Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matthias Wagner' _publ_contact_author_address ; Inst. fuer Anorganische Chemie Goethe-Universitaet Frankfurt Max-von Laue-Strasse 7 Frankfurt 60438 GERMANY ; _publ_contact_author_email MATTHIAS.WAGNER@CHEMIE.UNI-FRANKFURT.DE _publ_section_title ; Metallomacrocycles from Ditopic Chiral Scorpionate Ligands ; loop_ _publ_author_name 'Matthias Wagner' 'Susanne Bieller' 'Michael Bolte' 'Hans-Wolfram Lerner' 'Thorsten Morawitz' 'Fan Zhang' data_wa307 _database_code_depnum_ccdc_archive 'CCDC 645747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H96 B4 Fe2 N12 O2' _chemical_formula_weight 1340.57 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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4593(18) _cell_length_b 12.9493(18) _cell_length_c 13.503(2) _cell_angle_alpha 75.167(11) _cell_angle_beta 68.358(11) _cell_angle_gamma 63.880(10) _cell_volume 1806.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6685 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 25.2 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8870 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13843 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.1327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.32 _reflns_number_total 6336 _reflns_number_gt 3702 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0200P)^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 6336 _refine_ls_number_parameters 430 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.797 _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 Fe1 Fe 0.33466(5) 0.23198(4) 0.61554(4) 0.02955(13) Uani 1 1 d . . . B1 B 0.2433(3) 0.1680(3) 0.8537(3) 0.0290(8) Uani 1 1 d . . . O1 O 0.3893(2) 0.13654(18) 0.49971(15) 0.0284(5) Uani 1 1 d D . . H1 H 0.398(4) 0.0679(13) 0.519(3) 0.061(13) Uiso 1 1 d D . . C1 C 0.1958(3) 0.1194(3) 0.9813(2) 0.0338(7) Uani 1 1 d . . . C2 C 0.1521(3) 0.2058(3) 1.0620(2) 0.0434(9) Uani 1 1 d . . . H2A H 0.2195 0.2309 1.0517 0.065 Uiso 1 1 calc R . . H2B H 0.1306 0.1682 1.1353 0.065 Uiso 1 1 calc R . . H2C H 0.0784 0.2732 1.0503 0.065 Uiso 1 1 calc R . . C3 C 0.3030(3) 0.0090(3) 1.0101(2) 0.0426(9) Uani 1 1 d . . . H3A H 0.3749 0.0278 0.9993 0.064 Uiso 1 1 calc R . . H3B H 0.3276 -0.0499 0.9639 0.064 Uiso 1 1 calc R . . H3C H 0.2743 -0.0208 1.0853 0.064 Uiso 1 1 calc R . . C4 C 0.0875(3) 0.0826(3) 1.0009(3) 0.0419(8) Uani 1 1 d . . . H4A H 0.1125 0.0274 0.9510 0.063 Uiso 1 1 calc R . . H4B H 0.0143 0.1509 0.9897 0.063 Uiso 1 1 calc R . . H4C H 0.0666 0.0461 1.0748 0.063 Uiso 1 1 calc R . . B2 B 0.4274(3) 0.1817(3) 0.3808(2) 0.0264(7) Uani 1 1 d . . . C5 C 0.3144(3) 0.2119(3) 0.3310(2) 0.0320(7) Uani 1 1 d . . . C6 C 0.1963(3) 0.3093(3) 0.3872(3) 0.0471(9) Uani 1 1 d . . . H6A H 0.1720 0.2851 0.4644 0.071 Uiso 1 1 calc R . . H6B H 0.1281 0.3255 0.3585 0.071 Uiso 1 1 calc R . . H6C H 0.2135 0.3792 0.3745 0.071 Uiso 1 1 calc R . . C7 C 0.2780(3) 0.1087(3) 0.3490(3) 0.0420(8) Uani 1 1 d . . . H7A H 0.2564 0.0815 0.4257 0.063 Uiso 1 1 calc R . . H7B H 0.3485 0.0461 0.3097 0.063 Uiso 1 1 calc R . . H7C H 0.2057 0.1323 0.3232 0.063 Uiso 1 1 calc R . . C8 C 0.3485(3) 0.2548(3) 0.2099(2) 0.0432(9) Uani 1 1 d . . . H8A H 0.3717 0.3210 0.1984 0.065 Uiso 1 1 calc R . . H8B H 0.2763 0.2783 0.1841 0.065 Uiso 1 1 calc R . . H8C H 0.4191 0.1922 0.1706 0.065 Uiso 1 1 calc R . . N11 N 0.3623(2) 0.1971(2) 0.82753(18) 0.0278(6) Uani 1 1 d . . . N12 N 0.4235(2) 0.2187(2) 0.72101(18) 0.0292(6) Uani 1 1 d . . . C13 C 0.5189(3) 0.2403(3) 0.7170(3) 0.0363(8) Uani 1 1 d . . . H13 H 0.5764 0.2581 0.6528 0.044 Uiso 1 1 calc R . . C14 C 0.5239(3) 0.2333(3) 0.8195(3) 0.0451(9) Uani 1 1 d . . . H14 H 0.5836 0.2444 0.8391 0.054 Uiso 1 1 calc R . . C15 C 0.4246(3) 0.2071(3) 0.8856(2) 0.0347(8) Uani 1 1 d . . . H15 H 0.4022 0.1973 0.9617 0.042 Uiso 1 1 calc R . . N21 N 0.1389(2) 0.2850(2) 0.81860(18) 0.0281(6) Uani 1 1 d . . . N22 N 0.1649(2) 0.3258(2) 0.71145(19) 0.0313(6) Uani 1 1 d . . . C23 C 0.0657(3) 0.4197(3) 0.7000(3) 0.0364(8) Uani 1 1 d . . . H23 H 0.0586 0.4656 0.6337 0.044 Uiso 1 1 calc R . . C24 C -0.0260(3) 0.4424(3) 0.7968(3) 0.0416(8) Uani 1 1 d . . . H24 H -0.1058 0.5042 0.8104 0.050 Uiso 1 1 calc R . . C25 C 0.0245(3) 0.3549(3) 0.8694(2) 0.0343(8) Uani 1 1 d . . . H25 H -0.0159 0.3457 0.9441 0.041 Uiso 1 1 calc R . . N31 N 0.4366(2) 0.2972(2) 0.38898(18) 0.0272(6) Uani 1 1 d . . . N32 N 0.3919(2) 0.3398(2) 0.48564(19) 0.0337(6) Uani 1 1 d . . . C33 C 0.4111(4) 0.4372(3) 0.4659(3) 0.0469(9) Uani 1 1 d . . . H33 H 0.3895 0.4849 0.5189 0.056 Uiso 1 1 calc R . . C34 C 0.4672(4) 0.4598(3) 0.3570(3) 0.0452(9) Uani 1 1 d . . . H34 H 0.4905 0.5236 0.3217 0.054 Uiso 1 1 calc R . . C35 C 0.4813(3) 0.3689(3) 