Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'David J. Mihalcik' 'Jennifer L. White' 'Joseph M. Tanski' 'Lev N. Zakharov' 'Glenn P. A. Yap' 'Christopher D. Incarvito' 'Arnold L. Rheingold' 'Daniel Rabinovich' _publ_contact_author_name 'Prof. Lev Zakharov' _publ_contact_author_email lz@chem.ucsd.edu data_drab37a _database_code_depnum_ccdc_archive 'CCDC 229395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.5 H40 B1 Cl1 Co1 N6 S3' _chemical_formula_weight 607.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 35.234(2) _cell_length_b 35.516(2) _cell_length_c 9.4836(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11867.3(12) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 0.90 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.918 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18911 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.26 _reflns_number_total 6304 _reflns_number_gt 5866 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0562P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.049(14) _refine_ls_number_reflns 6304 _refine_ls_number_parameters 302 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.129727(11) 0.146593(11) 0.74389(4) 0.01524(10) Uani 1 1 d . . . S1 S 0.08414(2) 0.18022(2) 0.62181(8) 0.01857(16) Uani 1 1 d . . . S2 S 0.10009(2) 0.09507(2) 0.84263(9) 0.01918(16) Uani 1 1 d . . . S3 S 0.17451(2) 0.12327(2) 0.58852(9) 0.01872(16) Uani 1 1 d . . . Cl1 Cl 0.15599(2) 0.18601(2) 0.89920(8) 0.01979(16) Uani 1 1 d . . . B1 B 0.08607(11) 0.09111(10) 0.4816(4) 0.0205(7) Uani 1 1 d . . . H1B H 0.0738(10) 0.0731(9) 0.407(4) 0.013(8) Uiso 1 1 d . . . N1 N 0.09615(8) 0.12903(8) 0.4097(3) 0.0183(5) Uani 1 1 d . . . N2 N 0.11103(8) 0.18696(7) 0.3497(3) 0.0177(5) Uani 1 1 d . . . N3 N 0.05643(8) 0.09434(7) 0.6018(3) 0.0185(5) Uani 1 1 d . . . N4 N 0.02282(8) 0.09899(8) 0.7966(3) 0.0213(6) Uani 1 1 d . . . N5 N 0.12196(8) 0.06838(7) 0.5302(3) 0.0188(6) Uani 1 1 d . . . N6 N 0.17543(8) 0.04556(7) 0.6129(3) 0.0189(5) Uani 1 1 d . . . C1 C 0.10885(10) 0.12840(9) 0.2716(3) 0.0205(7) Uani 1 1 d . . . H1A H 0.1109 0.1067 0.2133 0.025 Uiso 1 1 calc R . . C2 C 0.11790(10) 0.16410(9) 0.2343(4) 0.0222(7) Uani 1 1 d . . . H2A H 0.1272 0.1720 0.1451 0.027 Uiso 1 1 calc R . . C3 C 0.09754(9) 0.16521(9) 0.4570(3) 0.0178(6) Uani 1 1 d . . . C4 C 0.12271(10) 0.22793(9) 0.3580(4) 0.0213(7) Uani 1 1 d . . . C5 C 0.08914(11) 0.25228(9) 0.4018(4) 0.0300(8) Uani 1 1 d . . . H5A H 0.0685 0.2493 0.3333 0.045 Uiso 1 1 calc R . . H5B H 0.0970 0.2787 0.4051 0.045 Uiso 1 1 calc R . . H5C H 0.0803 0.2445 0.4953 0.045 Uiso 1 1 calc R . . C6 C 0.13531(12) 0.24056(10) 0.2115(4) 0.0304(8) Uani 1 1 d . . . H6A H 0.1140 0.2384 0.1457 0.046 Uiso 1 1 calc R . . H6B H 0.1563 0.2246 0.1793 0.046 Uiso 1 1 calc R . . H6C H 0.1438 0.2668 0.2155 0.046 Uiso 1 1 calc R . . C7 C 0.15640(10) 0.23082(10) 0.4606(4) 0.0267(8) Uani 1 1 d . . . H7A H 0.1772 0.2148 0.4273 0.040 Uiso 1 1 calc R . . H7B H 0.1484 0.2226 0.5546 0.040 Uiso 1 1 calc R . . H7C H 0.1651 0.2570 0.4653 0.040 Uiso 1 1 calc R . . C8 C 0.01831(9) 0.09656(9) 0.5651(4) 0.0237(7) Uani 1 1 d . . . H8A H 0.0084 0.0963 0.4718 0.028 Uiso 1 1 calc R . . C9 C -0.00203(10) 0.09904(9) 0.6835(4) 0.0237(7) Uani 1 1 d . . . H9A H -0.0289 0.1006 0.6892 0.028 Uiso 1 1 calc R . . C10 C 0.05885(9) 0.09634(8) 0.7445(4) 0.0179(6) Uani 1 1 d . . . C11 C 0.01128(11) 0.10359(12) 0.9478(4) 0.0311(8) Uani 1 1 d . . . C12 C 0.02443(13) 0.07021(14) 1.0338(5) 0.0441(11) Uani 1 1 d . . . H12A H 0.0522 0.0689 1.0321 0.066 Uiso 1 1 calc R . . H12B H 0.0139 0.0470 0.9936 0.066 Uiso 1 1 calc R . . H12C H 0.0157 0.0730 1.1313 0.066 Uiso 1 1 calc R . . C13 C -0.03236(12) 0.10485(16) 0.9523(5) 0.0509(13) Uani 1 1 d . . . H13A H -0.0426 0.0809 0.9175 0.076 Uiso 1 1 calc R . . H13B H -0.0415 0.1255 0.8927 0.076 Uiso 1 1 calc R . . H13C H -0.0408 0.1089 1.0496 0.076 Uiso 1 1 calc R . . C14 C 0.02714(12) 0.14130(12) 1.0007(5) 0.0413(10) Uani 1 1 d . . . H14A H 0.0549 0.1406 0.9980 0.062 Uiso 1 1 calc R . . H14B H 0.0186 0.1457 1.0977 0.062 Uiso 1 1 calc R . . H14C H 0.0180 0.1617 0.9400 0.062 Uiso 1 1 calc R . . C15 C 0.11812(10) 0.02949(9) 0.5432(4) 0.0231(7) Uani 1 1 d . . . H15A H 0.0961 0.0153 0.5206 0.028 Uiso 1 1 calc R . . C16 C 0.15083(10) 0.01549(8) 0.5931(4) 0.0224(7) Uani 1 1 d . . . H16A H 0.1562 -0.0103 0.6115 0.027 Uiso 1 1 calc R . . C17 C 0.15693(9) 0.07777(8) 0.5762(3) 0.0177(6) Uani 1 1 d . . . C18 C 0.21413(10) 0.04168(9) 0.6786(4) 0.0237(7) Uani 1 1 d . . . C19 C 0.22341(11) -0.00043(10) 0.6934(5) 0.0336(9) Uani 1 1 d . . . H19A H 0.2047 -0.0124 0.7553 0.050 Uiso 1 1 calc R . . H19B H 0.2488 -0.0034 0.7341 0.050 Uiso 1 1 calc R . . H19C H 0.2227 -0.0124 0.6003 0.050 Uiso 1 1 calc R . . C20 C 0.24410(10) 0.05992(10) 0.5820(5) 0.0307(8) Uani 1 1 d . . . H20A H 0.2388 0.0869 0.5727 0.046 Uiso 1 1 calc R . . H20B H 0.2432 0.0480 0.4888 0.046 Uiso 1 1 calc R . . H20C H 0.2694 0.0564 0.6231 0.046 Uiso 1 1 calc R . . C21 C 0.21316(11) 0.05967(10) 0.8252(4) 0.0305(8) Uani 1 1 d . . . H21A H 0.2071 0.0865 0.8163 0.046 Uiso 1 1 calc R . . H21B H 0.2380 0.0568 0.8703 0.046 Uiso 1 1 calc R . . H21C H 0.1937 0.0473 0.8827 0.046 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 Co1 0.0168(2) 0.01433(17) 0.01461(19) -0.00040(16) 0.00048(16) -0.00050(17) S1 0.0232(4) 0.0181(3) 0.0144(4) -0.0005(3) 0.0009(3) 0.0030(3) S2 0.0177(4) 0.0207(3) 0.0192(4) 0.0041(3) -0.0017(3) -0.0017(3) S3 0.0183(4) 0.0142(3) 0.0236(4) -0.0019(3) 0.0041(3) -0.0017(3) Cl1 0.0205(4) 0.0204(3) 0.0186(4) -0.0031(3) -0.0014(3) 0.0000(3) B1 0.0224(18) 0.0164(15) 0.0228(19) -0.0044(15) -0.0011(15) 0.0006(13) N1 0.0192(13) 0.0211(13) 0.0147(13) 0.0002(10) 0.0002(10) -0.0030(10) N2 0.0215(13) 0.0186(12) 0.0131(13) 0.0043(10) -0.0009(10) -0.0019(10) N3 0.0178(13) 0.0165(11) 0.0210(14) 0.0030(11) 0.0001(11) -0.0043(10) N4 0.0148(13) 0.0216(13) 0.0275(15) 0.0031(11) 0.0029(11) -0.0017(11) N5 0.0197(14) 0.0167(12) 0.0200(14) -0.0009(10) 0.0007(11) -0.0018(10) N6 0.0203(13) 0.0174(11) 0.0191(14) -0.0048(11) 0.0028(11) 0.0010(10) C1 0.0237(17) 0.0211(15) 0.0167(16) -0.0003(12) 0.0000(12) -0.0012(13) C2 0.0287(17) 0.0229(15) 0.0149(15) -0.0033(13) -0.0036(13) -0.0023(13) C3 0.0165(15) 0.0190(14) 0.0179(16) -0.0009(12) -0.0026(11) 0.0003(12) C4 0.0283(17) 0.0165(14) 0.0192(16) -0.0006(12) -0.0026(13) -0.0050(13) C5 0.039(2) 0.0177(15) 0.034(2) 0.0058(15) 0.0022(16) 0.0045(15) C6 0.041(2) 0.0278(17) 0.0225(19) 0.0024(15) 0.0027(15) -0.0079(16) C7 0.0269(18) 0.0250(16) 0.028(2) 0.0000(14) -0.0015(14) -0.0085(14) C8 0.0159(15) 0.0286(16) 0.0265(19) 0.0052(14) -0.0048(13) -0.0019(13) C9 0.0163(16) 0.0244(15) 0.0305(19) 0.0014(14) 0.0000(14) -0.0017(13) C10 0.0189(15) 0.0136(12) 0.0213(15) 0.0029(12) 0.0009(13) -0.0029(11) C11 0.0224(18) 0.049(2) 0.0219(17) 0.0011(16) 0.0085(14) -0.0027(16) C12 0.043(3) 0.060(3) 0.029(2) 0.0146(19) 0.0093(18) -0.007(2) C13 0.024(2) 0.092(4) 0.036(2) -0.006(2) 0.0131(17) 0.001(2) C14 0.040(2) 0.051(2) 0.033(2) -0.016(2) 0.0062(19) 0.0056(19) C15 0.0298(19) 0.0169(14) 0.0226(17) -0.0030(13) 0.0013(13) -0.0034(13) C16 0.0255(17) 0.0156(14) 0.0260(17) -0.0042(13) 0.0010(13) -0.0013(12) C17 0.0186(15) 0.0173(14) 0.0173(15) -0.0022(12) 0.0060(12) -0.0011(12) C18 0.0193(16) 0.0221(15) 0.0297(19) 0.0076(14) 0.0002(13) 0.0038(13) C19 0.0285(19) 0.0255(17) 