 0.027(2) 0.029(2) 0.023(2) 0.0009(16) 0.0020(16) 0.0030(17) N5 0.027(2) 0.0203(19) 0.028(2) 0.0003(15) 0.0048(16) 0.0035(16) N6 0.030(2) 0.0210(19) 0.024(2) 0.0005(15) 0.0065(17) 0.0035(17) N7 0.025(2) 0.029(2) 0.028(2) -0.0006(16) -0.0004(17) 0.0091(17) N8 0.038(3) 0.037(2) 0.030(2) 0.0005(19) 0.001(2) 0.0113(19) S1 0.0412(7) 0.0253(6) 0.0322(7) -0.0002(5) 0.0071(5) -0.0066(5) S2 0.0359(7) 0.0319(6) 0.0267(6) 0.0010(5) 0.0017(5) 0.0081(6) Fe 0.0294(4) 0.0215(4) 0.0241(4) 0.0007(3) 0.0047(3) 0.0009(4) B 0.023(3) 0.029(3) 0.020(3) 0.000(2) 0.002(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.447(5) . ? C2 N1 1.474(5) . ? C3 N2 1.292(5) . ? C3 N1 1.358(5) . ? C3 S1 1.769(4) . ? C4 N3 1.280(4) . ? C4 C5 1.511(5) . ? C4 C14 1.511(4) . ? C5 C16 1.534(5) . ? C5 N4 1.548(4) . ? C5 C15 1.554(5) . ? C6 N4 1.499(4) . ? C6 C7 1.511(4) . ? C7 C8 1.519(4) . ? C8 N5 1.487(4) . ? C9 C10 1.521(5) . ? C9 C18 1.535(5) . ? C9 N5 1.537(4) . ? C9 C17 1.567(5) . ? C10 N6 1.272(4) . ? C10 C19 1.501(4) . ? C11 N7 1.297(4) . ? C11 N8 1.357(5) . ? C11 S2 1.761(4) . ? C12 N8 1.465(4) . ? C12 C13 1.519(5) . ? C20 C25 1.400(5) . ? C20 C21 1.417(4) . ? C20 B 1.640(5) . ? C21 C22 1.377(5) . ? C22 C23 1.387(5) . ? C23 C24 1.394(4) . ? C24 C25 1.375(5) . ? C26 C31 1.404(5) . ? C26 C27 1.408(4) . ? C26 B 1.664(5) . ? C27 C28 1.391(5) . ? C28 C29 1.376(5) . ? C29 C30 1.389(5) . ? C30 C31 1.383(5) . ? C32 C37 1.396(5) . ? C32 C33 1.400(5) . ? C32 B 1.668(5) . ? C33 C34 1.406(5) . ? C34 C35 1.395(6) . ? C35 C36 1.369(6) . ? C36 C37 1.394(5) . ? C38 C43 1.407(5) . ? C38 C39 1.413(5) . ? C38 B 1.637(5) . ? C39 C40 1.392(5) . ? C40 C41 1.374(5) . ? C41 C42 1.385(6) . ? C42 C43 1.379(5) . ? N2 N3 1.396(4) . ? N3 Fe 1.929(3) . ? N4 Fe 2.043(3) . ? N5 Fe 2.075(3) . ? N6 N7 1.398(4) . ? N6 Fe 1.930(3) . ? S1 Fe 2.2314(12) . ? S2 Fe 2.2380(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 C1 C2 N1 112.2(4) . . ? N2 C3 N1 120.2(4) . . ? N2 C3 S1 125.2(3) . . ? N1 C3 S1 114.6(3) . . ? N3 C4 C5 118.5(3) . . ? N3 C4 C14 122.4(3) . . ? C5 C4 C14 119.1(3) . . ? C4 C5 C16 110.3(3) . . ? C4 C5 N4 106.9(3) . . ? C16 C5 N4 106.7(3) . . ? C4 C5 C15 109.9(3) . . ? C16 C5 C15 107.9(3) . . ? N4 C5 C15 115.3(3) . . ? N4 C6 C7 114.5(3) . . ? C6 C7 C8 115.2(3) . . ? N5 C8 C7 116.6(3) . . ? C10 C9 C18 111.3(3) . . ? C10 C9 N5 107.6(3) . . ? C18 C9 N5 108.2(3) . . ? C10 C9 C17 108.2(3) . . ? C18 C9 C17 107.6(3) . . ? N5 C9 C17 114.1(3) . . ? N6 C10 C19 123.1(4) . . ? N6 C10 C9 117.4(3) . . ? C19 