0.3123(2) 0.0354(8) Uani 1 1 d . . . H35 H 0.5173 0.3587 0.2383 0.042 Uiso 1 1 calc R . . C41 C 0.5690(3) 0.0926(2) 0.3275(2) 0.0250(6) Uani 1 1 d . . . C42 C 0.6017(3) 0.0095(2) 0.2612(2) 0.0246(6) Uani 1 1 d . . . H42 H 0.5378 0.0115 0.2375 0.030 Uiso 1 1 calc R . . C43 C 0.7216(3) -0.0765(3) 0.2271(2) 0.0263(7) Uani 1 1 d . . . C44 C 0.8143(3) -0.0757(3) 0.2629(2) 0.0311(7) Uani 1 1 d . . . H44 H 0.8970 -0.1322 0.2427 0.037 Uiso 1 1 calc R . . C45 C 0.7872(3) 0.0060(3) 0.3270(2) 0.0304(7) Uani 1 1 d . . . H45 H 0.8513 0.0054 0.3495 0.036 Uiso 1 1 calc R . . C46 C 0.6673(3) 0.0883(3) 0.3583(2) 0.0291(7) Uani 1 1 d . . . H46 H 0.6508 0.1438 0.4019 0.035 Uiso 1 1 calc R . . C51 C 0.7526(3) 0.4218(3) 0.1053(3) 0.0451(9) Uani 1 1 d . . . C52 C 0.7773(3) 0.3054(3) 0.1354(3) 0.0444(9) Uani 1 1 d . . . H52 H 0.8181 0.2658 0.1893 0.053 Uiso 1 1 calc R . . C53 C 0.7439(4) 0.2455(3) 0.0887(3) 0.0482(9) Uani 1 1 d . . . H53 H 0.7610 0.1655 0.1111 0.058 Uiso 1 1 calc R . . C54 C 0.6857(4) 0.3011(4) 0.0099(3) 0.0578(11) Uani 1 1 d . . . H54 H 0.6629 0.2600 -0.0227 0.069 Uiso 1 1 calc R . . C55 C 0.6614(4) 0.4167(4) -0.0209(3) 0.0612(11) Uani 1 1 d . . . H55 H 0.6223 0.4556 -0.0760 0.073 Uiso 1 1 calc R . . C56 C 0.6928(4) 0.4774(4) 0.0268(3) 0.0549(10) Uani 1 1 d . . . H56 H 0.6734 0.5578 0.0056 0.066 Uiso 1 1 calc R . . C57 C 0.7879(4) 0.4872(4) 0.1569(4) 0.0694(12) Uani 1 1 d . . . H57A H 0.8318 0.5324 0.1012 0.104 Uiso 1 1 calc R . . H57B H 0.8428 0.4324 0.1997 0.104 Uiso 1 1 calc R . . H57C H 0.7122 0.5394 0.2034 0.104 Uiso 1 1 calc R . . C61 C 0.8654(4) 0.2269(4) 0.5208(3) 0.0591(11) Uani 1 1 d . . . C62 C 0.8618(4) 0.3054(4) 0.5759(4) 0.0676(12) Uani 1 1 d . . . H62 H 0.8605 0.3793 0.5406 0.081 Uiso 1 1 calc R . . C63 C 0.8600(4) 0.2762(4) 0.6839(4) 0.0655(12) Uani 1 1 d . . . H63 H 0.8559 0.3306 0.7223 0.079 Uiso 1 1 calc R . . C64 C 0.8643(4) 0.1682(4) 0.7337(3) 0.0610(11) Uani 1 1 d . . . H64 H 0.8650 0.1474 0.8063 0.073 Uiso 1 1 calc R . . C65 C 0.8677(4) 0.0908(4) 0.6793(4) 0.0674(12) Uani 1 1 d . . . H65 H 0.8693 0.0168 0.7145 0.081 Uiso 1 1 calc R . . C66 C 0.8690(4) 0.1196(4) 0.5746(4) 0.0663(12) Uani 1 1 d . . . H66 H 0.8724 0.0644 0.5375 0.080 Uiso 1 1 calc R . . C67 C 0.8668(6) 0.2574(6) 0.4049(4) 0.0960(19) Uani 1 1 d . . . H67A H 0.9131 0.1871 0.3685 0.144 Uiso 1 1 calc R . . H67B H 0.9076 0.3125 0.3700 0.144 Uiso 1 1 calc R . . H67C H 0.7808 0.2923 0.4009 0.144 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 0.0310(3) 0.0331(3) 0.0232(2) -0.00662(18) -0.00480(18) -0.0119(2) B1 0.0268(19) 0.0286(19) 0.0327(18) -0.0073(15) -0.0081(15) -0.0099(16) O1 0.0362(12) 0.0244(12) 0.0226(10) 0.0000(9) -0.0033(9) -0.0157(10) C1 0.0368(18) 0.0383(18) 0.0282(15) -0.0044(13) -0.0076(13) -0.0174(16) C2 0.047(2) 0.054(2) 0.0308(17) -0.0079(16) -0.0086(15) -0.0206(19) C3 0.049(2) 0.040(2) 0.0350(17) 0.0044(15) -0.0125(15) -0.0185(18) C4 0.047(2) 0.045(2) 0.0347(17) -0.0036(15) -0.0062(15) -0.0237(18) B2 0.0347(19) 0.0237(17) 0.0217(15) -0.0014(13) -0.0076(14) -0.0132(16) C5 0.0332(17) 0.0331(17) 0.0313(15) -0.0055(13) -0.0118(13) -0.0112(15) C6 0.0364(19) 0.044(2) 0.056(2) -0.0136(17) -0.0190(17) -0.0027(17) C7 0.0371(19) 0.049(2) 0.0473(19) -0.0102(16) -0.0132(16) -0.0197(17) C8 0.051(2) 0.051(2) 0.0356(17) 0.0028(15) -0.0243(16) -0.0208(19) N11 0.0290(14) 0.0283(13) 0.0277(12) -0.0060(10) -0.0085(11) -0.0109(11) N12 0.0296(14) 0.0327(14) 0.0264(12) -0.0034(10) -0.0032(10) -0.0171(12) C13 0.0311(18) 0.0371(18) 0.0458(19) -0.0063(15) -0.0075(15) -0.0199(16) C14 0.044(2) 0.050(2) 0.057(2) -0.0060(17) -0.0227(18) -0.0257(19) C15 0.0376(19) 0.0388(19) 0.0353(16) -0.0041(14) -0.0183(15) -0.0151(16) N21 0.0292(14) 0.0278(14) 0.0277(12) -0.0042(10) -0.0067(11) -0.0121(12) N22 0.0328(15) 0.0299(14) 0.0273(12) -0.0010(10) -0.0091(11) -0.0097(13) C23 0.0406(19) 0.0312(18) 0.0365(16) -0.0018(14) -0.0142(15) -0.0117(16) C24 0.0310(18) 0.0335(18) 0.0487(19) -0.0119(15) -0.0083(15) -0.0013(15) C25 0.0293(17) 0.0330(18) 0.0324(16) -0.0114(14) -0.0018(14) -0.0067(15) N31 0.0342(15) 0.0217(13) 0.0233(12) -0.0024(10) -0.0069(11) -0.0098(12) N32 0.0371(15) 0.0323(15) 0.0300(13) -0.0106(11) -0.0062(11) -0.0111(13) C33 0.062(3) 0.038(2) 0.0448(19) -0.0139(16) -0.0034(17) -0.0277(19) C34 0.057(2) 0.0338(19) 0.0448(19) -0.0002(15) -0.0030(17) -0.0290(18) C35 0.042(2) 0.0320(17) 0.0291(15) -0.0018(13) -0.0024(14) -0.0195(16) C41 0.0300(16) 0.0243(15) 0.0223(13) 0.0023(11) -0.0094(12) -0.0130(14) C42 0.0281(16) 0.0252(15) 0.0211(13) 0.0019(11) -0.0079(12) -0.0126(13) C43 0.0298(16) 0.0268(16) 0.0223(13) 0.0000(12) -0.0065(12) -0.0133(14) C44 0.0243(16) 0.0333(17) 0.0345(15) -0.0037(13) -0.0073(13) -0.0113(14) C45 0.0292(17) 0.0323(17) 