0.047(3) 0.0136(17) -0.0001(17) 0.0041(15) C20 0.0212(17) 0.0318(17) 0.039(2) 0.0064(17) 0.0077(16) 0.0071(14) C21 0.0317(19) 0.0294(17) 0.030(2) 0.0062(16) -0.0060(16) -0.0026(15) _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 Cl1 2.2329(9) . ? Co1 S2 2.3058(9) . ? Co1 S1 2.3122(9) . ? Co1 S3 2.3124(9) . ? S1 C3 1.718(3) . ? S2 C10 1.726(3) . ? S3 C17 1.735(3) . ? B1 N3 1.550(5) . ? B1 N1 1.551(5) . ? B1 N5 1.569(5) . ? B1 H1B 1.04(3) . ? N1 C3 1.362(4) . ? N1 C1 1.383(4) . ? N2 C3 1.363(4) . ? N2 C2 1.385(4) . ? N2 C4 1.514(4) . ? N3 C10 1.358(4) . ? N3 C8 1.390(4) . ? N4 C10 1.365(4) . ? N4 C9 1.384(4) . ? N4 C11 1.500(5) . ? N5 C17 1.349(4) . ? N5 C15 1.393(4) . ? N6 C17 1.362(4) . ? N6 C16 1.388(4) . ? N6 C18 1.505(4) . ? C1 C2 1.354(4) . ? C1 H1A 0.9500 . ? C2 H2A 0.9500 . ? C4 C6 1.525(5) . ? C4 C5 1.523(5) . ? C4 C7 1.538(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 C9 1.335(5) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C11 C12 1.512(6) . ? C11 C14 1.535(6) . ? C11 C13 1.539(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.341(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C18 C21 1.530(5) . ? C18 C19 1.537(5) . ? C18 C20 1.541(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 Cl1 Co1 S2 114.67(3) . . ? Cl1 Co1 S1 107.12(3) . . ? S2 Co1 S1 107.38(3) . . ? Cl1 Co1 S3 111.23(3) . . ? S2 Co1 S3 106.47(3) . . ? S1 Co1 S3 109.87(3) . . ? C3 S1 Co1 96.00(11) . . ? C10 S2 Co1 98.14(11) . . ? C17 S3 Co1 97.64(11) . . ? N3 B1 N1 114.4(3) . . ? N3 B1 N5 111.4(3) . . ? N1 B1 N5 113.0(3) . . ? N3 B1 H1B 105.2(19) . . ? N1 B1 H1B 109.1(19) . . ? N5 B1 H1B 102.5(19) . . ? C3 N1 C1 108.4(3) . . ? C3 N1 B1 133.0(3) . . ? C1 N1 B1 118.5(3) . . ? C3 N2 C2 108.6(3) . . ? C3 N2 C4 127.0(3) . . ? C2 N2 C4 123.8(3) . . ? C10 N3 C8 107.9(3) . . ? C10 N3 B1 134.0(3) . . ? C8 N3 B1 118.1(3) . . ? C10 N4 C9 107.9(3) . . ? C10 N4 C11 127.2(3) . . ? C9 N4 C11 124.7(3) . . ? C17 N5 C15 107.7(3) . . ? C17 N5 B1 134.7(3) . . ? C15 N5 B1 117.3(3) . . ? C17 N6 C16 108.2(3) . . ? C17 N6 C18 128.1(3) . . ? C16 N6 C18 123.4(3) . . ? C2 C1 N1 108.0(3) . . ? C2 C1 H1A 126.0 . . ? N1 C1 H1A 126.0 . . ? C1 C2 N2 107.5(3) . . ? C1 C2 H2A 126.2 . . ? N2 C2 H2A 126.2 . . ? N1 C3 N2 107.6(3) . . ? N1 C3 S1 125.6(2) . . ? N2 C3 S1 126.8(2) . . ? N2 C4 C6 108.3(3) . . ? N2 C4 C5 110.4(3) . . ? C6 C4 C5 107.9(3) . . ? N2 C4 C7 107.8(3) . . ? C6 C4 C7 109.4(3) . . ? C5 C4 C7 112.9(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 N3 108.2(3) . . ? C9 C8 H8A 125.9 . . ? N3 C8 H8A 125.9 . . ? C8 C9 N4 108.2(3) . . ? C8 C9 H9A 125.9 . . ? N4 C9 H9A 125.9 . . ? N3 C10 N4 107.8(3) . . ? N3 C10 S2 126.1(2) . . ? N4 C10 S2 126.1(3) . . ? N4 C11 C12 110.3(3) . . ? N4 C11 C14 108.0(3) . . ? C12 C11 C14 113.4(4) . . ? N4 C11 C13 107.5(3) . . ? C12 C11 C13 108.3(4) . . ? C14 C11 C13 109.2(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N5 108.4(3) . . ? C16 C15 H15A 125.8 . . ? N5 C15 H15A 125.8 . . ? C15 C16 N6 107.4(3) . . ? C15 C16 H16A 126.3 . . ? N6 C16 H16A 126.3 . . ? N5 C17 N6 108.2(3) . . ? N5 C17 S3 125.3(2) . . ? N6 C17 S3 126.5(2) . . ? N6 C18 C21 108.5(3) . . ? N6 C18 C19 108.6(3) . . ? C21 C18 C19 109.2(3) . . ? N6 C18 C20 109.6(3) . . ? C21 C18 C20 112.3(3) . . ? C19 C18 C20 108.5(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.467 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.076 data_drab40 _database_code_depnum_ccdc_archive 'CCDC 229396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H36 B Br Cl2 Co N6 S3' _chemical_formula_weight 701.30 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5500(19) _cell_length_b 32.730(7) _cell_length_c 10.410(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.11(3) _cell_angle_gamma 90.00 _cell_volume 3035.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blade _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 2.288 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4614 _exptl_absorpt_correction_T_max 0.8035 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34253 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.36 _reflns_number_total 7205 _reflns_number_gt 5845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 7205 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 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 0.17325(6) 0.126264(15) 0.41457(5) 0.01878(15) Uani 1 1 d . . . Br1 Br 0.03336(5) 0.161184(12) 0.52948(5) 0.02944(15) Uani 1 1 d . . . S1 S 0.32944(11) 0.17133(3) 0.35905(10) 0.0204(2) Uani 1 1 d . . . S2 S 0.04051(11) 0.09154(3) 0.21093(10) 0.0225(2) Uani 1 1 d . . . S3 S 0.32546(10) 0.07931(3) 0.57052(9) 0.0204(2) Uani 1 1 d . . . N1 N 0.2598(4) 0.16864(9) 0.0769(3) 0.0199(6) Uani 1 1 d . . . N2 N 0.3534(4) 0.11157(9) 0.1820(3) 0.0207(6) Uani 1 1 d . . . N3 N 0.0916(3) 0.00955(9) 0.2666(3) 0.0195(6) Uani 1 1 d . . . N4 N 0.2946(4) 0.04383(9) 0.2811(3) 0.0199(6) Uani 1 1 d . . . N5 N 0.5171(3) 0.08931(9) 0.4300(3) 0.0197(6) Uani 1 1 d . . . N6 N 0.6100(3) 0.11200(9) 0.6434(3) 0.0191(6) Uani 1 1 d . . . C1 C 0.3149(4) 0.14987(11) 0.2021(4) 0.0195(7) Uani 1 1 d . . . C2 C 0.3224(4) 0.10647(12) 0.0441(4) 0.0239(8) Uani 1 1 d . . . H2A H 0.3407 0.0829 0.0028 0.029 Uiso 1 1 calc R . . C3 C 0.2612(5) 0.14102(12) -0.0223(4) 0.0246(8) Uani 1 1 d . . . H3A H 0.2265 0.1454 -0.1169 0.030 Uiso 1 1 calc R . . C4 C 0.2033(5) 0.21184(11) 0.0472(4) 0.0225(8) Uani 1 1 d . . . C5 C 0.3298(5) 0.24093(12) 0.1232(4) 0.0259(8) Uani 1 1 d . . . H5A H 0.3599 0.2364 0.2205 0.039 Uiso 1 1 calc R . . H5B H 0.2960 0.2686 0.1021 0.039 Uiso 1 1 calc R . . H5C H 0.4136 0.2361 0.0949 0.039 Uiso 1 1 calc R . . C6 C 0.1568(5) 0.21973(13) -0.1078(4) 0.0323(10) Uani 1 1 d . . . H6A H 0.0770 0.2015 -0.1574 0.048 Uiso 1 1 calc R . . H6B H 0.2413 0.2152 -0.1355 0.048 Uiso 1 1 calc R . . H6C H 0.1232 0.2475 -0.1277 0.048 Uiso 1 1 calc R . . C7 C 0.0659(5) 0.21712(12) 0.0879(4) 0.0258(8) Uani 1 1 d . . . H7A H 0.0938 0.2125 0.1850 0.039 Uiso 1 1 calc R . . H7B H -0.0101 0.1978 0.0382 0.039 Uiso 1 1 calc R . . H7C H 0.0275 0.2444 0.0662 0.039 Uiso 1 1 calc R . . C8 C 0.1450(4) 0.04714(11) 0.2519(4) 0.0195(7) Uani 1 1 d . . . C9 C 0.3348(4) 0.00400(11) 0.3178(4) 0.0216(8) Uani 1 1 d . . . H9A H 0.4317 -0.0064 0.3448 0.026 Uiso 1 1 calc R . . C10 C 0.2145(4) -0.01694(11) 0.3084(4) 0.0236(8) Uani 1 1 d . . . H10A H 0.2116 -0.0447 0.3265 0.028 Uiso 1 1 calc R . . C11 C -0.0696(4) -0.00300(11) 0.2326(4) 0.0205(7) Uani 1 1 d . . . C12 C -0.1402(5) 0.02043(13) 0.3193(5) 0.0301(9) Uani 1 1 d . . . H12A H -0.0852 0.0152 0.4151 0.045 Uiso 1 1 calc R . . H12B H -0.2424 0.0118 0.2963 0.045 Uiso 1 1 calc R . . H12C H -0.1376 0.0492 0.3016 0.045 Uiso 1 1 calc R . . C13 C -0.0720(4) -0.04878(11) 0.2630(4) 0.0242(8) Uani 1 1 d . . . H13A H -0.0286 -0.0638 0.2073 0.036 Uiso 1 1 calc R . . H13B H -0.1738 -0.0575 0.2420 0.036 Uiso 1 1 calc R . . H13C H -0.0152 -0.0537 0.3585 0.036 Uiso 1 1 calc R . . C14 C -0.1548(4) 0.00409(13) 0.0771(4) 0.0264(9) Uani 1 1 d . . . H14A H -0.1084 -0.0116 0.0253 0.040 Uiso 1 1 calc R . . H14B H -0.1515 0.0326 0.0564 0.040 Uiso 1 1 calc R . . H14C H -0.2574 -0.0043 0.0530 0.040 Uiso 1 1 calc R . . C15 C 0.4882(4) 0.09359(11) 0.5477(4) 0.0186(7) Uani 1 1 d . . . C16 C 0.6576(4) 0.10571(11) 0.4515(4) 0.0220(8) Uani 1 1 d . . . H16A H 0.7048 0.1066 0.3874 0.026 Uiso 1 1 calc R . . C17 C 