C10 C9 119.5(4) . . ? N7 C11 N8 118.2(4) . . ? N7 C11 S2 125.5(3) . . ? N8 C11 S2 116.3(3) . . ? N8 C12 C13 110.0(3) . . ? C25 C20 C21 115.1(4) . . ? C25 C20 B 118.9(3) . . ? C21 C20 B 125.9(4) . . ? C22 C21 C20 121.6(4) . . ? C21 C22 C23 121.7(4) . . ? C22 C23 C24 117.9(4) . . ? C25 C24 C23 120.2(4) . . ? C24 C25 C20 123.5(4) . . ? C31 C26 C27 114.0(4) . . ? C31 C26 B 121.1(3) . . ? C27 C26 B 124.9(3) . . ? C28 C27 C26 122.2(4) . . ? C29 C28 C27 121.6(4) . . ? C28 C29 C30 118.1(4) . . ? C31 C30 C29 119.8(4) . . ? C30 C31 C26 124.1(4) . . ? C37 C32 C33 114.5(4) . . ? C37 C32 B 121.6(4) . . ? C33 C32 B 123.9(4) . . ? C32 C33 C34 123.1(5) . . ? C35 C34 C33 119.2(5) . . ? C36 C35 C34 119.3(5) . . ? C35 C36 C37 120.0(5) . . ? C36 C37 C32 123.6(4) . . ? C43 C38 C39 114.0(4) . . ? C43 C38 B 121.9(4) . . ? C39 C38 B 124.1(4) . . ? C40 C39 C38 122.9(4) . . ? C41 C40 C39 120.7(5) . . ? C40 C41 C42 118.3(5) . . ? C43 C42 C41 120.8(4) . . ? C42 C43 C38 123.3(4) . . ? C3 N1 C2 121.7(4) . . ? C3 N2 N3 111.5(3) . . ? C4 N3 N2 116.3(3) . . ? C4 N3 Fe 120.3(3) . . ? N2 N3 Fe 123.3(2) . . ? C6 N4 C5 118.3(3) . . ? C6 N4 Fe 116.8(2) . . ? C5 N4 Fe 112.3(2) . . ? C8 N5 C9 118.1(3) . . ? C8 N5 Fe 116.2(2) . . ? C9 N5 Fe 111.0(2) . . ? C10 N6 N7 116.0(3) . . ? C10 N6 Fe 121.3(3) . . ? N7 N6 Fe 122.5(2) . . ? C11 N7 N6 111.9(3) . . ? C11 N8 C12 121.8(4) . . ? C3 S1 Fe 94.64(14) . . ? C11 S2 Fe 94.31(15) . . ? N6 Fe N3 178.18(13) . . ? N6 Fe N4 100.08(12) . . ? N3 Fe N4 81.57(12) . . ? N6 Fe N5 80.74(12) . . ? N3 Fe N5 100.09(12) . . ? N4 Fe N5 88.91(12) . . ? N6 Fe S1 93.06(10) . . ? N3 Fe S1 85.33(10) . . ? N4 Fe S1 166.57(9) . . ? N5 Fe S1 90.48(9) . . ? N6 Fe S2 85.77(10) . . ? N3 Fe S2 93.51(10) . . ? N4 Fe S2 89.64(10) . . ? N5 Fe S2 165.96(9) . . ? S1 Fe S2 94.11(5) . . ? C20 B C38 109.9(3) . . ? C20 B C32 112.6(3) . . ? C38 B C32 109.7(4) . . ? C20 B C26 105.8(3) . . ? C38 B C26 112.1(3) . . ? C32 B C26 106.7(3) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 73.43 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.301 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.058 # Attachment 'jmwpd89.cif' data_jmwpd89 _database_code_depnum_ccdc_archive 'CCDC 745072' #TrackingRef 'jmwpd89.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H58 B Co N8 S2' _chemical_formula_weight 820.