0.0345(15) -0.0032(13) -0.0113(13) -0.0150(14) C46 0.0346(18) 0.0286(17) 0.0287(15) -0.0049(13) -0.0099(13) -0.0148(15) C51 0.0363(19) 0.048(2) 0.0484(19) -0.0118(17) -0.0024(16) -0.0188(18) C52 0.040(2) 0.046(2) 0.0380(18) -0.0068(16) -0.0042(15) -0.0139(17) C53 0.051(2) 0.044(2) 0.0448(19) -0.0113(16) -0.0033(17) -0.0187(19) C54 0.057(3) 0.068(3) 0.054(2) -0.024(2) -0.012(2) -0.023(2) C55 0.058(3) 0.069(3) 0.050(2) -0.006(2) -0.019(2) -0.015(2) C56 0.051(2) 0.047(2) 0.053(2) 0.0010(18) -0.0118(19) -0.013(2) C57 0.071(3) 0.058(3) 0.093(3) -0.018(2) -0.026(3) -0.030(2) C61 0.050(2) 0.068(3) 0.060(2) -0.007(2) -0.016(2) -0.024(2) C62 0.067(3) 0.054(3) 0.084(3) -0.006(2) -0.024(2) -0.026(2) C63 0.065(3) 0.073(3) 0.072(3) -0.010(2) -0.026(2) -0.033(3) C64 0.044(2) 0.075(3) 0.060(2) 0.001(2) -0.0178(19) -0.022(2) C65 0.067(3) 0.060(3) 0.072(3) -0.005(2) -0.012(2) -0.029(2) C66 0.057(3) 0.070(3) 0.076(3) -0.017(2) -0.007(2) -0.033(2) C67 0.107(4) 0.136(5) 0.060(3) -0.005(3) -0.027(3) -0.060(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 O1 1.975(2) . ? Fe1 N22 2.037(2) . ? Fe1 N12 2.038(3) . ? Fe1 N32 2.058(3) . ? B1 N11 1.581(4) . ? B1 N21 1.601(4) . ? B1 C43 1.625(4) 2_656 ? B1 C1 1.655(4) . ? O1 B2 1.532(4) . ? O1 H1 0.828(10) . ? C1 C4 1.535(5) . ? C1 C2 1.544(4) . ? C1 C3 1.548(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? B2 N31 1.584(4) . ? B2 C41 1.631(4) . ? B2 C5 1.633(5) . ? C5 C7 1.528(5) . ? C5 C6 1.537(4) . ? C5 C8 1.547(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N11 C15 1.351(4) . ? N11 N12 1.379(3) . ? N12 C13 1.316(4) . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.358(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N21 C25 1.335(4) . ? N21 N22 1.375(3) . ? N22 C23 1.323(4) . ? C23 C24 1.378(4) . ? C23 H23 0.9500 . ? C24 C25 1.378(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N31 C35 1.335(4) . ? N31 N32 1.371(3) . ? N32 C33 1.329(4) . ? C33 C34 1.392(5) . ? C33 H33 0.9500 . ? C34 C35 1.372(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C42 1.401(4) . ? C41 C46 1.407(4) . ? C42 C43 1.405(4) . ? C42 H42 0.9500 . ? C43 C44 1.413(4) . ? C43 B1 1.625(4) 2_656 ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.381(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.379(5) . ? C51 C56 1.385(5) . ? C51 C57 1.500(5) . ? C52 C53 1.379(5) . ? C52 H52 0.9500 . ? C53 C54 1.376(5) . ? C53 H53 0.9500 . ? C54 C55 1.372(6) . ? C54 H54 0.9500 . ? C55 C56 1.379(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 C62 1.383(6) . ? C61 C66 1.383(6) . ? C61 C67 1.508(6) . ? C62 C63 1.404(6) . ? C62 H62 0.9500 . ? C63 C64 1.374(6) . ? C63 H63 0.9500 . ? C64 C65 1.364(6) . ? C64 H64 0.9500 . ? C65 C66 1.363(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? 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 O1 Fe1 N22 134.17(10) . . ? O1 Fe1 N12 129.82(10) . . ? N22 Fe1 N12 92.08(10) . . ? O1 Fe1 N32 80.39(9) . . ? N22 Fe1 N32 109.17(10) . . ? N12 Fe1 N32 104.90(11) . . ? N11 B1 N21 105.8(2) . . ? N11 B1 C43 107.3(2) . 2_656 ? N21 B1 C43 105.8(2) . 2_656 ? N11 B1 C1 112.2(3) . . ? N21 B1 C1 112.5(2) . . ? C43 B1 C1 112.7(3) 2_656 . ? B2 O1 Fe1 122.53(18) . . ? B2 O1 H1 121(3) . . ? Fe1 O1 H1 116(3) . . ? C4 C1 C2 107.5(3) . . ? C4 C1 C3 106.0(3) . . ? C2 C1 C3 107.9(3) . . ? C4 C1 B1 110.4(3) . . ? C2 C1 B1 115.3(3) . . ? C3 C1 B1 109.4(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 B2 N31 100.6(2) . . ? O1 B2 C41 106.9(2) . . ? N31 B2 C41 107.2(3) . . ? O1 B2 C5 109.0(3) . . ? N31 B2 C5 110.2(2) . . ? C41 B2 C5 121.0(2) . . ? C7 C5 C6 106.3(3) . . ? C7 C5 C8 109.5(3) . . ? C6 C5 C8 107.2(3) . . ? C7 C5 B2 112.2(2) . . ? C6 C5 B2 109.8(3) . . ? C8 C5 B2 111.6(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 N11 N12 106.9(3) . . ? C15 N11 B1 135.7(2) . . ? N12 N11 B1 117.4(2) . . ? C13 N12 N11 107.6(3) . . ? C13 N12 Fe1 136.5(2) . . ? N11 N12 Fe1 115.17(19) . . ? N12 C13 C14 110.6(3) . . ? N12 C13 H13 124.7 . . ? C14 C13 H13 124.7 . . ? C15 C14 C13 104.7(3) . . ? C15 C14 H14 127.7 . . ? C13 C14 H14 127.7 . . ? N11 C15 C14 110.2(3) . . ? N11 C15 H15 124.9 . . ? C14 C15 H15 124.9 . . ? C25 N21 N22 108.3(2) . . ? C25 N21 B1 134.9(2) . . ? N22 N21 B1 116.7(2) . . ? C23 N22 N21 106.7(2) . . ? C23 N22 Fe1 137.4(2) . . ? N21 N22 Fe1 115.95(18) . . ? N22 C23 C24 111.2(3) . . ? N22 C23 H23 124.4 . . ? C24 C23 H23 124.4 . . ? C23 C24 C25 104.2(3) . . ? C23 C24 H24 127.9 . . ? C25 C24 H24 127.9 . . ? N21 C25 C24 109.6(3) . . ? N21 C25 H25 125.2 . . ? C24 C25 H25 125.2 . . ? C35 N31 N32 109.1(2) . . ? C35 N31 B2 130.1(2) . . ? N32 N31 B2 120.8(2) . . ? C33 N32 N31 106.5(2) . . ? C33 N32 Fe1 138.7(2) . . ? N31 N32 Fe1 114.38(19) . . ? N32 C33 C34 110.7(3) . . ? N32 C33 H33 124.7 . . ? C34 C33 H33 124.7 . . ? C35 C34 C33 104.4(3) . . ? C35 C34 H34 127.8 . . ? C33 C34 H34 127.8 . . ? N31 C35 C34 109.4(3) . . ? N31 C35 H35 125.3 . . ? C34 C35 H35 125.3 . . ? C42 C41 C46 115.5(3) . . ? C42 C41 B2 125.7(3) . . ? C46 C41 B2 118.5(3) . . ? C41 C42 C43 125.1(3) . . ? C41 C42 H42 117.5 . . ? C43 C42 H42 117.5 . . ? C42 C43 C44 115.8(3) . . ? C42 C43 B1 123.4(3) . 