0.7135(4) 0.12000(11) 0.5808(4) 0.0227(8) Uani 1 1 d . . . H17A H 0.8055 0.1330 0.6216 0.027 Uiso 1 1 calc R . . C18 C 0.6248(4) 0.12622(12) 0.7852(4) 0.0240(8) Uani 1 1 d . . . C19 C 0.6016(5) 0.09055(12) 0.8700(4) 0.0272(9) Uani 1 1 d . . . H19A H 0.5020 0.0799 0.8268 0.041 Uiso 1 1 calc R . . H19B H 0.6146 0.0999 0.9611 0.041 Uiso 1 1 calc R . . H19C H 0.6735 0.0695 0.8756 0.041 Uiso 1 1 calc R . . C20 C 0.7848(5) 0.14236(14) 0.8575(5) 0.0317(9) Uani 1 1 d . . . H20A H 0.8018 0.1651 0.8069 0.048 Uiso 1 1 calc R . . H20B H 0.8556 0.1211 0.8618 0.048 Uiso 1 1 calc R . . H20C H 0.7972 0.1510 0.9491 0.048 Uiso 1 1 calc R . . C21 C 0.5124(5) 0.16052(12) 0.7711(5) 0.0288(9) Uani 1 1 d . . . H21A H 0.5313 0.1824 0.7181 0.043 Uiso 1 1 calc R . . H21B H 0.5228 0.1704 0.8609 0.043 Uiso 1 1 calc R . . H21C H 0.4124 0.1504 0.7255 0.043 Uiso 1 1 calc R . . B1 B 0.4181(5) 0.07510(12) 0.2820(5) 0.0216(9) Uani 1 1 d . . . H10B H 0.4855 0.0604 0.2459 0.026 Uiso 1 1 calc R . . C22 C 0.7409(10) 0.2171(3) 0.2575(8) 0.089(3) Uani 1 1 d . . . H22A H 0.8430 0.2128 0.3208 0.106 Uiso 1 1 calc R . . H22B H 0.6805 0.2254 0.3105 0.106 Uiso 1 1 calc R . . Cl1 Cl 0.7383(2) 0.25631(6) 0.1370(3) 0.0882(7) Uani 1 1 d . . . Cl2 Cl 0.6695(2) 0.17106(5) 0.16950(17) 0.0670(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0207(3) 0.0143(3) 0.0219(3) -0.00102(18) 0.0083(2) 0.00086(18) Br1 0.0311(3) 0.0218(2) 0.0438(3) -0.00552(16) 0.0237(2) -0.00152(15) S1 0.0293(5) 0.0134(4) 0.0194(4) -0.0008(3) 0.0099(4) -0.0005(3) S2 0.0241(5) 0.0130(4) 0.0260(5) -0.0006(3) 0.0037(4) 0.0029(3) S3 0.0195(5) 0.0192(5) 0.0228(5) 0.0033(3) 0.0080(4) -0.0014(3) N1 0.0261(17) 0.0147(14) 0.0202(16) 0.0013(12) 0.0099(13) -0.0014(12) N2 0.0289(17) 0.0131(14) 0.0225(16) 0.0014(12) 0.0121(14) 0.0006(12) N3 0.0232(16) 0.0126(14) 0.0220(15) 0.0005(12) 0.0074(13) 0.0015(12) N4 0.0234(16) 0.0117(14) 0.0251(16) -0.0010(12) 0.0094(13) 0.0005(11) N5 0.0218(15) 0.0132(14) 0.0260(17) 0.0016(12) 0.0107(13) -0.0002(11) N6 0.0204(15) 0.0148(14) 0.0236(16) 0.0018(12) 0.0096(13) 0.0008(11) C1 0.0225(18) 0.0147(16) 0.0240(19) 0.0012(14) 0.0116(15) -0.0003(14) C2 0.033(2) 0.0190(19) 0.0223(19) -0.0044(15) 0.0137(17) -0.0022(15) C3 0.037(2) 0.0204(18) 0.0200(18) -0.0037(15) 0.0139(17) -0.0032(16) C4 0.030(2) 0.0119(16) 0.0235(19) 0.0035(14) 0.0068(16) -0.0001(14) C5 0.031(2) 0.0167(18) 0.030(2) 0.0019(15) 0.0104(17) -0.0041(15) C6 0.045(3) 0.024(2) 0.025(2) 0.0038(16) 0.0100(19) 0.0025(18) C7 0.026(2) 0.0150(17) 0.032(2) -0.0037(16) 0.0056(17) -0.0009(15) C8 0.0248(19) 0.0149(17) 0.0191(17) -0.0027(13) 0.0081(15) -0.0021(14) C9 0.0219(18) 0.0136(17) 0.0269(19) -0.0010(14) 0.0060(15) 0.0040(14) C10 0.027(2) 0.0130(17) 0.030(2) 0.0045(15) 0.0098(17) 0.0051(14) C11 0.0194(17) 0.0205(18) 0.0214(18) 0.0002(14) 0.0072(15) -0.0011(14) C12 0.031(2) 0.028(2) 0.033(2) -0.0048(17) 0.0147(19) 0.0005(17) C13 0.024(2) 0.0204(18) 0.029(2) -0.0017(15) 0.0107(16) -0.0043(15) C14 0.028(2) 0.024(2) 0.023(2) 0.0022(15) 0.0031(16) -0.0028(16) C15 0.0181(17) 0.0164(17) 0.0197(17) 0.0047(13) 0.0048(14) 0.0027(13) C16 0.0214(18) 0.0182(18) 0.030(2) 0.0055(15) 0.0137(16) 0.0008(14) C17 0.0187(18) 0.0162(17) 0.033(2) 0.0022(15) 0.0091(16) -0.0012(14) C18 0.024(2) 0.0219(19) 0.0222(19) -0.0015(15) 0.0032(16) -0.0001(15) C19 0.033(2) 0.0218(19) 0.024(2) 0.0035(15) 0.0070(17) 0.0014(16) C20 0.026(2) 0.030(2) 0.035(2) -0.0044(18) 0.0060(18) -0.0066(17) C21 0.032(2) 0.020(2) 0.032(2) 0.0016(16) 0.0074(18) 0.0053(16) B1 0.026(2) 0.0150(19) 0.024(2) -0.0010(16) 0.0100(18) -0.0005(16) C22 0.087(6) 0.094(6) 0.064(5) -0.022(4) 0.003(4) 0.018(5) Cl1 0.0739(12) 0.0567(10) 0.144(2) -0.0146(11) 0.0509(13) -0.0056(8) Cl2 0.0842(12) 0.0608(10) 0.0546(9) -0.0033(7) 0.0233(8) -0.0143(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 S1 2.3142(11) . ? Co1 S3 2.3261(12) . ? Co1 S2 2.3360(12) . ? Co1 Br1 2.3817(8) . ? S1 C1 1.737(4) . ? S2 C8 1.727(4) . ? S3 C15 1.720(4) . ? N1 C1 1.364(5) . ? N1 C3 1.376(5) . ? N1 C4 1.505(5) . ? N2 C1 1.344(5) . ? N2 C2 1.368(5) . ? N2 B1 1.558(5) . ? N3 C8 1.362(5) . ? N3 C10 1.397(5) . ? N3 C11 1.507(5) . ? N4 C8 1.354(5) . ? N4 C9 1.374(5) . ? N4 B1 1.559(5) . ? N5 C15 1.357(5) . ? N5 C16 1.386(5) . ? N5 B1 1.560(5) . ? N6 C15 1.369(5) . ? N6 C17 1.390(5) . ? N6 C18 1.505(5) . ? C2 C3 1.344(6) . ? C4 C5 1.518(5) . ? C4 C6 1.534(6) . ? C4 C7 1.527(6) . ? C9 C10 1.310(5) . ? C11 C12 1.515(6) . ? C11 C13 1.533(5) . ? C11 C14 1.546(5) . ? C16 C17 1.342(6) . ? C18 C19 1.527(6) . ? C18 C21 1.523(5) . ? C18 C20 1.534(6) . ? C22 Cl2 1.767(8) . ? C22 Cl1 1.789(9) . ? 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 S1 Co1 S3 107.36(4) . . ? S1 Co1 S2 105.74(4) . . ? S3 Co1 S2 108.08(4) . . ? S1 Co1 Br1 110.38(3) . . ? S3 Co1 Br1 106.81(4) . . ? S2 Co1 Br1 118.03(4) . . ? C1 S1 Co1 97.86(13) . . ? C8 S2 Co1 96.24(13) . . ? C15 S3 Co1 95.33(12) . . ? C1 N1 C3 108.5(3) . . ? C1 N1 C4 127.3(3) . . ? C3 N1 C4 124.2(3) . . ? C1 N2 C2 108.0(3) . . ? C1 N2 B1 132.5(3) . . ? C2 N2 B1 119.5(3) . . ? C8 N3 C10 106.8(3) . . ? C8 N3 C11 127.7(3) . . ? C10 N3 C11 125.2(3) . . ? C8 N4 C9 107.8(3) . . ? C8 N4 B1 133.2(3) . . ? C9 N4 B1 119.1(3) . . ? C15 N5 C16 108.3(3) . . ? C15 N5 B1 132.4(3) . . ? C16 N5 B1 118.8(3) . . ? C15 N6 C17 107.6(3) . . ? C15 N6 C18 127.2(3) . . ? C17 N6 C18 124.7(3) . . ? N2 C1 N1 107.7(3) . . ? N2 C1 S1 126.1(3) . . ? N1 C1 S1 126.1(3) . . ? C3 C2 N2 109.1(3) . . ? C2 C3 N1 106.6(3) . . ? N1 C4 C5 108.8(3) . . ? N1 C4 C6 108.7(3) . . ? C5 C4 C6 108.5(3) . . ? N1 C4 C7 109.2(3) . . ? C5 C4 C7 112.8(3) . . ? C6 C4 C7 108.7(3) . . ? N4 C8 N3 108.1(3) . . ? N4 C8 S2 126.3(3) . . ? N3 C8 S2 125.6(3) . . ? C10 C9 N4 109.0(3) . . ? C9 C10 N3 108.3(3) . . ? N3 C11 C12 111.0(3) . . ? N3 C11 C13 107.9(3) . . ? C12 C11 C13 109.2(3) . . ? N3 C11 C14 108.2(3) . . ? C12 C11 C14 111.6(3) . . ? C13 C11 C14 108.7(3) . . ? N5 C15 N6 107.9(3) . . ? N5 C15 S3 125.8(3) . . ? N6 C15 S3 126.4(3) . . ? C17 C16 N5 108.0(3) . . ? C16 C17 N6 108.2(3) . . ? N6 C18 C19 110.4(3) . . ? N6 C18 C21 108.6(3) . . ? C19 C18 C21 112.0(4) . . ? N6 C18 C20 108.2(3) . . ? C19 C18 C20 107.8(3) . . ? C21 C18 C20 109.6(3) . . ? N4 B1 N2 112.5(3) . . ? N4 B1 N5 113.0(3) . . ? N2 B1 N5 112.6(3) . . ? Cl2 C22 Cl1 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.988 _refine_diff_density_min -2.198 _refine_diff_density_rms 0.139 data_drab42 _database_code_depnum_ccdc_archive 'CCDC 229397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H34 B Co I N6 S3' _chemical_formula_weight 663.36 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.4384(12) _cell_length_b 16.788(2) _cell_length_c 16.2395(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.499(2) _cell_angle_gamma 90.00 _cell_volume 2845.