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 10.0066(2) _cell_length_b 18.1840(3) _cell_length_c 23.1069(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.265(2) _cell_angle_gamma 90.00 _cell_volume 4179.42(13) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4159 _cell_measurement_theta_min 3.8446 _cell_measurement_theta_max 73.2443 _exptl_crystal_description rod _exptl_crystal_colour purple _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 4.467 _exptl_absorpt_correction_T_min 0.33990 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite #'Oxford Diffraction Gemini-S CCD-detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15936 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.1019 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 69.99 _reflns_number_total 7713 _reflns_number_gt 4333 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7713 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 Co Co 0.25294(8) 0.18791(3) 0.50030(3) 0.01659(15) Uani 1 1 d . . . S1 S 0.09072(11) 0.10351(6) 0.48480(4) 0.0213(3) Uani 1 1 d . . . S2 S 0.40327(11) 0.09670(6) 0.51106(4) 0.0212(3) Uani 1 1 d . . . N5 N 0.1236(4) 0.26927(19) 0.47201(14) 0.0190(8) Uani 1 1 d . . . N6 N 0.3008(3) 0.19457(18) 0.42286(13) 0.0186(8) Uani 1 1 d . . . N3 N 0.2034(3) 0.19090(18) 0.57769(13) 0.0169(7) Uani 1 1 d . . . N4 N 0.3996(3) 0.25683(19) 0.53351(15) 0.0199(8) Uani 1 1 d . . . N2 N 0.0886(3) 0.15773(19) 0.59385(14) 0.0210(8) Uani 1 1 d . . . N8 N 0.5782(4) 0.0769(2) 0.43450(16) 0.0274(9) Uani 1 1 d . . . N7 N 0.4143(4) 0.16071(19) 0.40541(14) 0.0247(9) Uani 1 1 d . . . C36 C -0.1582(4) 0.2006(2) 0.73764(18) 0.0247(10) Uani 1 1 d . . . H36 H -0.1078 0.1576 0.7376 0.030 Uiso 1 1 calc R . . N1 N -0.0809(4) 0.0785(2) 0.56174(16) 0.0268(9) Uani 1 1 d . . . C38 C 0.0029(5) 0.4177(2) 0.68096(18) 0.0264(10) Uani 1 1 d . . . C26 C -0.2463(5) 0.4691(2) 0.6747(2) 0.0307(11) Uani 1 1 d . . . C9 C 0.1070(4) 0.2725(2) 0.40533(17) 0.0210(10) Uani 1 1 d . . . C3 C 0.0314(4) 0.1148(2) 0.55266(17) 0.0206(10) Uani 1 1 d . . . C4 C 0.2757(4) 0.2298(2) 0.61629(17) 0.0195(9) Uani 1 1 d . . . C33 C -0.3029(4) 0.3299(2) 0.73756(17) 0.0221(9) Uani 1 1 d . . . H33 H -0.3526 0.3729 0.7387 0.027 Uiso 1 1 calc R . . C25 C -0.1948(4) 0.3031(2) 0.56872(18) 0.0267(10) Uani 1 1 d . . . H25 H -0.1888 0.2643 0.5951 0.032 Uiso 1 1 calc R . . C10 C 0.2319(4) 0.2371(2) 0.38581(17) 0.0215(10) Uani 1 1 d . . . C32 C -0.1986(4) 0.3273(2) 0.70196(17) 0.0208(9) Uani 1 1 d . . . C11 C 0.4665(4) 0.1139(2) 0.44478(18) 0.0237(10) Uani 1 1 d . . . C5 C 0.4051(4) 0.2598(2) 0.59992(17) 0.0215(10) Uani 1 1 d . . . C37 C -0.1275(4) 0.2602(2) 0.70410(17) 