2_656 ? C44 C43 B1 120.7(3) . 2_656 ? C45 C44 C43 121.3(3) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 C44 120.3(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 122.0(3) . . ? C45 C46 H46 119.0 . . ? C41 C46 H46 119.0 . . ? C52 C51 C56 118.1(4) . . ? C52 C51 C57 121.2(4) . . ? C56 C51 C57 120.7(4) . . ? C53 C52 C51 121.2(4) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C54 C53 C52 120.3(4) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C55 C54 C53 118.9(4) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 121.0(4) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C55 C56 C51 120.5(4) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C62 C61 C66 118.2(4) . . ? C62 C61 C67 120.7(5) . . ? C66 C61 C67 121.1(5) . . ? C61 C62 C63 120.2(4) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C64 C63 C62 119.4(4) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C65 C64 C63 120.4(4) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C66 C65 C64 120.1(5) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 121.8(4) . . ? C65 C66 H66 119.1 . . ? C61 C66 H66 119.1 . . ? C61 C67 H67A 109.5 . . ? C61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 Fe1 O1 B2 99.8(2) . . . . ? N12 Fe1 O1 B2 -109.1(2) . . . . ? N32 Fe1 O1 B2 -7.7(2) . . . . ? N11 B1 C1 C4 -175.2(3) . . . . ? N21 B1 C1 C4 65.6(3) . . . . ? C43 B1 C1 C4 -53.9(3) 2_656 . . . ? N11 B1 C1 C2 62.9(3) . . . . ? N21 B1 C1 C2 -56.3(4) . . . . ? C43 B1 C1 C2 -175.8(3) 2_656 . . . ? N11 B1 C1 C3 -58.9(3) . . . . ? N21 B1 C1 C3 -178.1(3) . . . . ? C43 B1 C1 C3 62.4(3) 2_656 . . . ? Fe1 O1 B2 N31 11.7(3) . . . . ? Fe1 O1 B2 C41 123.5(2) . . . . ? Fe1 O1 B2 C5 -104.1(2) . . . . ? O1 B2 C5 C7 -55.1(3) . . . . ? N31 B2 C5 C7 -164.6(2) . . . . ? C41 B2 C5 C7 69.4(3) . . . . ? O1 B2 C5 C6 62.9(3) . . . . ? N31 B2 C5 C6 -46.6(3) . . . . ? C41 B2 C5 C6 -172.6(3) . . . . ? O1 B2 C5 C8 -178.4(3) . . . . ? N31 B2 C5 C8 72.1(3) . . . . ? C41 B2 C5 C8 -53.9(4) . . . . ? N21 B1 N11 C15 112.0(3) . . . . ? C43 B1 N11 C15 -135.4(3) 2_656 . . . ? C1 B1 N11 C15 -11.1(5) . . . . ? N21 B1 N11 N12 -68.1(3) . . . . ? C43 B1 N11 N12 44.5(3) 2_656 . . . ? C1 B1 N11 N12 168.9(2) . . . . ? C15 N11 N12 C13 0.2(3) . . . . ? B1 N11 N12 C13 -179.7(2) . . . . ? C15 N11 N12 Fe1 -171.65(19) . . . . ? B1 N11 N12 Fe1 8.4(3) . . . . ? O1 Fe1 N12 C13 73.2(3) . . . . ? N22 Fe1 N12 C13 -127.1(3) . . . . ? N32 Fe1 N12 C13 -16.6(3) . . . . ? O1 Fe1 N12 N11 -118.13(19) . . . . ? N22 Fe1 N12 N11 41.6(2) . . . . ? N32 Fe1 N12 N11 152.05(19) . . . . ? N11 N12 C13 C14 0.2(4) . . . . ? Fe1 N12 C13 C14 169.5(2) . . . . ? N12 C13 C14 C15 -0.5(4) . . . . ? N12 N11 C15 C14 -0.6(3) . . . . ? B1 N11 C15 C14 179.4(3) . . . . ? C13 C14 C15 N11 0.7(4) . . . . ? N11 B1 N21 C25 -119.5(4) . . . . ? C43 B1 N21 C25 126.8(4) 2_656 . . . ? C1 B1 N21 C25 3.3(5) . . . . ? N11 B1 N21 N22 63.5(3) . . . . ? C43 B1 N21 N22 -50.2(3) 2_656 . . . ? C1 B1 N21 N22 -173.6(3) . . . . ? C25 N21 N22 C23 0.3(4) . . . . ? B1 N21 N22 C23 178.0(3) . . . . ? C25 N21 N22 Fe1 -179.2(2) . . . . ? B1 N21 N22 Fe1 -1.4(3) . . . . ? O1 Fe1 N22 C23 -66.3(4) . . . . ? N12 Fe1 N22 C23 135.4(3) . . . . ? N32 Fe1 N22 C23 28.9(4) . . . . ? O1 Fe1 N22 N21 112.9(2) . . . . ? N12 Fe1 N22 N21 -45.3(2) . . . . ? N32 Fe1 N22 N21 -151.9(2) . . . . ? N21 N22 C23 C24 -0.2(4) . . . . ? Fe1 N22 C23 C24 179.0(3) . . . . ? N22 C23 C24 C25 0.1(4) . . . . ? N22 N21 C25 C24 -0.2(4) . . . . ? B1 N21 C25 C24 -177.3(3) . . . . ? C23 C24 C25 N21 0.0(4) . . . . ? O1 B2 N31 C35 170.5(3) . . . . ? C41 B2 N31 C35 58.9(4) . . . . ? C5 B2 N31 C35 -74.6(4) . . . . ? O1 B2 N31 N32 -11.4(3) . . . . ? C41 B2 N31 N32 -123.0(3) . . . . ? C5 B2 N31 N32 103.5(3) . . . . ? C35 N31 N32 C33 -0.4(4) . . . . ? B2 N31 N32 C33 -178.9(3) . . . . ? C35 N31 N32 Fe1 -174.4(2) . . . . ? B2 N31 N32 Fe1 7.1(3) . . . . ? O1 Fe1 N32 C33 -171.1(4) . . . . ? N22 Fe1 N32 C33 55.3(4) . . . . ? N12 Fe1 N32 C33 -42.3(4) . . . . ? O1 Fe1 N32 N31 0.1(2) . . . . ? N22 Fe1 N32 N31 -133.5(2) . . . . ? N12 Fe1 N32 N31 128.9(2) . . . . ? N31 N32 C33 C34 0.5(4) . . . . ? Fe1 N32 C33 C34 172.1(3) . . . . ? N32 C33 C34 C35 -0.3(4) . . . . ? N32 N31 C35 C34 0.2(4) . . . . ? B2 N31 C35 C34 178.5(3) . . . . ? C33 C34 C35 N31 0.1(4) . . . . ? O1 B2 C41 C42 104.9(3) . . . . ? N31 B2 C41 C42 -147.9(3) . . . . ? C5 B2 C41 C42 -20.6(4) . . . . ? O1 B2 C41 C46 -67.9(3) . . . . ? N31 B2 C41 C46 39.3(3) . . . . ? C5 B2 C41 C46 166.6(3) . . . . ? C46 C41 C42 C43 1.7(4) . . . . ? B2 C41 C42 C43 -171.3(3) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? C41 C42 C43 B1 -177.5(3) . . . 