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5763 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.35 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.929 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17307 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6567 _reflns_number_gt 4483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1173P)^2^+0.1142P] 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 6567 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _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 0.14452(6) 0.05995(4) 0.75768(4) 0.02629(17) Uani 1 1 d . . . I1 I -0.03388(3) 0.16532(2) 0.76958(3) 0.04650(15) Uani 1 1 d . . . S1 S 0.30708(11) 0.08628(7) 0.66392(7) 0.0285(3) Uani 1 1 d . . . S2 S 0.04805(11) -0.05919(7) 0.72250(7) 0.0275(3) Uani 1 1 d . . . S3 S 0.24856(11) 0.03832(8) 0.88202(7) 0.0295(3) Uani 1 1 d . . . B1 B 0.3698(5) -0.1012(3) 0.7456(3) 0.0265(11) Uani 1 1 d . . . H1B H 0.4331 -0.1455 0.7404 0.032 Uiso 1 1 calc R . . N1 N 0.3318(3) -0.0767(2) 0.6551(2) 0.0248(8) Uani 1 1 d . . . N2 N 0.2751(3) -0.0230(2) 0.5385(2) 0.0255(8) Uani 1 1 d . . . N3 N 0.2532(3) -0.1366(2) 0.7929(2) 0.0241(8) Uani 1 1 d . . . N4 N 0.0712(4) -0.1635(2) 0.8528(2) 0.0276(8) Uani 1 1 d . . . N5 N 0.4400(3) -0.0336(2) 0.7928(2) 0.0258(8) Uani 1 1 d . . . N6 N 0.5054(3) 0.0718(2) 0.8619(2) 0.0254(8) Uani 1 1 d . . . C1 C 0.3055(4) -0.0071(3) 0.6184(3) 0.0247(9) Uani 1 1 d . . . C2 C 0.3157(4) -0.1375(3) 0.5988(3) 0.0283(10) Uani 1 1 d . . . H2A H 0.3272 -0.1928 0.6091 0.034 Uiso 1 1 calc R . . C3 C 0.2809(4) -0.1044(3) 0.5272(3) 0.0289(10) Uani 1 1 d . . . H3A H 0.2633 -0.1320 0.4773 0.035 Uiso 1 1 calc R . . C4 C 0.2474(4) 0.0368(3) 0.4701(3) 0.0274(10) Uani 1 1 d . . . C5 C 0.2187(5) -0.0097(3) 0.3916(3) 0.0361(12) Uani 1 1 d . . . H5A H 0.2933 -0.0421 0.3771 0.054 Uiso 1 1 calc R . . H5B H 0.1996 0.0276 0.3466 0.054 Uiso 1 1 calc R . . H5C H 0.1446 -0.0445 0.4003 0.054 Uiso 1 1 calc R . . C6 C 0.1317(5) 0.0879(3) 0.4924(3) 0.0367(11) Uani 1 1 d . . . H6A H 0.1148 0.1263 0.4482 0.055 Uiso 1 1 calc R . . H6B H 0.1495 0.1166 0.5438 0.055 Uiso 1 1 calc R . . H6C H 0.0566 0.0537 0.4996 0.055 Uiso 1 1 calc R . . C7 C 0.3675(5) 0.0863(3) 0.4569(3) 0.0348(11) Uani 1 1 d . . . H7A H 0.4389 0.0511 0.4427 0.052 Uiso 1 1 calc R . . H7B H 0.3885 0.1154 0.5075 0.052 Uiso 1 1 calc R . . H7C H 0.3525 0.1242 0.4120 0.052 Uiso 1 1 calc R . . C8 C 0.1261(4) -0.1202(3) 0.7920(2) 0.0243(9) Uani 1 1 d . . . C9 C 0.2773(5) -0.1921(3) 0.8541(3) 0.0300(10) Uani 1 1 d . . . H9A H 0.3583 -0.2147 0.8674 0.036 Uiso 1 1 calc R . . C10 C 0.1654(5) -0.2086(3) 0.8919(3) 0.0316(10) Uani 1 1 d . . . H10A H 0.1535 -0.2442 0.9366 0.038 Uiso 1 1 calc R . . C11 C -0.0660(5) -0.1595(3) 0.8809(3) 0.0339(11) Uani 1 1 d . . . C12 C -0.1536(5) -0.1912(4) 0.8129(4) 0.0502(15) Uani 1 1 d . . . H12A H -0.1296 -0.2462 0.7998 0.075 Uiso 1 1 calc R . . H12B H -0.1448 -0.1580 0.7636 0.075 Uiso 1 1 calc R . . H12C H -0.2426 -0.1898 0.8314 0.075 Uiso 1 1 calc R . . C13 C -0.0811(5) -0.2122(4) 0.9567(3) 0.0491(15) Uani 1 1 d . . . H13A H -0.0252 -0.1926 1.0011 0.074 Uiso 1 1 calc R . . H13B H -0.0574 -0.2671 0.9429 0.074 Uiso 1 1 calc R . . H13C H -0.1704 -0.2108 0.9748 0.074 Uiso 1 1 calc R . . C14 C -0.0962(5) -0.0736(3) 0.9052(3) 0.0436(13) Uani 1 1 d . . . H14A H -0.0370 -0.0565 0.9489 0.065 Uiso 1 1 calc R . . H14B H -0.1844 -0.0704 0.9252 0.065 Uiso 1 1 calc R . . H14C H -0.0866 -0.0389 0.8572 0.065 Uiso 1 1 calc R . . C15 C 0.4020(4) 0.0256(3) 0.8443(2) 0.0250(9) Uani 1 1 d . . . C16 C 0.5696(4) -0.0231(3) 0.7788(3) 0.0292(10) Uani 1 1 d . . . H16A H 0.6216 -0.0562 0.7454 0.035 Uiso 1 1 calc R . . C17 C 0.6095(4) 0.0413(3) 0.8203(3) 0.0311(10) Uani 1 1 d . . . H17A H 0.6940 0.0623 0.8210 0.037 Uiso 1 1 calc R . . C18 C 0.5101(5) 0.1464(3) 0.9135(3) 0.0311(10) Uani 1 1 d . . . C19 C 0.4678(5) 0.1275(4) 1.0007(3) 0.0441(14) Uani 1 1 d . . . H19A H 0.5249 0.0872 1.0247 0.066 Uiso 1 1 calc R . . H19B H 0.3799 0.1071 0.9995 0.066 Uiso 1 1 calc R . . H19C H 0.4715 0.1760 1.0342 0.066 Uiso 1 1 calc R . . C20 C 0.6464(5) 0.1784(3) 0.9150(3) 0.0396(12) Uani 1 1 d . . . H20A H 0.7033 0.1393 0.9411 0.059 Uiso 1 1 calc R . . H20B H 0.6491 0.2283 0.9463 0.059 Uiso 1 1 calc R . . H20C H 0.6745 0.1882 0.8585 0.059 Uiso 1 1 calc R . . C21 C 0.4230(6) 0.2097(3) 0.8728(4) 0.0477(14) Uani 1 1 d . . . H21A H 0.3346 0.1902 0.8708 0.071 Uiso 1 1 calc R . . H21B H 0.4525 0.2202 0.8167 0.071 Uiso 1 1 calc R . . H21C H 0.4267 0.2591 0.9050 0.071 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 Co1 0.0249(3) 0.0276(4) 0.0265(3) -0.0008(2) 0.0073(2) 0.0018(2) I1 0.0322(2) 0.0320(2) 0.0756(3) -0.00070(17) 0.01460(17) 0.00490(14) S1 0.0363(6) 0.0235(6) 0.0261(5) -0.0014(4) 0.0117(5) -0.0003(5) S2 0.0267(6) 0.0291(6) 0.0266(5) 0.0033(5) 0.0022(4) -0.0005(5) S3 0.0227(5) 0.0405(7) 0.0254(5) -0.0052(5) 0.0094(4) 0.0001(5) B1 0.025(3) 0.032(3) 0.023(2) 0.000(2) 0.0098(19) 0.003(2) N1 0.0238(19) 0.030(2) 0.0211(17) 0.0014(15) 0.0091(14) 0.0002(16) N2 0.0269(19) 0.030(2) 0.0194(17) -0.0001(15) 0.0101(14) -0.0024(16) N3 0.027(2) 0.0245(19) 0.0206(17) 0.0049(15) 0.0055(14) -0.0015(16) N4 0.027(2) 0.030(2) 0.0260(19) 0.0029(16) 0.0073(15) -0.0038(16) N5 0.0235(19) 0.030(2) 0.0234(18) 0.0032(15) 0.0063(14) 0.0015(16) N6 0.0231(18) 0.031(2) 0.0222(18) -0.0021(15) 0.0039(14) -0.0006(16) C1 0.028(2) 0.025(2) 0.022(2) -0.0026(17) 0.0127(17) -0.0007(18) C2 0.032(2) 0.025(2) 0.028(2) -0.0059(19) 0.0125(19) -0.0039(19) C3 0.030(2) 0.029(2) 0.028(2) -0.0046(19) 0.0072(18) -0.0023(19) C4 0.027(2) 0.032(3) 0.024(2) 0.0055(18) 0.0088(17) 0.0016(19) C5 0.034(3) 0.049(3) 0.025(2) 0.001(2) 0.0069(19) 0.001(2) C6 0.028(3) 0.039(3) 0.043(3) 0.003(2) 0.002(2) 0.003(2) C7 0.033(3) 0.044(3) 0.027(2) 0.006(2) 0.0098(19) -0.008(2) C8 0.030(2) 0.022(2) 0.021(2) -0.0019(17) 0.0075(17) -0.0033(18) C9 0.030(2) 0.030(2) 0.029(2) 0.004(2) 0.0014(19) 0.000(2) C10 0.034(3) 0.029(3) 0.032(2) 0.010(2) 0.003(2) -0.001(2) C11 0.026(2) 0.039(3) 0.036(3) 0.008(2) 0.012(2) 0.000(2) C12 0.039(3) 0.061(4) 0.051(3) -0.004(3) 0.008(3) -0.019(3) C13 0.040(3) 0.056(4) 0.052(3) 0.018(3) 0.018(2) -0.010(3) C14 0.042(3) 0.045(3) 0.044(3) 0.002(2) 0.021(2) 0.007(3) C15 0.027(2) 0.029(2) 0.019(2) 0.0004(17) 0.0054(16) 0.0042(19) C16 0.021(2) 0.039(3) 0.028(2) 0.000(2) 0.0107(18) 0.001(2) C17 0.022(2) 0.037(3) 0.035(2) -0.001(2) 0.0126(19) 0.002(2) C18 0.030(2) 0.032(3) 0.032(2) -0.006(2) 0.0035(19) -0.004(2) C19 0.042(3) 0.063(4) 0.027(2) -0.006(2) 0.009(2) -0.011(3) C20 0.031(3) 0.043(3) 0.044(3) -0.008(2) -0.002(2) -0.007(2) C21 0.043(3) 0.034(3) 0.065(4) -0.006(3) -0.002(3) 0.006(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 Co1 S2 2.3089(14) . ? Co1 S3 2.3130(13) . ? Co1 S1 2.3319(12) . ? Co1 I1 2.5769(7) . ? S1 C1 1.734(4) . ? S2 C8 1.724(5) . ? S3 C15 1.733(4) . ? B1 N5 1.550(6) . ? B1 N3 1.562(6) . ? B1 N1 1.573(6) . ? N1 C1 1.339(6) . ? N1 C2 1.379(6) . ? N2 C1 1.360(5) . ? N2 C3 1.379(6) . ? N2 C4 1.523(6) . ? N3 C8 1.355(6) . ? N3 C9 1.384(6) . ? N4 C8 1.357(5) . ? N4 C10 1.390(6) . ? N4 C11 1.509(6) . ? N5 C15 1.360(6) . ? N5 C16 1.385(5) . ? N6 C15 1.358(6) . ? N6 C17 1.383(5) . ? N6 C18 1.507(6) . ? C2 C3 1.337(7) . ? C4 C7 1.521(6) . ? C4 C5 1.523(7) . ? C4 C6 1.529(6) . ? C9 C10 1.352(7) . ? C11 C13 1.525(7) . ? C11 C14 1.528(7) . ? C11 C12 1.524(7) . ? C16 C17 1.339(7) . ? C18 C19 1.521(7) . ? C18 C20 1.521(7) . ? C18 C21 1.545(7) . ? 