0.0234(9) Uani 1 1 d . . . H37 H -0.0561 0.2558 0.6818 0.028 Uiso 1 1 calc R . . C35 C -0.2649(4) 0.2055(2) 0.77130(17) 0.0255(10) Uani 1 1 d . . . H35 H -0.2882 0.1656 0.7933 0.031 Uiso 1 1 calc R . . C8 C 0.1507(5) 0.3402(2) 0.50415(18) 0.0272(10) Uani 1 1 d . . . H8A H 0.1443 0.3312 0.5451 0.033 Uiso 1 1 calc R . . H8B H 0.0802 0.3747 0.4907 0.033 Uiso 1 1 calc R . . C41 C 0.2110(5) 0.4809(3) 0.6643(2) 0.0378(12) Uani 1 1 d . . . H41 H 0.2597 0.5070 0.6391 0.045 Uiso 1 1 calc R . . C42 C 0.2665(5) 0.4678(3) 0.7204(2) 0.0372(12) Uani 1 1 d . . . H42 H 0.3526 0.4843 0.7333 0.045 Uiso 1 1 calc R . . C34 C -0.3352(4) 0.2702(3) 0.77142(17) 0.0286(11) Uani 1 1 d . . . H34 H -0.4055 0.2744 0.7944 0.034 Uiso 1 1 calc R . . C6 C 0.4084(5) 0.3272(2) 0.50048(19) 0.0300(11) Uani 1 1 d . . . H6A H 0.4242 0.3153 0.4609 0.036 Uiso 1 1 calc R . . H6B H 0.4857 0.3546 0.5179 0.036 Uiso 1 1 calc R . . C44 C 0.0638(5) 0.4050(2) 0.73748(19) 0.0309(11) Uani 1 1 d . . . H44 H 0.0161 0.3787 0.7630 0.037 Uiso 1 1 calc R . . C20 C -0.1784(4) 0.3744(2) 0.59069(18) 0.0241(10) Uani 1 1 d . . . C19 C 0.2643(4) 0.2473(3) 0.32480(17) 0.0314(11) Uani 1 1 d . . . H19A H 0.3457 0.2214 0.3195 0.047 Uiso 1 1 calc R . . H19B H 0.2760 0.2987 0.3174 0.047 Uiso 1 1 calc R . . H19C H 0.1921 0.2283 0.2982 0.047 Uiso 1 1 calc R . . C15 C 0.5176(4) 0.2087(2) 0.62575(18) 0.0272(10) Uani 1 1 d . . . H15A H 0.6025 0.2266 0.6159 0.041 Uiso 1 1 calc R . . H15B H 0.5023 0.1600 0.6103 0.041 Uiso 1 1 calc R . . H15C H 0.5187 0.2073 0.6673 0.041 Uiso 1 1 calc R . . C21 C -0.1841(4) 0.4296(3) 0.54779(19) 0.0309(11) Uani 1 1 d . . . H21 H -0.1698 0.4781 0.5597 0.037 Uiso 1 1 calc R . . C12 C 0.6398(5) 0.0826(3) 0.38004(19) 0.0353(13) Uani 1 1 d . . . H12A H 0.6571 0.1339 0.3719 0.042 Uiso 1 1 calc R . . H12B H 0.5785 0.0634 0.3482 0.042 Uiso 1 1 calc R . . C18 C -0.0150(4) 0.2257(2) 0.38124(18) 0.0292(11) Uani 1 1 d . . . H18A H -0.0956 0.2470 0.3930 0.044 Uiso 1 1 calc R . . H18B H -0.0046 0.1766 0.3962 0.044 Uiso 1 1 calc R . . H18C H -0.0207 0.2246 0.3395 0.044 Uiso 1 1 calc R . . C16 C 0.4344(5) 0.3369(2) 0.62421(19) 0.0350(12) Uani 1 1 d . . . H16A H 0.5180 0.3541 0.6124 0.052 Uiso 1 1 calc R . . H16B H 0.4404 0.3354 0.6659 0.052 Uiso 1 1 calc R . . H16C H 0.3633 0.3695 0.6096 0.052 Uiso 1 1 calc R . . C23 C -0.2294(4) 0.3434(3) 0.46972(19) 0.0377(13) Uani 1 1 d . . . H23 H -0.2490 0.3335 0.4302 0.045 Uiso 1 1 calc R . . B B -0.1554(5) 0.3963(3) 0.6613(2) 0.0242(11) Uani 1 1 d . . . C22 C -0.2099(5) 0.4154(3) 0.4889(2) 0.0400(13) Uani 1 1 d . . . H22 H -0.2142 0.4539 0.4623 0.048 Uiso 1 1 calc R . . C14 C 0.2385(4) 0.2416(3) 0.67631(17) 0.0283(11) Uani 1 1 d . . . H14A H 0.1533 0.2187 0.6799 0.042 Uiso 1 1 calc R . . H14B H 0.2322 0.2933 0.6837 0.042 Uiso 1 1 calc R . . H14C H 0.3059 0.2202 0.7040 0.042 Uiso 1 1 calc R . . C7 C 0.2851(4) 0.3765(2) 0.4984(2) 0.0362(13) Uani 1 1 d . . . H7A H 0.3011 0.4125 0.5294 0.043 Uiso 1 1 calc R . . H7B H 0.2774 0.4031 0.4619 0.043 Uiso 1 1 calc R . . C43 C 0.1915(5) 0.4295(3) 0.7574(2) 0.0341(12) Uani 1 1 d . . . H43 H 0.2270 0.4203 0.7956 0.041 Uiso 1 1 calc R . . C1 C -0.2673(4) 0.0408(3) 0.61433(19) 0.0325(12) Uani 1 1 d . . . H1A H -0.2996 0.0410 0.6519 0.049 Uiso 1 1 calc R . . H1B H -0.2594 -0.0090 0.6013 0.049 Uiso 1 1 calc R . . H1C H -0.3292 0.0670 0.5871 0.049 Uiso 1 1 calc R . . C27 C -0.3607(5) 0.4931(3) 0.6393(3) 0.0423(13) Uani 1 1 d . . . H27 H -0.3840 0.4704 0.6036 0.051 Uiso 1 1 calc R . . C17 C 0.0855(5) 0.3505(2) 0.38058(19) 0.0316(11) Uani 1 1 d . . . H17A H 0.0061 0.3713 0.3938 0.047 Uiso 1 1 calc R . . H17B H 0.0751 0.3484 0.3388 0.047 Uiso 1 1 calc R . . H17C H 0.1619 0.3804 0.3936 0.047 Uiso 1 1 calc R . . C28 C -0.4418(6) 0.5514(3) 0.6567(3) 0.0605(19) Uani 1 1 d . . . H28 H -0.5161 0.5670 0.6321 0.073 Uiso 1 1 calc R . . C2 C -0.1334(4) 0.0770(3) 0.61830(18) 0.0278(11) Uani 1 1 d . . . H2A H -0.1411 0.1269 0.6324 0.033 Uiso 1 1 calc R . . H2B H -0.0712 0.0507 0.6460 0.033 Uiso 1 1 calc R . . C39 C 0.0835(5) 0.4558(3) 0.6450(2) 0.0326(11) Uani 1 1 d . . . H39 H 0.0497 0.4646 0.6065 0.039 Uiso 1 1 calc R . . C13 C 0.7679(5) 0.0406(3) 0.38442(19) 0.0413(14) Uani 1 1 d . . . H13A H 0.8073 0.0448 0.3485 0.062 Uiso 1 1 calc R . . H13B H 0.7504 -0.0102 0.3919 0.062 Uiso 1 1 calc R . . H13C H 0.8288 0.0601 0.4156 0.062 Uiso 1 1 calc R . . C24 C -0.2194(4) 0.2867(3) 0.50978(19) 0.0359(12) Uani 1 1 d . . . H24 H -0.2290 0.2381 0.4974 0.043 Uiso 1 1 calc R . . C31 C -0.2195(5) 0.5061(2) 0.7271(2) 0.0405(13) Uani 1 1 d . . . H31 H -0.1436 0.4926 0.7517 0.049 Uiso 1 1 calc R . . C30 C -0.2998(7) 0.5621(3) 0.7450(3) 0.0586(18) Uani 1 1 d . . . H30 H -0.2780 0.5842 0.7810 0.070 Uiso 1 1 calc R . . C29 C -0.4107(6) 0.5848(3) 0.7098(3) 0.064(2) Uani 1 1 d . . . H29 H -0.4645 0.6224 0.7217 0.077 Uiso 1 1 calc R . . H H 0.037(4) 0.255(3) 0.4808(18) 0.040 Uiso 1 1 d . . . H1 H 0.474(4) 0.235(3) 0.5275(19) 0.040 Uiso 1 1 d . . . H8 H 0.602(5) 0.044(3) 0.4577(19) 0.040 Uiso 1 1 d . . . H1D