2_656 ? C42 C43 C44 C45 -0.4(4) . . . . ? B1 C43 C44 C45 176.4(3) 2_656 . . . ? C43 C44 C45 C46 0.7(4) . . . . ? C44 C45 C46 C41 0.3(5) . . . . ? C42 C41 C46 C45 -1.4(4) . . . . ? B2 C41 C46 C45 172.1(3) . . . . ? C56 C51 C52 C53 0.1(5) . . . . ? C57 C51 C52 C53 179.4(4) . . . . ? C51 C52 C53 C54 0.6(6) . . . . ? C52 C53 C54 C55 -0.2(6) . . . . ? C53 C54 C55 C56 -0.8(6) . . . . ? C54 C55 C56 C51 1.5(6) . . . . ? C52 C51 C56 C55 -1.2(5) . . . . ? C57 C51 C56 C55 179.5(4) . . . . ? C66 C61 C62 C63 -0.9(7) . . . . ? C67 C61 C62 C63 179.8(4) . . . . ? C61 C62 C63 C64 1.2(7) . . . . ? C62 C63 C64 C65 -1.3(7) . . . . ? C63 C64 C65 C66 1.1(7) . . . . ? C64 C65 C66 C61 -0.7(7) . . . . ? C62 C61 C66 C65 0.7(7) . . . . ? C67 C61 C66 C65 180.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.281 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.052 # Attachment 'compd4xTHF.cif' data_wa398 _database_code_depnum_ccdc_archive 'CCDC 645748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H72 B4 Co2 N12 O3' _chemical_formula_weight 1050.30 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P bcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.9069(12) _cell_length_b 15.2037(12) _cell_length_c 25.5526(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5402.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9006 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.1 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8406 _exptl_absorpt_correction_T_max 0.9184 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17052 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4715 _reflns_number_gt 3049 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0600P)^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 SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4715 _refine_ls_number_parameters 317 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.098 _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 Co1 Co 0.51185(4) 0.61328(4) 0.61346(2) 0.02406(19) Uani 1 1 d . . . O1 O 0.4731(2) 0.6832(2) 0.67368(13) 0.0247(7) Uani 1 1 d . . . H1 H 0.509(5) 0.697(4) 0.694(3) 0.06(2) Uiso 1 1 d . . . B1 B 0.7211(4) 0.5544(3) 0.59823(19) 0.0231(11) Uani 1 1 d . . . C1 C 0.8349(4) 0.5245(3) 0.59397(19) 0.0303(11) Uani 1 1 d . . . C1A C 0.8574(4) 0.4563(4) 0.6374(2) 0.0444(14) Uani 1 1 d . . . H1A1 H 0.8167 0.4043 0.6327 0.067 Uiso 1 1 calc R . . H1A2 H 0.8445 0.4824 0.6718 0.067 Uiso 1 1 calc R . . H1A3 H 0.9252 0.4391 0.6353 0.067 Uiso 1 1 calc R . . C1B C 0.8671(4) 0.4837(4) 0.5411(2) 0.0410(13) Uani 1 1 d . . . H1B1 H 0.8263 0.4329 0.5330 0.061 Uiso 1 1 calc R . . H1B2 H 0.9342 0.4647 0.5438 0.061 Uiso 1 1 calc R . . H1B3 H 0.8610 0.5277 0.5133 0.061 Uiso 1 1 calc R . . C1C C 0.9020(4) 0.6032(4) 0.6047(2) 0.0470(14) Uani 1 1 d . . . H1C1 H 0.8909 0.6489 0.5783 0.071 Uiso 1 1 calc R . . H1C2 H 0.9691 0.5837 0.6029 0.071 Uiso 1 1 calc R . . H1C3 H 0.8887 0.6270 0.6396 0.071 Uiso 1 1 calc R . . B2 B 0.3676(4) 0.7070(3) 0.6838(2) 0.0219(11) Uani 1 1 d . . . C2 C 0.3482(3) 0.8096(3) 0.66611(17) 0.0235(10) Uani 1 1 d . . . C2A C 0.3821(4) 0.8227(3) 0.60931(19) 0.0326(11) Uani 1 1 d . . . H2A1 H 0.3468 0.7825 0.5862 0.049 Uiso 1 1 calc R . . H2A2 H 0.4511 0.8103 0.6069 0.049 Uiso 1 1 calc R . . H2A3 H 0.3698 0.8835 0.5986 0.049 Uiso 1 1 calc R . . C2B C 0.4058(4) 0.8742(3) 0.69998(18) 0.0309(11) Uani 1 1 d . . . H2B1 H 0.3861 0.8682 0.7366 0.046 Uiso 1 1 calc R . . H2B2 H 0.3936 0.9344 0.6881 0.046 Uiso 1 1 calc R . . H2B3 H 0.4746 0.8611 0.6968 0.046 Uiso 1 1 calc R . . C2C C 0.2403(4) 0.8355(3) 0.6689(2) 0.0354(12) Uani 1 1 d . . . H2C1 H 0.2024 0.7949 0.6475 0.053 Uiso 1 1 calc R . . H2C2 H 0.2321 0.8956 0.6558 0.053 Uiso 1 1 calc R . . H2C3 H 0.2184 0.8325 0.7053 0.053 Uiso 1 1 calc R . . N11 N 0.6482(3) 0.4751(2) 0.58893(14) 0.0234(8) Uani 1 1 d . . . N12 N 0.5528(3) 0.4904(2) 0.59777(15) 0.0273(9) Uani 1 1 d . . . C13 C 0.5044(4) 0.4158(3) 0.5874(2) 0.0403(13) Uani 1 1 d . . . H13 H 0.4367 0.4088 0.5899 0.048 Uiso 1 1 calc R . . C14 C 0.5686(5) 0.3509(3) 0.5726(2) 0.0454(14) Uani 1 1 d . . . H14 H 0.5542 0.2917 0.5637 0.055 Uiso 1 1 calc R . . C15 C 0.6585(4) 0.3906(3) 0.57367(19) 0.0349(12) Uani 1 1 d . . . H15 H 0.7176 0.3628 0.5651 0.042 Uiso 1 1 calc R . . N21 N 0.6903(3) 0.6268(2) 0.55528(13) 0.0237(8) Uani 1 1 d . . . N22 N 0.6015(3) 0.6649(2) 0.56028(14) 0.0228(8) Uani 1 1 d . . . C23 C 0.5944(4) 0.7263(3) 0.52332(17) 0.0293(11) Uani 1 1 d . . . H23 H 0.5402 0.7635 0.5184 