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 S2 Co1 S3 106.29(5) . . ? S2 Co1 S1 108.71(5) . . ? S3 Co1 S1 105.13(5) . . ? S2 Co1 I1 107.42(4) . . ? S3 Co1 I1 112.11(4) . . ? S1 Co1 I1 116.70(4) . . ? C1 S1 Co1 95.90(14) . . ? C8 S2 Co1 98.65(15) . . ? C15 S3 Co1 97.99(15) . . ? N5 B1 N3 113.7(3) . . ? N5 B1 N1 112.7(4) . . ? N3 B1 N1 111.6(4) . . ? C1 N1 C2 109.1(4) . . ? C1 N1 B1 133.9(4) . . ? C2 N1 B1 117.0(4) . . ? C1 N2 C3 108.1(4) . . ? C1 N2 C4 127.4(4) . . ? C3 N2 C4 124.4(4) . . ? C8 N3 C9 108.4(4) . . ? C8 N3 B1 133.2(4) . . ? C9 N3 B1 118.2(4) . . ? C8 N4 C10 108.8(4) . . ? C8 N4 C11 127.2(4) . . ? C10 N4 C11 123.8(4) . . ? C15 N5 C16 107.4(4) . . ? C15 N5 B1 134.4(4) . . ? C16 N5 B1 118.1(4) . . ? C15 N6 C17 108.1(4) . . ? C15 N6 C18 127.9(4) . . ? C17 N6 C18 123.9(4) . . ? N1 C1 N2 107.4(4) . . ? N1 C1 S1 126.7(3) . . ? N2 C1 S1 125.9(3) . . ? C3 C2 N1 107.4(4) . . ? C2 C3 N2 108.0(4) . . ? C7 C4 C5 108.6(4) . . ? C7 C4 N2 108.1(4) . . ? C5 C4 N2 107.9(4) . . ? C7 C4 C6 112.4(4) . . ? C5 C4 C6 109.7(4) . . ? N2 C4 C6 110.1(4) . . ? N3 C8 N4 107.7(4) . . ? N3 C8 S2 125.8(3) . . ? N4 C8 S2 126.5(3) . . ? C10 C9 N3 108.1(4) . . ? C9 C10 N4 107.0(4) . . ? N4 C11 C13 108.9(4) . . ? N4 C11 C14 108.6(4) . . ? C13 C11 C14 108.4(4) . . ? N4 C11 C12 109.3(4) . . ? C13 C11 C12 108.5(4) . . ? C14 C11 C12 113.1(5) . . ? N5 C15 N6 108.1(4) . . ? N5 C15 S3 125.7(3) . . ? N6 C15 S3 126.2(3) . . ? C17 C16 N5 108.7(4) . . ? C16 C17 N6 107.7(4) . . ? N6 C18 C19 109.7(4) . . ? N6 C18 C20 109.1(4) . . ? C19 C18 C20 109.8(4) . . ? N6 C18 C21 108.5(4) . . ? C19 C18 C21 111.6(4) . . ? C20 C18 C21 108.1(4) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.908 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.133 data_drab44 _database_code_depnum_ccdc_archive 'CCDC 229398' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H74 B2 Co N12 S6' _chemical_formula_weight 1092.10 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 19.4434(12) _cell_length_b 19.4434(12) _cell_length_c 29.922(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11312.0(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1018 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 24.52 _exptl_crystal_description block _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4632 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35520 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6798 _reflns_number_gt 5279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0663P)^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 6798 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 0.5000 0.2500 0.096203(11) 0.02129(10) Uani 1 2 d S . . S1 S 0.42158(2) 0.28820(2) 0.040384(15) 0.02694(12) Uani 1 1 d . . . S2 S 0.44866(2) 0.15378(2) 0.130872(15) 0.02446(11) Uani 1 1 d . . . S3 S 0.73205(3) 0.04776(3) 0.180106(16) 0.03176(13) Uani 1 1 d . . . N1 N 0.32768(7) 0.31723(7) 0.10568(5) 0.0240(3) Uani 1 1 d . . . N2 N 0.27907(8) 0.27915(8) 0.04439(5) 0.0275(3) Uani 1 1 d . . . N3 N 0.57705(7) 0.09755(7) 0.12093(5) 0.0210(3) Uani 1 1 d . . . N4 N 0.49575(7) 0.03434(8) 0.09105(5) 0.0245(3) Uani 1 1 d . . . N5 N 0.64260(7) 0.15550(7) 0.18746(5) 0.0221(3) Uani 1 1 d . . . N6 N 0.69384(8) 0.12952(8) 0.25112(5) 0.0274(3) Uani 1 1 d . . . B1 B 0.61497(10) 0.16199(10) 0.13922(7) 0.0217(4) Uani 1 1 d . . . H1 H 0.5790(9) 0.2046(9) 0.1398(6) 0.017(4) Uiso 1 1 d . . . C1 C 0.34085(9) 0.29499(9) 0.06372(6) 0.0246(4) Uani 1 1 d . . . C2 C 0.25793(9) 0.31289(10) 0.11333(7) 0.0298(4) Uani 1 1 d . . . H2A H 0.2350 0.3243 0.1404 0.036 Uiso 1 1 calc R . . C3 C 0.22822(10) 0.28969(10) 0.07584(7) 0.0331(4) Uani 1 1 d . . . H3A H 0.1804 0.2818 0.0716 0.040 Uiso 1 1 calc R . . C4 C 0.26644(10) 0.25301(10) -0.00229(6) 0.0325(4) Uani 1 1 d . . . C5 C 0.18917(11) 0.24732(12) -0.00940(8) 0.0440(6) Uani 1 1 d . . . H5A H 0.1683 0.2931 -0.0071 0.066 Uiso 1 1 calc R . . H5B H 0.1694 0.2171 0.0134 0.066 Uiso 1 1 calc R . . H5C H 0.1800 0.2282 -0.0391 0.066 Uiso 1 1 calc R . . C6 C 0.29915(12) 0.18203(10) -0.00661(7) 0.0391(5) Uani 1 1 d . . . H6A H 0.3490 0.1858 -0.0022 0.059 Uiso 1 1 calc R . . H6B H 0.2897 0.1634 -0.0364 0.059 Uiso 1 1 calc R . . H6C H 0.2798 0.1513 0.0161 0.059 Uiso 1 1 calc R . . C7 C 0.29542(12) 0.30397(11) -0.03615(7) 0.0423(5) Uani 1 1 d . . . H7A H 0.3453 0.3079 -0.0321 0.063 Uiso 1 1 calc R . . H7B H 0.2740 0.3491 -0.0317 0.063 Uiso 1 1 calc R . . H7C H 0.2856 0.2877 -0.0665 0.063 Uiso 1 1 calc R . . C8 C 0.50830(9) 0.09303(9) 0.11402(6) 0.0220(4) Uani 1 1 d . . . C9 C 0.60771(9) 0.04099(9) 0.10126(6) 0.0261(4) Uani 1 1 d . . . H9A H 0.6556 0.0315 0.1006 0.031 Uiso 1 1 calc R . . C10 C 0.55810(10) 0.00192(10) 0.08321(6) 0.0289(4) Uani 1 1 d . . . H10A H 0.5645 -0.0403 0.0678 0.035 Uiso 1 1 calc R . . C11 C 0.42677(10) 0.00766(10) 0.07528(6) 0.0302(4) Uani 1 1 d . . . C12 C 0.39210(11) 0.06137(11) 0.04583(7) 0.0388(5) Uani 1 1 d . . . H12A H 0.3843 0.1034 0.0632 0.058 Uiso 1 1 calc R . . H12B H 0.3479 0.0435 0.0351 0.058 Uiso 1 1 calc R . . H12C H 0.4217 0.0718 0.0202 0.058 Uiso 1 1 calc R . . C13 C 0.38367(11) -0.00984(12) 0.11628(7) 0.0398(5) Uani 1 1 d . . . H13A H 0.4077 -0.0444 0.1343 0.060 Uiso 1 1 calc R . . H13B H 0.3390 -0.0281 0.1067 0.060 Uiso 1 1 calc R . . H13C H 0.3766 0.0318 0.1342 0.060 Uiso 1 1 calc R . . C14 C 0.43790(12) -0.05690(11) 0.04755(8) 0.0443(5) Uani 1 1 d . . . H14A H 0.4601 -0.0922 0.0660 0.066 Uiso 1 1 calc R . . H14B H 0.4673 -0.0461 0.0219 0.066 Uiso 1 1 calc R . . H14C H 0.3934 -0.0741 0.0369 0.066 Uiso 1 1 calc R . . C15 C 0.68905(9) 0.11103(9) 0.20684(6) 0.0236(4) Uani 1 1 d . . . C16 C 0.61999(10) 0.20081(9) 0.22000(6) 0.0277(4) Uani 1 1 d . . . H16A H 0.5877 0.2368 0.2156 0.033 Uiso 1 1 calc R . . C17 C 0.65105(10) 0.18563(10) 0.25845(7) 0.0335(4) Uani 1 1 d . . . H17A H 0.6450 0.2091 0.2860 0.040 Uiso 1 1 calc R . . C18 C 0.74274(10) 0.09999(10) 0.28536(6) 0.0335(4) Uani 1 1 d . . . C19 C 0.73100(15) 0.13589(14) 0.32981(8) 0.0592(7) Uani 1 1 d . . . H19A H 0.7400 0.1852 0.3265 0.089 Uiso 1 1 calc R . . H19B H 0.7621 0.1166 0.3523 0.089 Uiso 1 1 calc R . . H19C H 0.6833 0.1290 0.3393 0.089 Uiso 1 1 calc R . . C20 C 0.72895(11) 0.02364(11) 0.29119(7) 0.0406(5) Uani 1 1 d . . . H20A H 0.7363 0.0000 0.2627 0.061 Uiso 1 1 calc R . . H20B H 0.6813 0.0168 0.3009 0.061 Uiso 1 1 calc R . . H20C H 0.7603 0.0049 0.3137 0.061 Uiso 1 1 calc R . . C21 C 0.81607(11) 0.11374(11) 0.26949(8) 0.0440(5) Uani 1 1 d . . . H21A H 0.8230 0.1634 0.2661 0.066 Uiso 1 1 calc R . . H21B H 0.8236 0.0910 0.2407 0.066 Uiso 1 1 calc R . . H21C H 0.8487 0.0957 0.2915 0.066 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 Co1 0.02321(18) 0.02287(18) 0.01780(17) 0.000 0.000 0.00101(13) S1 0.0264(2) 0.0362(3) 0.0182(2) 0.00004(18) -0.00119(17) 0.00483(19) S2 0.0211(2) 0.0247(2) 0.0276(2) 0.00155(17) 0.00352(17) 0.00240(17) S3 0.0363(3) 0.0288(3) 0.0302(3) -0.00320(19) -0.0039(2) 0.0112(2) N1 0.0224(8) 0.0263(8) 0.0233(8) -0.0030(6) -0.0023(6) -0.0004(6) N2 0.0260(8) 0.0294(8) 0.0270(8) -0.0029(6) -0.0074(6) 0.0025(6) N3 0.0201(7) 0.0224(7) 0.0206(7) 0.0005(6) 0.0007(6) 0.0026(6) N4 0.0252(8) 0.0253(8) 0.0228(8) -0.0008(6) -0.0020(6) -0.0012(6) N5 0.0233(7) 0.0212(7) 0.0217(7) 0.0002(6) -0.0012(6) 0.0014(6) N6 0.0316(8) 0.0274(8) 0.0232(8) -0.0004(6) -0.0055(6) 0.0026(7) B1 0.0211(10) 0.0224(10) 0.0217(9) 0.0011(8) 0.0007(8) 0.0015(8) C1 0.0265(9) 0.0245(9) 0.0228(9) 0.0015(7) -0.0047(7) 0.0031(7) C2 0.0216(9) 0.0334(10) 0.0345(11) -0.0054(8) 0.0025(8) -0.0022(8) C3 0.0217(9) 0.0357(11) 0.0420(12) -0.0049(9) -0.0041(8) 0.0000(8) C4 0.0389(11) 0.0317(10) 0.0270(10) -0.0041(8) -0.0140(8) 0.0039(9) C5 0.0437(13) 0.0446(13) 0.0436(13) -0.0066(10) -0.0219(10) 0.0035(10) C6 0.0493(13) 0.0331(11) 0.0350(11) -0.0083(9) -0.0140(9) 0.0055(10) C7 0.0530(14) 0.0427(12) 0.0312(11) 0.0033(9) -0.0138(10) 