H -0.099(5) 0.044(3) 0.5409(19) 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0245(3) 0.0119(3) 0.0135(3) 0.0001(3) 0.0028(2) -0.0002(3) S1 0.0314(7) 0.0177(5) 0.0151(5) -0.0039(4) 0.0042(4) -0.0057(5) S2 0.0323(7) 0.0151(5) 0.0169(5) 0.0023(4) 0.0057(4) 0.0048(5) N5 0.026(2) 0.0165(19) 0.0140(17) -0.0020(14) -0.0017(15) 0.0011(15) N6 0.029(2) 0.0129(17) 0.0148(17) 0.0036(15) 0.0053(15) 0.0006(15) N3 0.019(2) 0.0148(18) 0.0169(17) 0.0022(15) 0.0019(14) 0.0004(15) N4 0.023(2) 0.0152(18) 0.0214(18) 0.0012(15) 0.0034(15) 0.0021(15) N2 0.027(2) 0.0204(19) 0.0156(18) -0.0005(16) 0.0032(15) -0.0049(16) N8 0.035(2) 0.023(2) 0.025(2) 0.0067(17) 0.0084(18) 0.0097(18) N7 0.033(2) 0.020(2) 0.0220(19) 0.0076(17) 0.0072(17) 0.0047(17) C36 0.029(3) 0.018(2) 0.025(2) -0.0017(19) -0.0078(19) -0.0001(19) N1 0.039(3) 0.021(2) 0.022(2) -0.0101(17) 0.0110(18) -0.0107(18) C38 0.039(3) 0.016(2) 0.026(2) -0.0027(18) 0.009(2) -0.002(2) C26 0.038(3) 0.013(2) 0.045(3) 0.003(2) 0.021(2) -0.002(2) C9 0.024(2) 0.019(2) 0.019(2) 0.0024(18) 0.0003(18) -0.0011(19) C3 0.028(3) 0.016(2) 0.017(2) 0.0023(19) 0.0015(18) 0.0026(19) C4 0.026(3) 0.017(2) 0.015(2) -0.0035(17) -0.0025(18) 0.0035(18) C33 0.026(2) 0.019(2) 0.021(2) -0.0039(18) 0.0005(17) -0.0018(19) C25 0.019(2) 0.031(3) 0.031(2) 0.009(2) 0.0066(18) 0.0051(19) C10 0.029(3) 0.021(2) 0.015(2) -0.0012(18) 0.0010(18) -0.0038(19) C32 0.020(2) 0.021(2) 0.021(2) -0.0061(18) 0.0004(17) -0.0017(18) C11 0.029(3) 0.019(2) 0.024(2) -0.001(2) 0.007(2) -0.002(2) C5 0.025(2) 0.020(2) 0.018(2) -0.0026(18) -0.0056(18) -0.0004(19) C37 0.022(2) 0.025(2) 0.023(2) -0.0048(19) 0.0005(17) -0.0023(19) C35 0.032(3) 0.025(2) 0.018(2) 0.0011(18) -0.0025(18) -0.012(2) C8 0.040(3) 0.017(2) 0.024(2) -0.0038(19) -0.003(2) 0.009(2) C41 0.038(3) 0.036(3) 0.041(3) 0.001(2) 0.013(2) -0.011(2) C42 0.043(3) 0.026(3) 0.041(3) -0.009(2) -0.001(2) -0.011(2) C34 0.035(3) 0.035(3) 0.016(2) -0.004(2) 0.0048(19) -0.014(2) C6 0.036(3) 0.025(2) 0.029(2) 0.003(2) 0.001(2) -0.008(2) C44 0.038(3) 0.024(2) 0.031(2) 0.000(2) 0.007(2) -0.009(2) C20 0.021(2) 0.023(2) 0.029(2) 0.0021(19) 0.0063(18) 0.0024(18) C19 0.041(3) 0.034(3) 0.020(2) 0.008(2) 0.009(2) 0.002(2) C15 0.028(3) 0.028(2) 0.024(2) -0.001(2) -0.0015(19) 0.001(2) C21 0.027(3) 0.030(3) 0.035(3) 0.004(2) 0.001(2) 0.002(2) C12 0.038(3) 0.044(3) 0.026(3) 0.011(2) 0.014(2) 0.011(3) C18 0.032(3) 0.032(3) 0.022(2) 0.001(2) -0.001(2) 0.003(2) C16 0.047(3) 0.024(3) 0.033(3) -0.003(2) 0.001(2) -0.006(2) C23 