0.035 Uiso 1 1 calc R . . C24 C 0.6766(4) 0.7285(3) 0.49320(18) 0.0347(12) Uani 1 1 d . . . H24 H 0.6898 0.7656 0.4641 0.042 Uiso 1 1 calc R . . C25 C 0.7355(4) 0.6648(3) 0.51465(18) 0.0302(11) Uani 1 1 d . . . H25 H 0.7981 0.6502 0.5026 0.036 Uiso 1 1 calc R . . N31 N 0.3163(3) 0.6430(2) 0.64258(13) 0.0221(8) Uani 1 1 d . . . N32 N 0.3675(3) 0.6078(2) 0.60192(13) 0.0256(8) Uani 1 1 d . . . C33 C 0.3050(4) 0.5642(3) 0.57175(18) 0.0289(11) Uani 1 1 d . . . H33 H 0.3213 0.5326 0.5409 0.035 Uiso 1 1 calc R . . C34 C 0.2128(4) 0.5718(3) 0.59209(19) 0.0314(11) Uani 1 1 d . . . H34 H 0.1549 0.5482 0.5782 0.038 Uiso 1 1 calc R . . C35 C 0.2240(3) 0.6216(3) 0.63706(18) 0.0281(10) Uani 1 1 d . . . H35 H 0.1737 0.6378 0.6603 0.034 Uiso 1 1 calc R . . C41 C 0.3398(3) 0.6720(3) 0.74213(16) 0.0210(10) Uani 1 1 d . . . C42 C 0.3076(3) 0.7226(3) 0.78487(17) 0.0221(10) Uani 1 1 d . . . H42 H 0.2961 0.7836 0.7798 0.027 Uiso 1 1 calc R . . C43 C 0.2920(3) 0.6868(3) 0.83400(17) 0.0234(10) Uani 1 1 d . . . H43 H 0.2715 0.7246 0.8614 0.028 Uiso 1 1 calc R . . C44 C 0.3051(3) 0.5975(3) 0.84509(16) 0.0209(9) Uani 1 1 d . . . C45 C 0.3369(4) 0.5460(3) 0.80253(17) 0.0262(11) Uani 1 1 d . . . H45 H 0.3471 0.4848 0.8076 0.031 Uiso 1 1 calc R . . C46 C 0.3536(4) 0.5820(3) 0.75321(18) 0.0257(10) Uani 1 1 d . . . H46 H 0.3752 0.5445 0.7259 0.031 Uiso 1 1 calc R . . O51 O 0.0000 0.8429(10) 0.7500 0.188(6) Uiso 1 2 d S . . C52 C 0.0334(9) 0.7761(7) 0.7918(5) 0.148(5) Uiso 1 1 d D . . H52A H 0.0394 0.8054 0.8262 0.178 Uiso 1 1 d R . . H52B H 0.0965 0.7509 0.7819 0.178 Uiso 1 1 d R . . C53 C -0.0379(8) 0.7078(7) 0.7942(4) 0.047(3) Uiso 0.50 1 d PD . . H53A H -0.1021 0.7310 0.8035 0.057 Uiso 0.50 1 d PR . . H53B H -0.0208 0.6579 0.8173 0.057 Uiso 0.50 1 d PR . . C54 C -0.0276(17) 0.6846(9) 0.7370(5) 0.116(8) Uiso 0.50 1 d PD . . H54A H -0.0802 0.6451 0.7257 0.140 Uiso 0.50 1 d PR . . H54B H 0.0348 0.6557 0.7297 0.140 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0267(3) 0.0243(3) 0.0212(3) 0.0002(3) 0.0053(3) 0.0006(3) O1 0.0214(19) 0.0350(17) 0.0178(15) -0.0004(13) -0.0024(15) 0.0038(14) B1 0.030(3) 0.022(2) 0.017(3) -0.0027(19) 0.001(2) 0.004(2) C1 0.028(3) 0.034(3) 0.029(2) -0.005(2) 0.002(2) 0.008(2) C1A 0.047(4) 0.051(3) 0.036(3) -0.003(3) -0.009(3) 0.019(3) C1B 0.038(3) 0.047(3) 0.038(3) -0.009(2) 0.006(3) 0.008(2) C1C 0.032(3) 0.054(3) 0.055(4) -0.016(3) 0.006(3) -0.005(3) B2 0.016(3) 0.031(3) 0.019(2) 0.000(2) -0.003(2) 0.000(2) C2 0.024(3) 0.027(2) 0.020(2) 0.0042(18) -0.005(2) -0.0038(18) C2A 0.040(3) 0.032(2) 0.026(2) 0.007(2) -0.003(2) -0.003(2) C2B 0.038(3) 0.029(2) 0.026(2) 0.0045(19) 0.002(2) -0.006(2) C2C 0.028(3) 0.034(3) 0.044(3) 0.010(2) 0.000(2) 0.006(2) N11 0.032(2) 0.0204(18) 0.0175(18) -0.0018(14) 0.0004(18) 0.0030(16) N12 0.033(2) 0.0219(19) 0.027(2) 0.0005(15) 0.0022(18) -0.0031(16) C13 0.036(3) 0.031(2) 0.054(3) 0.003(2) -0.001(3) -0.007(2) C14 0.052(4) 0.025(3) 0.060(4) -0.008(2) -0.006(3) -0.003(2) C15 0.049(3) 0.019(2) 0.036(3) -0.008(2) 0.000(2) 0.007(2) N21 0.031(2) 0.022(2) 0.0181(18) -0.0034(15) 0.0032(16) 0.0023(16) N22 0.025(2) 0.0231(19) 0.0204(19) 0.0014(15) 0.0018(17) 0.0022(15) C23 0.044(3) 0.022(2) 0.021(2) 0.0011(18) 0.001(2) 0.003(2) C24 0.052(4) 0.032(3) 0.020(2) 0.007(2) 0.008(2) -0.003(2) C25 0.037(3) 0.030(3) 0.023(2) 0.0005(19) 0.010(2) -0.002(2) N31 0.026(2) 0.0267(18) 0.0138(17) 0.0020(15) 0.0026(17) -0.0002(15) N32 0.031(2) 0.0290(19) 0.0163(18) 0.0010(15) 0.0017(15) 0.0008(17) C33 0.040(3) 0.028(2) 0.018(2) 0.0002(18) -0.006(2) -0.006(2) C34 0.038(3) 0.030(2) 0.027(2) 0.003(2) -0.007(2) -0.010(2) C35 0.027(3) 0.033(2) 0.025(2) 0.007(2) -0.001(2) -0.007(2) C41 0.024(3) 0.023(2) 0.016(2) 0.0026(16) -0.0002(19) 0.0033(18) C42 0.024(3) 0.022(2) 0.021(2) 0.0018(17) 0.002(2) 0.0019(17) C43 0.023(3) 0.028(2) 0.019(2) -0.0042(18) 0.0024(19) 0.0003(18) C44 0.024(2) 0.019(2) 0.020(2) 0.0020(16) -0.0025(19) -0.0032(17) C45 0.038(3) 0.020(2) 0.021(2) 0.0020(17) -0.004(2) -0.0013(19) C46 0.036(3) 0.025(2) 0.017(2) -0.0023(18) 0.000(2) 0.0026(18) _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 Co1 O1 1.946(3) . ? Co1 N12 1.994(4) . ? Co1 N22 2.005(4) . ? Co1 N32 2.031(4) . ? O1 B2 1.532(6) . ? O1 H1 0.75(7) . ? B1 N11 1.594(6) . ? B1 N21 1.612(6) . ? B1 C44 1.630(6) 3_656 ? B1 C1 1.650(7) . ? C1 C1C 1.542(7) . ? C1 C1A 1.552(7) . ? C1 C1B 1.552(7) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? B2 N31 1.601(6) . ? B2 C41 1.631(6) . ? B2 C2 1.646(6) . ? C2 C2B 1.535(6) . ? C2 C2A 1.539(6) . ? C2 C2C 1.553(7) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? N11 C15 1.351(6) . ? N11 N12 1.366(6) . ? N12 C13 1.345(6) . ? C13 C14 1.384(8) . ? C13 H13 0.9500 . ? C14 C15 