0.0039(10) C8 0.0231(9) 0.0238(9) 0.0192(8) 0.0023(7) 0.0009(7) 0.0012(7) C9 0.0248(9) 0.0281(9) 0.0253(9) -0.0024(7) 0.0016(7) 0.0057(7) C10 0.0322(10) 0.0273(10) 0.0272(10) -0.0060(8) 0.0005(8) 0.0035(8) C11 0.0294(10) 0.0296(10) 0.0316(10) -0.0009(8) -0.0081(8) -0.0057(8) C12 0.0399(12) 0.0419(12) 0.0345(11) 0.0029(9) -0.0163(9) -0.0015(9) C13 0.0334(11) 0.0452(13) 0.0407(12) 0.0038(10) -0.0027(9) -0.0119(10) C14 0.0476(13) 0.0378(12) 0.0474(14) -0.0102(10) -0.0115(11) -0.0056(10) C15 0.0249(9) 0.0218(9) 0.0239(9) 0.0013(7) -0.0010(7) -0.0007(7) C16 0.0326(10) 0.0233(9) 0.0272(10) -0.0033(7) 0.0001(8) 0.0041(7) C17 0.0410(12) 0.0325(11) 0.0270(10) -0.0081(8) -0.0046(8) 0.0064(9) C18 0.0367(11) 0.0384(11) 0.0253(10) 0.0006(8) -0.0105(8) 0.0047(9) C19 0.0781(19) 0.0689(17) 0.0305(12) -0.0122(11) -0.0233(12) 0.0246(14) C20 0.0417(12) 0.0424(12) 0.0377(12) 0.0148(10) -0.0074(10) -0.0038(9) C21 0.0389(12) 0.0422(12) 0.0509(14) 0.0068(10) -0.0188(10) -0.0067(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 S2 2.3607(5) 6_554 ? Co1 S2 2.3607(5) . ? Co1 S1 2.3804(5) . ? Co1 S1 2.3804(5) 6_554 ? S1 C1 1.7230(19) . ? S2 C8 1.7304(17) . ? S3 C15 1.6889(18) . ? N1 C1 1.352(2) . ? N1 C2 1.378(2) . ? N1 B1 1.554(2) 6_554 ? N2 C1 1.368(2) . ? N2 C3 1.380(2) . ? N2 C4 1.507(2) . ? N3 C8 1.355(2) . ? N3 C9 1.382(2) . ? N3 B1 1.553(2) . ? N4 C8 1.355(2) . ? N4 C10 1.386(2) . ? N4 C11 1.513(2) . ? N5 C15 1.378(2) . ? N5 C16 1.385(2) . ? N5 B1 1.545(2) . ? N6 C15 1.376(2) . ? N6 C17 1.389(2) . ? N6 C18 1.511(2) . ? B1 H1 1.084(17) . ? B1 N1 1.554(2) 6_554 ? C2 C3 1.340(3) . ? C4 C5 1.522(3) . ? C4 C7 1.525(3) . ? C4 C6 1.525(3) . ? C9 C10 1.341(3) . ? C11 C14 1.520(3) . ? C11 C12 1.524(3) . ? C11 C13 1.524(3) . ? C16 C17 1.332(3) . ? C18 C20 1.519(3) . ? C18 C19 1.519(3) . ? C18 C21 1.526(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Co1 S2 127.86(3) 6_554 . ? S2 Co1 S1 109.385(16) 6_554 . ? S2 Co1 S1 106.544(16) . . ? S2 Co1 S1 106.544(16) 6_554 6_554 ? S2 Co1 S1 109.385(16) . 6_554 ? S1 Co1 S1 90.88(3) . 6_554 ? C1 S1 Co1 108.85(6) . . ? C8 S2 Co1 97.44(6) . . ? C1 N1 C2 108.73(15) . . ? C1 N1 B1 123.16(15) . 6_554 ? C2 N1 B1 127.94(15) . 6_554 ? C1 N2 C3 107.90(15) . . ? C1 N2 C4 127.65(16) . . ? C3 N2 C4 124.44(16) . . ? C8 N3 C9 107.99(14) . . ? C8 N3 B1 125.03(14) . . ? C9 N3 B1 125.94(14) . . ? C8 N4 C10 108.15(14) . . ? C8 N4 C11 127.34(15) . . ? C10 N4 C11 124.50(15) . . ? C15 N5 C16 108.14(15) . . ? C15 N5 B1 132.22(15) . . ? C16 N5 B1 119.64(14) . . ? C15 N6 C17 108.46(15) . . ? C15 N6 C18 126.59(15) . . ? C17 N6 C18 124.62(15) . . ? H1 B1 N5 105.7(10) . . ? H1 B1 N3 108.4(9) . . ? N5 B1 N3 115.36(14) . . ? H1 B1 N1 106.0(9) . 6_554 ? N5 B1 N1 112.04(14) . 6_554 ? N3 B1 N1 108.83(14) . 6_554 ? N1 C1 N2 107.34(15) . . ? N1 C1 S1 124.97(13) . . ? N2 C1 S1 127.69(14) . . ? C3 C2 N1 107.80(17) . . ? C2 C3 N2 108.18(16) . . ? N2 C4 C5 108.37(17) . . ? N2 C4 C7 109.67(16) . . ? C5 C4 C7 108.61(17) . . ? N2 C4 C6 108.42(15) . . ? C5 C4 C6 109.52(17) . . ? C7 C4 C6 112.18(18) . . ? N4 C8 N3 108.04(14) . . ? N4 C8 S2 127.03(13) . . ? N3 C8 S2 124.91(13) . . ? C10 C9 N3 108.17(16) . . ? C9 C10 N4 107.65(16) . . ? N4 C11 C14 109.08(16) . . ? N4 C11 C12 109.73(15) . . ? C14 C11 C12 108.24(17) . . ? N4 C11 C13 108.25(15) . . ? C14 C11 C13 109.46(17) . . ? C12 C11 C13 112.04(17) . . ? N6 C15 N5 106.59(14) . . ? N6 C15 S3 127.81(13) . . ? N5 C15 S3 125.59(13) . . ? C17 C16 N5 108.80(16) . . ? C16 C17 N6 108.01(17) . . ? N6 C18 C20 109.77(16) . . ? N6 C18 C19 108.93(16) . . ? C20 C18 C19 108.78(19) . . ? N6 C18 C21 108.09(16) . . ? C20 C18 C21 111.84(17) . . ? C19 C18 C21 109.40(19) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.378 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.060 data_j10 _database_code_depnum_ccdc_archive 'CCDC 229399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H68 B2 Br Co2 F6 N12 P S6' _chemical_formula_weight 1297.80 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 34.694(2) _cell_length_b 40.456(2) _cell_length_c 19.3445(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27152(3) _cell_formula_units_Z 16 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10688 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5660 _exptl_absorpt_correction_T_max 0.7395 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46620 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.32 _reflns_number_total 15065 _reflns_number_gt 9575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0850P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(9) _refine_ls_number_reflns 15065 _refine_ls_number_parameters 676 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.003 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 -0.25654(2) 0.142084(16) 0.19614(4) 0.03908(17) Uani 1 1 d . . . Co2 Co -0.27379(2) 0.055669(16) 0.12853(4) 0.04154(18) Uani 1 1 d . . . Br Br -0.29347(2) 0.025780(16) 0.02923(3) 0.06502(19) Uani 1 1 d . . . B1 B -0.20590(17) 0.11820(14) 0.0738(3) 0.0362(12) Uani 1 1 d . . . H1 H -0.2167(14) 0.1133(11) 0.126(3) 0.034(12) Uiso 1 1 d . . . B2 B -0.28078(19) 0.09869(15) 0.3097(3) 0.0429(14) Uani 1 1 d . . . H2 H -0.2720(13) 0.1042(11) 0.258(3) 0.028(12) Uiso 1 1 d . . . S11 S -0.21032(4) 0.04913(3) 0.16241(8) 0.0471(3) Uani 1 1 d . . . S12 S -0.29568(4) 0.11001(3) 0.11558(7) 0.0414(3) Uani 1 1 d . . . S13 S -0.23504(4) 0.18756(3) 0.12839(9) 0.0521(4) Uani 1 1 d . . . S21 S -0.31316(4) 0.03734(4) 0.21812(7) 0.0475(3) Uani 1 1 d . . . S22 S -0.30720(4) 0.16914(3) 0.25367(8) 0.0492(3) Uani 1 1 d . . . S23 S -0.20402(4) 0.14061(4) 0.27112(8) 0.0591(4) Uani 1 1 d . . . N11 N -0.18557(12) 0.08600(10) 0.0524(2) 0.0407(10) Uani 1 1 d . . . N12 N -0.16516(15) 0.03505(11) 0.0494(3) 0.0536(12) Uani 1 1 d . . . N13 N -0.17805(12) 0.14861(10) 0.0724(2) 0.0390(10) Uani 1 1 d . . . N14 N -0.15974(13) 0.19982(10) 0.0895(2) 0.0443(10) Uani 1 1 d . . . N15 N -0.23908(12) 0.12578(10) 0.0231(2) 0.0429(10) Uani 1 1 d . . . N16 N -0.29666(13) 0.13662(11) -0.0166(3) 0.0486(12) Uani 1 1 d . . . N21 N -0.27512(13) 0.06207(11) 0.3298(2) 0.0452(11) Uani 1 1 d . . . N22 N -0.27162(15) 0.00781(11) 0.3234(2) 0.0507(12) Uani 1 1 d . . . N23 N -0.32335(13) 0.10906(10) 0.3125(2) 0.0445(10) Uani 1 1 d . . . N24 N -0.37253(13) 0.14299(11) 0.3139(2) 0.0470(11) Uani 1 1 d . . . N25 N -0.25890(14) 0.12100(11) 0.3616(2) 0.0457(11) Uani 1 1 d . . . N26 N -0.22065(15) 0.15756(12) 0.4059(2) 0.0529(12) Uani 1 1 d . . . C11 C -0.18616(15) 0.05673(12) 0.0866(3) 0.0405(12) Uani 1 1 d . . . C12 C -0.16461(18) 0.08199(15) -0.0072(3) 0.0517(14) Uani 1 1 d . . . H12A H -0.1600 0.0984 -0.0406 0.062 Uiso 1 1 calc R . . C13 C -0.1518(2) 0.05102(16) -0.0097(3) 0.0613(17) Uani 1 1 d . . . H13A H -0.1366 0.0417 -0.0448 0.074 Uiso 1 1 calc R . . C14 C -0.1564(2) -0.00130(15) 0.0659(4) 0.0662(18) Uani 1 1 d . . . C15 C -0.1318(4) -0.0148(2) 0.0062(6) 0.126(4) Uani 1 1 d . . . H15A H -0.1263 -0.0380 0.0142 0.190 Uiso 1 1 calc R . . H15B H -0.1078 -0.0026 0.0036 0.190 Uiso 1 1 calc R . . H15C H -0.1458 -0.0124 -0.0370 0.190 Uiso 1 1 calc R . . C16 C -0.1357(3) -0.00306(19) 0.1330(5) 0.094(3) Uani 1 1 d . . . H16A H -0.1514 0.0069 0.1689 0.142 Uiso 1 1 calc R . . H16B H -0.1114 0.0088 0.1294 0.142 Uiso 1 1 calc R . . H16C H -0.1307 -0.0260 0.1445 0.142 Uiso 1 1 calc R . . C17 C -0.1940(3) -0.01952(16) 0.0662(5) 0.090(3) Uani 1 1 d . . . H17A H -0.2103 -0.0109 0.1027 0.134 Uiso 1 1 calc R . . H17B H -0.1893 -0.0428 0.0742 0.134 Uiso 1 1 calc R . . H17C H -0.2067 -0.0166 0.0220 0.134 Uiso 1 1 calc R . . C18 C -0.27685(15) 0.12414(12) 0.0380(3) 0.0409(12) Uani 1 1 d . . . C19 C -0.23453(18) 0.13954(15) -0.0422(3) 0.0537(15) Uani 1 1 d . . . H19A H -0.2111 0.1433 -0.0653 0.064 Uiso 1 1 calc R . . C21 C -0.28568(15) 0.03508(13) 0.2916(3) 0.0430(12) Uani 1 1 d . . . C22 C -0.2542(2) 0.05041(15) 0.3856(3) 0.0576(16) Uani 1 1 d . . . H22A H -0.2433 0.0636 0.4206 0.069 Uiso 1 1 calc R . . C23 C -0.2518(2) 0.01807(14) 0.3820(3) 0.0603(17) Uani 1 1 d . . . H23A H -0.2389 0.0043 0.4135 0.072 Uiso 1 1 calc R . . C24 C -0.2764(2) -0.02745(14) 0.3008(3) 0.0641(18) Uani 1 1 d . . . C25 C -0.2557(3) -0.03217(15) 0.2325(4) 0.080(2) Uani 1 1 d . . . H25A H -0.2692 -0.0201 0.1966 0.119 Uiso 1 1 calc R . . H25B H -0.2552 -0.0555 0.2209 0.119 Uiso 1 1 calc R . . H25C H -0.2295 -0.0240 0.2364 0.119 Uiso 1 1 calc R . . C26 C -0.2571(3) -0.04939(16) 0.3557(4) 0.086(2) Uani 1 1 d . . . H26A H -0.2657 -0.0427 0.4013 0.129 Uiso 1 1 calc R . . H26B H -0.2293 -0.0470 0.3528 0.129 Uiso 1 1 calc R . . H26C H -0.2640 -0.0723 0.3478 0.129 Uiso 1 1 calc R . . C27 C -0.3189(2) -0.0357(2) 0.2978(5) 0.094(3) Uani 1 1 d . . . H27A H -0.3308 -0.0236 0.2601 0.141 Uiso 1 1 calc R . . H27B H -0.3311 -0.0294 0.3411 0.141 Uiso 1 1 calc R . . H27C H -0.3221 -0.0592 0.2904 0.141 Uiso 1 1 calc R . . C28 C -0.33562(16) 0.13977(12) 0.2935(3) 0.0427(12) Uani 1 1 d . . . C29 C -0.35298(17) 0.09305(16) 0.3455(3) 0.0555(15) Uani 1 1 d . . . H29A H -0.3524 0.0716 0.3639 0.067 Uiso 1 1 calc R . . C110 C -0.26975(19) 0.14637(15) -0.0661(3) 0.0613(18) Uani 1 1 d . . . H11A H -0.2754 0.1561 -0.1091 0.074 Uiso 1 1 calc R . . C111 C -0.34002(17) 0.13808(13) -0.0256(3) 0.0545(15) Uani 1 1 d . . . C112 C -0.35365(18) 0.10251(15) -0.0309(4) 0.0583(16) Uani 1 1 d . . . H11B H -0.3464 0.0906 0.0107 0.087 Uiso 1 1 calc R . . H11C H -0.3418 0.0921 -0.0707 0.087 Uiso 1 1 calc R . . H11D H -0.3815 0.1021 -0.0359 0.087 Uiso 1 1 calc R . . C113 C -0.35790(19) 0.15688(16) 0.0340(4) 0.076(2) Uani 1 1 d . . . H11E H -0.3508 0.1800 0.0309 0.114 Uiso 1 1 calc R . . H11F H -0.3487 0.1478 0.0774 0.114 Uiso 1 1 calc R . . H11G H -0.3857 0.1548 0.0319 0.114 Uiso 1 1 calc R . . C114 C -0.3485(2) 0.15550(19) -0.0932(4) 0.083(2) Uani 1 1 d . . . H11H H -0.3418 0.1787 -0.0891 0.125 Uiso 1 1 calc R . . H11I H -0.3757 0.1534 -0.1040 0.125 Uiso 1 1 calc R . . H11J H -0.3333 0.1456 -0.1299 0.125 Uiso 1 1 calc R . . C115 C -0.18982(15) 0.17856(12) 0.0980(3) 0.0391(12) Uani 1 1 d . . . C116 C -0.14136(15) 0.15219(13) 0.0462(3) 0.0434(12) Uani 1 1 d . . . H11K H -0.1267 0.1355 0.0249 0.052 Uiso 1 1 calc R . . C117 C -0.13013(16) 0.18325(14) 0.0561(3) 0.0476(13) Uani 1 1 d . . . H11L H -0.1063 0.1924 0.0428 0.057 Uiso 1 1 calc R . . C118 C -0.15801(19) 0.23573(13) 0.1129(4) 0.0648(19) Uani 1 1 d . . . C119 C -0.1173(2) 0.24912(16) 0.0972(4) 0.073(2) Uani 1 1 d . . . H11M H -0.1112 0.2454 0.0489 0.110 Uiso 1 1 calc R . . H11N H -0.0986 0.2377 0.1259 0.110 Uiso 1 1 calc R . . H11O H -0.1164 0.2726 0.1071 0.110 Uiso 1 1 calc R . . C120 C -0.1874(2) 0.25487(16) 0.0718(6) 0.100(3) Uani 1 1 d . . . H12B H -0.2120 0.2434 0.0734 0.150 Uiso 1 1 calc R . . H12C H -0.1789 0.2567 0.0242 0.150 Uiso 1 1 calc R . . H12D H -0.1904 0.2768 0.0915 0.150 Uiso 1 1 calc R . . C121 C -0.1656(3) 0.2371(2) 0.1890(5) 0.106(3) Uani 1 1 d . . . H12E H -0.1915 0.2293 0.1984 0.160 Uiso 1 1 calc R . . H12F H -0.1630 0.2598 0.2050 0.160 Uiso 1 1 calc R . . H12G H -0.1471 0.2232 0.2130 0.160 Uiso 1 1 calc R . . C210 C -0.38349(18) 0.11432(15) 0.3464(3) 0.0565(16) Uani 1 1 d . . . H21A H -0.4078 0.1101 0.3658 0.068 Uiso 1 1 calc R . . C211 C -0.39828(18) 0.17337(16) 0.3068(4) 0.0630(17) Uani 1 1 d . . . C212 C -0.4370(2) 0.1649(2) 0.3390(6) 0.102(3) Uani 1 1 d . . . H21B H -0.4331 0.1570 0.3858 0.153 Uiso 1 1 calc R . . H21C H -0.4495 0.1478 0.3119 0.153 Uiso 1 1 calc R . . H21D H -0.4531 0.1845 0.3398 0.153 Uiso 1 1 calc R . . C213 C -0.3802(2) 0.20160(18) 0.3484(4) 0.080(2) Uani 1 1 d . . . H21E H -0.3773 0.1948 0.3962 0.121 Uiso 1 1 calc R . . H21F H -0.3967 0.2209 0.3460 0.121 Uiso 1 1 calc R . . H21G H -0.3551 0.2069 0.3292 0.121 Uiso 1 1 calc R . . C214 C -0.4037(2) 0.18072(19) 0.2286(4) 0.078(2) Uani 1 1 d . . . H21H H -0.4187 0.2007 0.2230 0.117 Uiso 1 1 calc R . . H21I H -0.4170 0.1624 0.2068 0.117 Uiso 1 1 calc R . . H21J H -0.3786 0.1836 0.2071 0.117 Uiso 1 1 calc R . . C215 C -0.22788(16) 0.13976(13) 0.3483(3) 0.0446(13) Uani 1 1 d . . . C216 C -0.27152(19) 0.12723(16) 0.4282(3) 0.0555(15) Uani 1 1 d . . . H21K H -0.2926 0.1173 0.4506 0.067 Uiso 1 1 calc R . . C217 C -0.2476(2) 0.15045(16) 0.4550(4) 0.0659(18) Uani 1 1 d . . . H21L H -0.2494 0.1599 0.4993 0.079 Uiso 1 1 calc R . . C218 C -0.1905(2) 0.1841(2) 0.4146(4) 0.080(2) Uani 1 1 d . . . C219 C -0.1515(3) 0.1681(3) 0.4042(5) 0.124(4) Uani 1 1 d . . . H21M H -0.1516 0.1462 0.4247 0.186 Uiso 1 1 calc R . . H21N H -0.1318 0.1815 0.4262 0.186 Uiso 1 1 calc R . . H21O H -0.1461 0.1664 0.3552 0.186 Uiso 1 1 calc R . . C220 C -0.1923(3) 0.1975(3) 0.4883(5) 0.110(3) Uani 1 1 d . . . H22B H -0.1926 0.1792 0.5208 0.166 Uiso 1 1 calc R . . H22C H -0.2156 0.2106 0.4940 0.166 Uiso 1 1 calc R . . H22D H -0.1699 0.2112 0.4971 0.166 Uiso 1 1 calc R . . C221 C -0.2024(4) 0.2128(2) 0.3636(5) 0.133(5) Uani 1 1 d . . . H22E H -0.2029 0.2045 0.3166 0.200 Uiso 1 1 calc R . . H22F H -0.1839 0.2307 0.3669 0.200 Uiso 1 1 calc R . . H22G H -0.2278 0.2209 0.3759 0.200 Uiso 1 1 calc R . . P P -0.1337(3) 0.13234(12) -0.1886(3) 0.333(6) Uani 1 1 d . . . F1 F -0.1624(8) 0.1181(3) -0.1595(6) 0.509(19) Uani 1 1 d . . . F2 F -0.1388(6) 0.1591(3) -0.1319(6) 0.372(12) Uani 1 1 d . . . F3 F -0.1537(6) 0.1578(3) -0.2458(7) 0.347(12) Uani 1 1 d . . . F4 F -0.0962(5) 0.1476(3) -0.2118(7) 0.303(9) Uani 1 1 d . . . F5 F -0.1319(5) 0.1075(2) -0.2484(4) 0.278(8) Uani 1 1 d . . . F6 F -0.1150(7) 0.0978(6) -0.161(3) 0.71(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0373(4) 0.0406(3) 0.0393(4) -0.0036(3) 0.0032(3) -0.0007(3) Co2 0.0479(4) 0.0408(3) 0.0359(4) 0.0005(3) 0.0006(3) -0.0041(3) Br 0.0813(5) 0.0665(4) 0.0472(3) -0.0177(3) -0.0013(3) 0.0014(3) B1 0.036(3) 0.041(3) 0.031(3) 0.001(2) -0.003(3) 0.000(2) B2 0.049(4) 0.044(3) 0.036(3) 0.001(3) -0.002(3) 0.003(3) S11 0.0526(8) 0.0461(7) 0.0425(8) 0.0066(6) -0.0025(7) 0.0011(6) S12 0.0386(7) 0.0446(6) 0.0411(7) -0.0007(6) -0.0010(6) -0.0036(5) S13 0.0440(8) 0.0379(6) 0.0743(10) 0.0042(7) 0.0148(8) 0.0028(6) S21 0.0470(8) 0.0600(8) 0.0355(7) 0.0081(6) -0.0072(6) -0.0102(6) S22 0.0477(8) 0.0417(7) 0.0582(9) 0.0012(6) 0.0154(7) 0.0041(6) S23 0.0394(8) 0.0905(11) 0.0473(9) -0.0140(8) 0.0006(7) -0.0054(8) N11 0.042(2) 0.045(2) 0.035(2) -0.0066(19) -0.002(2) 0.0000(19) N12 0.058(3) 0.049(2) 0.054(3) -0.004(2) -0.001(3) 0.009(2) N13 0.034(2) 0.043(2) 0.040(2) -0.0007(19) 0.0035(19) 0.0027(18) N14 0.045(3) 0.040(2) 0.048(3) 0.004(2) 0.008(2) -0.002(2) N15 0.041(3) 0.050(2) 0.037(3) 0.010(2) -0.004(2) -0.003(2) N16 0.042(3) 0.049(2) 0.055(3) 0.010(2) -0.014(2) -0.004(2) N21 0.049(3) 0.050(2) 0.036(3) 0.000(2) -0.008(2) 0.002(2) N22 0.060(3) 0.046(2) 0.046(3) 0.008(2) -0.006(2) -0.003(2) N23 0.048(3) 0.047(2) 