0.028(3) 0.062(4) 0.024(2) 0.002(2) 0.003(2) 0.010(3) B 0.031(3) 0.018(2) 0.025(3) 0.000(2) 0.011(2) 0.004(2) C22 0.044(3) 0.045(3) 0.032(3) 0.020(2) 0.008(2) 0.012(3) C14 0.025(3) 0.034(3) 0.024(2) -0.008(2) -0.0022(19) 0.002(2) C7 0.046(4) 0.019(2) 0.040(3) 0.002(2) -0.014(3) -0.001(2) C43 0.044(3) 0.029(3) 0.028(2) -0.001(2) -0.004(2) -0.004(2) C1 0.030(3) 0.035(3) 0.034(3) 0.002(2) 0.010(2) 0.000(2) C27 0.029(3) 0.021(3) 0.079(4) 0.005(3) 0.020(3) 0.001(2) C17 0.044(3) 0.024(2) 0.026(2) 0.009(2) -0.001(2) 0.008(2) C28 0.033(3) 0.027(3) 0.124(6) 0.016(4) 0.020(4) 0.001(3) C2 0.037(3) 0.026(2) 0.022(2) -0.001(2) 0.009(2) -0.004(2) C39 0.034(3) 0.034(3) 0.030(2) 0.002(2) 0.004(2) -0.005(2) C13 0.032(3) 0.064(4) 0.030(3) 0.008(3) 0.010(2) 0.008(3) C24 0.041(3) 0.035(3) 0.033(3) -0.006(2) 0.009(2) 0.008(2) C31 0.059(4) 0.017(2) 0.049(3) 0.004(2) 0.025(3) 0.009(2) C30 0.082(5) 0.024(3) 0.078(4) -0.009(3) 0.049(4) 0.004(3) C29 0.057(4) 0.021(3) 0.124(6) -0.007(4) 0.056(4) 0.005(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 Co N6 1.906(3) . ? Co N3 1.908(3) . ? Co N4 2.017(4) . ? Co N5 2.026(3) . ? Co S1 2.2342(12) . ? Co S2 2.2347(12) . ? S1 C3 1.748(4) . ? S2 C11 1.748(4) . ? N5 C8 1.498(5) . ? N5 C9 1.533(5) . ? N6 C10 1.295(5) . ? N6 N7 1.389(4) . ? N3 C4 1.295(5) . ? N3 N2 1.384(4) . ? N4 C6 1.497(5) . ? N4 C5 1.530(5) . ? N2 C3 1.313(5) . ? N8 C11 1.347(5) . ? N8 C12 1.464(5) . ? N7 C11 1.312(5) . ? C36 C37 1.387(5) . ? C36 C35 1.391(6) . ? N1 C3 1.339(5) . ? N1 C2 1.461(5) . ? C38 C44 1.399(6) . ? C38 C39 1.402(5) . ? C38 B 1.647(7) . ? C26 C31 1.386(6) . ? C26 C27 1.403(6) . ? C26 B 1.654(6) . ? C9 C10 1.518(5) . ? C9 C17 1.536(5) . ? C9 C18 1.540(6) . ? C4 C14 1.490(5) . ? C4 C5 1.492(5) . ? C33 C34 1.396(5) . ? C33 C32 1.398(5) . ? C25 C24 1.390(6) . ? C25 C20 1.396(6) . ? C10 C19 1.492(5) . ? C32 C37 1.410(5) . ? C32 B 1.653(6) . ? C5 C16 1.525(6) . ? C5 C15 1.531(5) . ? C35 C34 1.370(6) . ? C8 C7 1.516(6) . ? C41 C42 1.375(6) . ? C41 C39 1.382(6) . ? C42 C43 1.384(6) . ? C6 C7 1.522(6) . ? C44 C43 1.384(6) . ? C20 C21 1.407(5) . ? C20 B 1.670(6) . ? C21 C22 1.380(6) . ? C12 C13 1.486(6) . ? C23 C24 1.382(6) . ? C23 C22 1.389(7) . ? C1 C2 1.486(5) . ? C27 C28 1.419(7) . ? C28 C29 1.373(8) . ? C31 C30 1.387(6) . ? C30 C29 1.366(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 N6 Co N3 174.71(13) . . ? N6 Co N4 94.05(14) . . ? N3 Co N4 83.01(14) . . ? N6 Co N5 82.42(14) . . ? N3 Co N5 93.40(14) . . ? N4 Co N5 94.68(14) . . ? N6 Co