1.389(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N21 C25 1.344(6) . ? N21 N22 1.370(5) . ? N22 C23 1.332(6) . ? C23 C24 1.378(7) . ? C23 H23 0.9500 . ? C24 C25 1.382(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N31 C35 1.332(6) . ? N31 N32 1.369(5) . ? N32 C33 1.338(6) . ? C33 C34 1.388(7) . ? C33 H33 0.9500 . ? C34 C35 1.385(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C41 C46 1.409(6) . ? C41 C42 1.409(6) . ? C42 C43 1.385(6) . ? C42 H42 0.9500 . ? C43 C44 1.400(6) . ? C43 H43 0.9500 . ? C44 C45 1.411(6) . ? C44 B1 1.630(6) 3_656 ? C45 C46 1.394(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? O51 C52 1.544(14) . ? O51 C52 1.545(14) 3_556 ? C52 C53 1.438(9) . ? C52 C54 1.575(9) 3_556 ? C52 H52A 0.9900 . ? C52 H52B 0.9902 . ? C53 C54 1.26(2) 3_556 ? C53 C54 1.511(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9901 . ? C54 C54 1.02(4) 3_556 ? C54 C53 1.26(2) 3_556 ? C54 C52 1.575(9) 3_556 ? C54 H54A 0.9899 . ? C54 H54B 0.9899 . ? 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 O1 Co1 N12 138.56(14) . . ? O1 Co1 N22 119.64(14) . . ? N12 Co1 N22 93.04(15) . . ? O1 Co1 N32 82.15(14) . . ? N12 Co1 N32 102.38(16) . . ? N22 Co1 N32 122.20(15) . . ? B2 O1 Co1 121.8(3) . . ? B2 O1 H1 117(5) . . ? Co1 O1 H1 121(5) . . ? N11 B1 N21 104.2(3) . . ? N11 B1 C44 107.1(4) . 3_656 ? N21 B1 C44 105.8(3) . 3_656 ? N11 B1 C1 113.1(4) . . ? N21 B1 C1 113.5(4) . . ? C44 B1 C1 112.6(4) 3_656 . ? C1C C1 C1A 105.6(4) . . ? C1C C1 C1B 106.9(4) . . ? C1A C1 C1B 107.3(4) . . ? C1C C1 B1 110.8(4) . . ? C1A C1 B1 109.3(4) . . ? C1B C1 B1 116.4(4) . . ? C1 C1A H1A1 109.5 . . ? C1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1 C1B H1B1 109.5 . . ? C1 C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C1 C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C1 C1C H1C1 109.5 . . ? C1 C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C1 C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? O1 B2 N31 100.0(3) . . ? O1 B2 C41 107.7(4) . . ? N31 B2 C41 107.3(3) . . ? O1 B2 C2 109.6(4) . . ? N31 B2 C2 108.8(3) . . ? C41 B2 C2 121.4(4) . . ? C2B C2 C2A 106.8(4) . . ? C2B C2 C2C 108.4(4) . . ? C2A C2 C2C 107.9(4) . . ? C2B C2 B2 111.5(4) . . ? C2A C2 B2 109.3(4) . . ? C2C C2 B2 112.8(4) . . ? C2 C2A H2A1 109.5 . . ? C2 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C2 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C2 C2B H2B1 109.5 . . ? C2 C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C2 C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C2 C2C H2C1 109.5 . . ? C2 C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? C2 C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? C15 N11 N12 108.2(4) . . ? C15 N11 B1 134.1(4) . . ? N12 N11 B1 117.7(3) . . ? C13 N12 N11 108.1(4) . . ? C13 N12 Co1 133.4(4) . . ? N11 N12 Co1 118.0(3) . . ? N12 C13 C14 109.4(5) . . ? N12 C13 H13 125.3 . . ? C14 C13 H13 125.3 . . ? C13 C14 C15 105.4(5) . . ? C13 C14 H14 127.3 . . ? C15 C14 H14 127.3 . . ? N11 C15 C14 108.9(5) . . ? N11 C15 H15 125.6 . . ? C14 C15 H15 125.6 . . ? C25 N21 N22 108.1(4) . . ? C25 N21 B1 134.0(4) . . ? N22 N21 B1 117.7(3) . . ? C23 N22 N21 107.3(4) . . ? C23 N22 Co1 135.1(3) . . ? N21 N22 Co1 117.3(3) . . ? N22 C23 C24 110.6(4) . . ? N22 C23 H23 124.7 . . ? C24 C23 H23 124.7 . . ? C23 C24 C25 104.7(4) . . ? C23 C24 H24 127.7 . . ? C25 C24 H24 127.7 . . ? N21 C25 C24 109.3(4) . . ? N21 C25 H25 125.4 . . ? C24 C25 H25 125.4 . . ? C35 N31 N32 109.0(4) . . ? C35 N31 B2 130.4(4) . . ? N32 N31 B2 120.3(4) . . ? C33 N32 N31 107.1(4) . . ? C33 N32 Co1 138.3(3) . . ? N31 N32 Co1 112.8(3) . . ? N32 C33 C34 110.1(4) . . ? N32 C33 H33 125.0 . . ? C34 C33 H33 125.0 . . ? C35 C34 C33 104.6(4) . . ? C35 C34 H34 127.7 . . ? C33 C34 H34 127.7 . . ? N31 C35 C34 109.3(4) . . ? N31 C35 H35 125.4 . . ? C34 C35 H35 125.4 . . ? C46 C41 C42 114.7(4) . . ? C46 C41 B2 117.9(4) . . ? C42 C41 B2 127.3(4) . . ? C43 C42 C41 122.5(4) . . ? C43 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C42 C43 C44 123.0(4) . . ? C42 C43 H43 118.5 . . ? C44 C43 H43 118.5 . . ? C43 C44 C45 115.0(4) . . ? C43 C44 B1 122.7(4) . 3_656 ? C45 C44 B1 122.2(4) . 3_656 ? C46 C45 C44 122.1(4) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C46 C41 122.7(4) . . ? C45 C46 H46 118.6 . . ? C41 C46 H46 118.6 . . ? C52 O51 C52 97.8(13) . 3_556 ? C53 C52 O51 107.3(11) . . ? C53 C52 C54 49.2(10) . 3_556 ? O51 C52 C54 104.1(12) . 3_556 ? C53 C52 H52A 110.1 . . ? O51 C52 H52A 110.2 . . ? C54 C52 H52A 144.6 3_556 . ? C53 C52 H52B 110.1 . . ? O51 C52 H52B 110.2 . . ? C54 C52 H52B 65.5 3_556 . ? H52A C52 H52B 108.9 . . ? C54 C53 C52 71.1(8) 3_556 . ? C54 C53 C54 41.8(18) 3_556 . ? C52 C53 C54 93.5(10) . . ? C54 C53 H53A 154.7 3_556 . ? C52 C53 H53A 112.0 . . ? C54 C53 H53A 113.7 . . ? C54 C53 H53B 89.4 3_556 . ? C52 C53 H53B 114.5 . . ? C54 C53 H53B 112.1 . . ? H53A C53 H53B 110.3 . . ? C54 C54 C53 82(2) 3_556 3_556 ? C54 C54 C53 55.7(13) 3_556 . ? C53 C54 C53 128.0(17) 3_556 . ? C54 C54 C52 110.1(14) 3_556 3_556 ? C53 C54 C52 59.7(6) 3_556 3_556 ? C53 C54 C52 103.9(11) . 