S1 98.39(11) . . ? N3 Co S1 84.91(11) . . ? N4 Co S1 166.81(11) . . ? N5 Co S1 91.29(11) . . ? N6 Co S2 85.20(11) . . ? N3 Co S2 99.06(10) . . ? N4 Co S2 88.05(10) . . ? N5 Co S2 167.48(10) . . ? S1 Co S2 88.65(4) . . ? C3 S1 Co 95.03(15) . . ? C11 S2 Co 94.21(16) . . ? C8 N5 C9 117.4(3) . . ? C8 N5 Co 113.2(3) . . ? C9 N5 Co 110.3(2) . . ? C10 N6 N7 117.8(3) . . ? C10 N6 Co 119.2(3) . . ? N7 N6 Co 122.8(3) . . ? C4 N3 N2 118.0(3) . . ? C4 N3 Co 118.6(3) . . ? N2 N3 Co 123.3(2) . . ? C6 N4 C5 118.9(3) . . ? C6 N4 Co 114.7(3) . . ? C5 N4 Co 110.4(3) . . ? C3 N2 N3 111.9(3) . . ? C11 N8 C12 123.5(4) . . ? C11 N7 N6 111.3(3) . . ? C37 C36 C35 119.4(4) . . ? C3 N1 C2 122.6(4) . . ? C44 C38 C39 114.5(4) . . ? C44 C38 B 121.8(4) . . ? C39 C38 B 123.5(4) . . ? C31 C26 C27 115.2(5) . . ? C31 C26 B 119.7(4) . . ? C27 C26 B 124.8(4) . . ? C10 C9 N5 106.3(3) . . ? C10 C9 C17 111.5(4) . . ? N5 C9 C17 113.9(4) . . ? C10 C9 C18 107.8(3) . . ? N5 C9 C18 109.7(3) . . ? C17 C9 C18 107.6(4) . . ? N2 C3 N1 119.1(4) . . ? N2 C3 S1 123.8(3) . . ? N1 C3 S1 117.1(3) . . ? N3 C4 C14 122.8(4) . . ? N3 C4 C5 117.4(4) . . ? C14 C4 C5 119.7(4) . . ? C34 C33 C32 122.5(4) . . ? C24 C25 C20 123.9(4) . . ? N6 C10 C19 122.9(4) . . ? N6 C10 C9 116.9(4) . . ? C19 C10 C9 119.9(4) . . ? C33 C32 C37 114.5(4) . . ? C33 C32 B 124.5(4) . . ? C37 C32 B 121.0(4) . . ? N7 C11 N8 118.5(4) . . ? N7 C11 S2 124.7(3) . . ? N8 C11 S2 116.9(3) . . ? C4 C5 C16 112.4(4) . . ? C4 C5 N4 107.7(3) . . ? C16 C5 N4 112.7(4) . . ? C4 C5 C15 107.5(4) . . ? C16 C5 C15 108.1(4) . . ? N4 C5 C15 108.3(3) . . ? C36 C37 C32 123.7(4) . . ? C34 C35 C36 118.8(4) . . ? N5 C8 C7 116.5(4) . . ? C42 C41 C39 120.7(5) . . ? C41 C42 C43 118.6(5) . . ? C35 C34 C33 121.1(4) . . ? N4 C6 C7 115.2(4) . . ? C43 C44 C38 123.4(4) . . ? C25 C20 C21 114.3(4) . . ? C25 C20 B 125.1(4) . . ? C21 C20 B 120.6(4) . . ? C22 C21 C20 123.4(5) . . ? N8 C12 C13 110.2(4) . . ? C24 C23 C22 119.5(4) . . ? C38 B C26 106.9(4) . . ? C38 B C32 109.0(4) . . ? C26 B C32 108.5(3) . . ? C38 B C20 110.6(3) . . ? C26 B C20 110.7(4) . . ? C32 B C20 111.0(3) . . ? C21 C22 C23 119.7(5) . . ? C8 C7 C6 117.6(4) . . ? C44 C43 C42 119.9(4) . . ? C26 C27 C28 121.5(5) . . ? C29 C28 C27 120.2(6) . . ? N1 C2 C1 111.3(4) . . ? C41 C39 C38 122.9(4) . . ? C23 C24 C25 119.2(5) . . ? C26 C31 C30 123.6(6) . . ? C29 C30 C31 120.3(6) . . ? C30 C29 C28 119.2(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.461 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.068