3_556 ? C54 C54 H54A 138.5 3_556 . ? C53 C54 H54A 121.4 3_556 . ? C53 C54 H54A 110.6 . . ? C52 C54 H54A 111.3 3_556 . ? C54 C54 H54B 57.5 3_556 . ? C53 C54 H54B 51.1 3_556 . ? C53 C54 H54B 111.6 . . ? C52 C54 H54B 110.5 3_556 . ? H54A C54 H54B 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Co1 O1 B2 -103.7(4) . . . . ? N22 Co1 O1 B2 118.8(3) . . . . ? N32 Co1 O1 B2 -3.9(3) . . . . ? N11 B1 C1 C1C -178.6(4) . . . . ? N21 B1 C1 C1C 63.0(5) . . . . ? C44 B1 C1 C1C -57.1(5) 3_656 . . . ? N11 B1 C1 C1A -62.6(5) . . . . ? N21 B1 C1 C1A 179.0(4) . . . . ? C44 B1 C1 C1A 59.0(5) 3_656 . . . ? N11 B1 C1 C1B 59.1(5) . . . . ? N21 B1 C1 C1B -59.3(5) . . . . ? C44 B1 C1 C1B -179.4(4) 3_656 . . . ? Co1 O1 B2 N31 11.9(4) . . . . ? Co1 O1 B2 C41 123.8(3) . . . . ? Co1 O1 B2 C2 -102.2(3) . . . . ? O1 B2 C2 C2B -64.6(5) . . . . ? N31 B2 C2 C2B -172.9(4) . . . . ? C41 B2 C2 C2B 62.0(6) . . . . ? O1 B2 C2 C2A 53.3(5) . . . . ? N31 B2 C2 C2A -55.1(5) . . . . ? C41 B2 C2 C2A 179.8(4) . . . . ? O1 B2 C2 C2C 173.2(4) . . . . ? N31 B2 C2 C2C 64.9(5) . . . . ? C41 B2 C2 C2C -60.2(5) . . . . ? N21 B1 N11 C15 116.4(5) . . . . ? C44 B1 N11 C15 -131.8(5) 3_656 . . . ? C1 B1 N11 C15 -7.2(7) . . . . ? N21 B1 N11 N12 -64.0(4) . . . . ? C44 B1 N11 N12 47.8(5) 3_656 . . . ? C1 B1 N11 N12 172.3(4) . . . . ? C15 N11 N12 C13 -0.7(5) . . . . ? B1 N11 N12 C13 179.7(4) . . . . ? C15 N11 N12 Co1 -173.5(3) . . . . ? B1 N11 N12 Co1 6.8(5) . . . . ? O1 Co1 N12 C13 85.5(5) . . . . ? N22 Co1 N12 C13 -130.6(5) . . . . ? N32 Co1 N12 C13 -6.7(5) . . . . ? O1 Co1 N12 N11 -103.9(3) . . . . ? N22 Co1 N12 N11 40.0(3) . . . . ? N32 Co1 N12 N11 164.0(3) . . . . ? N11 N12 C13 C14 1.0(6) . . . . ? Co1 N12 C13 C14 172.3(4) . . . . ? N12 C13 C14 C15 -1.0(6) . . . . ? N12 N11 C15 C14 0.0(6) . . . . ? B1 N11 C15 C14 179.6(5) . . . . ? C13 C14 C15 N11 0.6(6) . . . . ? N11 B1 N21 C25 -118.9(5) . . . . ? C44 B1 N21 C25 128.3(5) 3_656 . . . ? C1 B1 N21 C25 4.5(7) . . . . ? N11 B1 N21 N22 65.7(4) . . . . ? C44 B1 N21 N22 -47.1(5) 3_656 . . . ? C1 B1 N21 N22 -170.9(4) . . . . ? C25 N21 N22 C23 -1.0(5) . . . . ? B1 N21 N22 C23 175.6(4) . . . . ? C25 N21 N22 Co1 174.1(3) . . . . ? B1 N21 N22 Co1 -9.4(5) . . . . ? O1 Co1 N22 C23 -71.6(5) . . . . ? N12 Co1 N22 C23 135.0(4) . . . . ? N32 Co1 N22 C23 28.3(5) . . . . ? O1 Co1 N22 N21 115.1(3) . . . . ? N12 Co1 N22 N21 -38.3(3) . . . . ? N32 Co1 N22 N21 -145.0(3) . . . . ? N21 N22 C23 C24 1.1(5) . . . . ? Co1 N22 C23 C24 -172.7(3) . . . . ? N22 C23 C24 C25 -0.8(5) . . . . ? N22 N21 C25 C24 0.5(5) . . . . ? B1 N21 C25 C24 -175.3(4) . . . . ? C23 C24 C25 N21 0.2(5) . . . . ? O1 B2 N31 C35 168.4(4) . . . . ? C41 B2 N31 C35 56.1(6) . . . . ? C2 B2 N31 C35 -76.9(5) . . . . ? O1 B2 N31 N32 -18.7(5) . . . . ? C41 B2 N31 N32 -130.9(4) . . . . ? C2 B2 N31 N32 96.0(4) . . . . ? C35 N31 N32 C33 -0.3(5) . . . . ? B2 N31 N32 C33 -174.6(4) . . . . ? C35 N31 N32 Co1 -167.8(3) . . . . ? B2 N31 N32 Co1 17.9(4) . . . . ? O1 Co1 N32 C33 -169.5(5) . . . . ? N12 Co1 N32 C33 -31.4(5) . . . . ? N22 Co1 N32 C33 70.3(5) . . . . ? O1 Co1 N32 N31 -7.6(3) . . . . ? N12 Co1 N32 N31 130.5(3) . . . . ? N22 Co1 N32 N31 -127.8(3) . . . . ? N31 N32 C33 C34 0.9(5) . . . . ? Co1 N32 C33 C34 163.4(4) . . . . ? N32 C33 C34 C35 -1.1(5) . . . . ? N32 N31 C35 C34 -0.4(5) . . . . ? B2 N31 C35 C34 173.2(4) . . . . ? C33 C34 C35 N31 0.9(5) . . . . ? O1 B2 C41 C46 -56.2(5) . . . . ? N31 B2 C41 C46 50.6(5) . . . . ? C2 B2 C41 C46 176.4(4) . . . . ? O1 B2 C41 C42 120.0(5) . . . . ? N31 B2 C41 C42 -133.2(5) . . . . ? C2 B2 C41 C42 -7.4(7) . . . . ? C46 C41 C42 C43 0.8(7) . . . . ? B2 C41 C42 C43 -175.5(4) . . . . ? C41 C42 C43 C44 -1.2(7) . . . . ? C42 C43 C44 C45 0.8(7) . . . . ? C42 C43 C44 B1 -175.2(4) . . . 3_656 ? C43 C44 C45 C46 -0.1(7) . . . . ? B1 C44 C45 C46 176.0(4) 3_656 . . . ? C44 C45 C46 C41 -0.3(8) . . . . ? C42 C41 C46 C45 0.0(7) . . . . ? B2 C41 C46 C45 176.6(4) . . . . ? C52 O51 C52 C53 -42.9(7) 3_556 . . . ? C52 O51 C52 C54 8.2(9) 3_556 . . 3_556 ? O51 C52 C53 C54 93.9(13) . . . 3_556 ? O51 C52 C53 C54 58.0(14) . . . . ? C54 C52 C53 C54 -35.9(14) 3_556 . . . ? C52 C53 C54 C54 56.3(9) . . . 3_556 ? C54 C53 C54 C53 -43(2) 3_556 . . 3_556 ? C52 C53 C54 C53 13(2) . . . 3_556 ? C54 C53 C54 C52 -105.1(18) 3_556 . . 3_556 ? C52 C53 C54 C52 -48.8(17) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.836 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.083