0.039(2) 0.004(2) 0.004(2) 0.000(2) N24 0.045(3) 0.056(3) 0.040(3) -0.001(2) 0.008(2) 0.006(2) N25 0.055(3) 0.048(2) 0.034(3) -0.004(2) 0.001(2) 0.008(2) N26 0.058(3) 0.060(3) 0.040(3) -0.010(2) -0.007(2) -0.004(2) C11 0.040(3) 0.041(3) 0.040(3) 0.000(2) -0.007(2) 0.003(2) C12 0.061(4) 0.058(3) 0.036(3) -0.002(3) 0.003(3) 0.001(3) C13 0.071(4) 0.062(4) 0.051(4) -0.015(3) 0.009(3) 0.014(3) C14 0.074(5) 0.054(3) 0.071(5) -0.001(3) 0.004(4) 0.022(3) C15 0.181(11) 0.066(5) 0.132(9) -0.007(5) 0.043(8) 0.061(6) C16 0.094(6) 0.069(4) 0.120(7) 0.002(5) -0.031(6) 0.026(4) C17 0.126(7) 0.042(3) 0.100(6) -0.001(4) -0.012(6) 0.013(4) C18 0.042(3) 0.039(2) 0.042(3) 0.004(2) -0.011(3) -0.004(2) C19 0.053(4) 0.066(4) 0.042(3) 0.009(3) -0.002(3) -0.009(3) C21 0.044(3) 0.048(3) 0.037(3) 0.006(2) -0.005(2) -0.003(2) C22 0.075(4) 0.054(3) 0.043(3) 0.003(3) -0.020(3) 0.007(3) C23 0.081(5) 0.051(3) 0.049(4) 0.003(3) -0.025(3) 0.004(3) C24 0.092(5) 0.044(3) 0.056(4) 0.009(3) -0.017(4) -0.007(3) C25 0.130(7) 0.041(3) 0.068(5) -0.010(3) 0.005(5) 0.006(4) C26 0.131(7) 0.049(3) 0.078(5) 0.010(3) -0.019(5) -0.008(4) C27 0.104(6) 0.080(5) 0.098(6) 0.031(5) -0.022(5) -0.043(5) C28 0.045(3) 0.046(3) 0.037(3) -0.001(2) 0.003(2) 0.005(2) C29 0.051(4) 0.065(4) 0.050(4) 0.015(3) 0.010(3) -0.004(3) C110 0.064(4) 0.068(4) 0.051(4) 0.025(3) -0.022(3) -0.011(3) C111 0.046(3) 0.049(3) 0.069(4) 0.008(3) -0.025(3) -0.006(3) C112 0.048(3) 0.061(3) 0.066(4) -0.006(3) -0.009(3) -0.011(3) C113 0.057(4) 0.057(3) 0.115(6) -0.028(4) -0.023(4) 0.014(3) C114 0.067(5) 0.076(4) 0.107(6) 0.023(4) -0.050(4) -0.003(4) C115 0.042(3) 0.035(2) 0.041(3) 0.000(2) 0.006(2) 0.000(2) C116 0.038(3) 0.048(3) 0.045(3) 0.001(2) 0.005(2) 0.000(2) C117 0.038(3) 0.059(3) 0.046(3) 0.002(3) 0.004(3) -0.002(3) C118 0.063(4) 0.035(3) 0.096(6) -0.006(3) 0.018(4) -0.009(3) C119 0.069(4) 0.052(3) 0.099(6) 0.002(4) 0.015(4) -0.018(3) C120 0.072(5) 0.051(4) 0.176(10) 0.035(5) 0.025(6) 0.001(3) C121 0.153(8) 0.071(5) 0.095(6) -0.042(5) 0.052(6) -0.044(5) C210 0.045(3) 0.068(4) 0.056(4) 0.016(3) 0.022(3) -0.001(3) C211 0.047(4) 0.068(4) 0.074(5) 0.000(3) 0.015(3) 0.016(3) C212 0.053(4) 0.098(6) 0.156(9) 0.011(6) 0.041(5) 0.015(4) C213 0.077(5) 0.077(5) 0.087(6) -0.017(4) 0.015(4) 0.021(4) C214 0.064(4) 0.088(5) 0.081(5) 0.024(4) 0.003(4) 0.029(4) C215 0.041(3) 0.055(3) 0.038(3) -0.008(2) -0.006(3) 0.003(3) C216 0.067(4) 0.065(4) 0.035(3) -0.003(3) 0.008(3) 0.000(3) C217 0.085(5) 0.068(4) 0.045(4) -0.020(3) -0.002(4) 0.004(4) C218 0.082(5) 0.089(5) 0.069(5) -0.028(4) -0.009(4) -0.019(4) C219 0.066(5) 0.209(11) 0.098(7) -0.064(8) -0.003(5) -0.037(7) C220 0.123(8) 0.120(7) 0.087(6) -0.042(6) -0.015(6) -0.042(6) C221 0.210(13) 0.100(7) 0.090(7) -0.005(6) 0.008(8) -0.073(8) P 0.705(16) 0.134(3) 0.159(4) -0.069(3) 0.249(7) -0.218(6) F1 1.11(5) 0.206(10) 0.213(11) -0.070(8) 0.39(2) -0.31(2) F2 0.68(3) 0.274(13) 0.165(8) -0.126(9) 0.171(14) -0.187(18) F3 0.60(3) 0.219(12) 0.217(12) -0.056(10) 0.191(18) -0.191(17) F4 0.413(19) 0.229(11) 0.268(14) -0.058(10) 0.202(15) -0.189(13) F5 0.59(2) 0.124(6) 0.118(6) -0.023(5) 0.116(10) -0.117(10) F6 0.41(3) 0.35(3) 1.38(10) 0.37(4) 0.51(5) 0.16(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 Co1 H2 2.02(5) . ? Co1 H1 2.26(5) . ? Co1 S23 2.3296(17) . ? Co1 S22 2.3505(15) . ? Co1 S13 2.3789(16) . ? Co1 S12 2.4405(15) . ? Co2 S11 2.3127(17) . ? Co2 S21 2.3278(16) . ? Co2 S12 2.3393(15) . ? Co2 Br 2.3701(9) . ? B1 N11 1.538(7) . ? B1 N15 1.542(7) . ? B1 N13 1.565(7) . ? B2 N23 1.536(8) . ? B2 N21 1.544(7) . ? B2 N25 1.550(8) . ? S11 C11 1.716(6) . ? S12 C18 1.734(6) . ? S13 C115 1.715(5) . ? S21 C21 1.713(5) . ? S22 C28 1.726(5) . ? S23 C215 1.707(6) . ? N11 C11 1.357(6) . ? N11 C12 1.373(7) . ? N12 C11 1.349(7) . ? N12 C13 1.392(8) . ? N12 C14 1.535(8) . ? N13 C115 1.371(6) . ? N13 C116 1.378(7) . ? N14 C115 1.362(7) . ? N14 C117 1.386(7) . ? N14 C118 1.523(7) . ? N15 C18 1.343(7) . ? N15 C19 1.391(7) . ? N16 C18 1.357(7) . ? N16 C110 1.395(8) . ? N16 C111 1.515(7) . ? N21 C21 1.369(7) . ? N21 C22 1.385(7) . ? N22 C21 1.354(7) . ? N22 C23 1.389(8) . ? N22 C24 1.501(7) . ? N23 C28 1.364(7) . ? N23 C29 1.372(7) . ? N24 C28 1.347(7) . ? N24 C210 1.372(7) . ? N24 C211 1.526(7) . ? N25 C215 1.342(7) . ? N25 C216 1.383(7) . ? N26 C215 1.351(7) . ? N26 C217 1.364(8) . ? N26 C218 1.508(9) . ? C12 C13 1.330(9) . ? C14 C16 1.486(11) . ? C14 C17 1.498(11) . ? C14 C15 1.537(11) . ? C19 C110 1.335(9) . ? C22 C23 1.313(8) . ? C24 C25 1.514(10) . ? C24 C27 1.515(11) . ? C24 C26 1.538(10) . ? C29 C210 1.364(9) . ? C111 C113 1.514(10) . ? C111 C114 1.515(9) . ? C111 C112 1.518(8) . ? C116 C117 1.330(8) . ? C118 C121 1.497(11) . ? C118 C120 1.508(11) . ? C118 C119 1.544(9) . ? C211 C212 1.519(10) . ? C211 C213 1.531(10) . ? C211 C214 1.553(10) . ? C216 C217 1.355(9) . ? C218 C219 1.513(12) . ? C218 C220 1.528(11) . ? C218 C221 1.581(14) . ? P F1 1.282(16) . ? P F4 1.507(13) . ? P F5 1.535(8) . ? P F2 1.551(10) . ? P F6 1.63(2) . ? P F3 1.66(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 H2 Co1 H1 97.4(18) . . ? H2 Co1 S23 79.6(13) . . ? H1 Co1 S23 83.3(13) . . ? H2 Co1 S22 82.7(13) . . ? H1 Co1 S22 168.9(12) . . ? S23 Co1 S22 107.57(6) . . ? H2 Co1 S13 176.3(13) . . ? H1 Co1 S13 82.8(12) . . ? S23 Co1 S13 96.75(6) . . ? S22 Co1 S13 97.77(5) . . ? H2 Co1 S12 80.0(13) . . ? H1 Co1 S12 71.4(12) . . ? S23 Co1 S12 145.00(6) . . ? S22 Co1 S12 97.69(6) . . ? S13 Co1 S12 103.53(6) . . ? S11 Co2 S21 108.14(6) . . ? S11 Co2 S12 116.54(5) . . ? S21 Co2 S12 100.87(6) . . ? S11 Co2 Br 116.46(5) . . ? S21 Co2 Br 105.77(5) . . ? S12 Co2 Br 107.41(5) . . ? N11 B1 N15 109.9(4) . . ? N11 B1 N13 112.2(4) . . ? N15 B1 N13 107.1(4) . . ? N23 B2 N21 112.0(5) . . ? N23 B2 N25 106.8(4) . . ? N21 B2 N25 109.5(4) . . ? C11 S11 Co2 101.70(18) . . ? C18 S12 Co2 106.28(17) . . ? C18 S12 Co1 99.67(17) . . ? Co2 S12 Co1 104.52(6) . . ? C115 S13 Co1 108.16(18) . . ? C21 S21 Co2 107.93(19) . . ? C28 S22 Co1 108.55(18) . . ? C215 S23 Co1 99.54(19) . . ? C11 N11 C12 108.3(4) . . ? C11 N11 B1 127.0(4) . . ? C12 N11 B1 124.6(5) . . ? C11 N12 C13 108.4(5) . . ? C11 N12 C14 128.2(5) . . ? C13 N12 C14 123.4(5) . . ? C115 N13 C116 108.4(4) . . ? C115 N13 B1 120.3(4) . . ? C116 N13 B1 131.3(4) . . ? C115 N14 C117 108.6(4) . . ? C115 N14 C118 126.6(4) . . ? C117 N14 C118 124.8(5) . . ? C18 N15 C19 109.0(4) . . ? C18 N15 B1 125.6(4) . . ? C19 N15 B1 124.9(5) . . ? C18 N16 C110 107.5(4) . . ? C18 N16 C111 127.3(5) . . ? C110 N16 C111 125.1(5) . . ? C21 N21 C22 106.9(4) . . ? C21 N21 B2 126.6(4) . . ? C22 N21 B2 126.1(5) . . ? C21 N22 C23 107.8(4) . . ? C21 N22 C24 127.0(5) . . ? C23 N22 C24 125.1(5) . . ? C28 N23 C29 108.8(5) . . ? C28 N23 B2 122.6(4) . . ? C29 N23 B2 127.4(5) . . ? C28 N24 C210 108.4(5) . . ? C28 N24 C211 127.5(5) . . ? C210 N24 C211 124.1(5) . . ? C215 N25 C216 109.3(5) . . ? C215 N25 B2 126.7(5) . . ? C216 N25 B2 123.7(5) . . ? C215 N26 C217 109.6(5) . . ? C215 N26 C218 126.8(5) . . ? C217 N26 C218 123.3(5) . . ? N12 C11 N11 107.4(5) . . ? N12 C11 S11 127.1(4) . . ? N11 C11 S11 125.5(4) . . ? C13 C12 N11 108.6(5) . . ? C12 C13 N12 107.3(5) . . ? C16 C14 C17 113.2(7) . . ? C16 C14 N12 108.9(6) . . ? C17 C14 N12 107.5(5) . . ? C16 C14 C15 111.7(7) . . ? C17 C14 C15 108.1(7) . . ? N12 C14 C15 107.1(6) . . ? N15 C18 N16 108.0(5) . . ? N15 C18 S12 124.7(4) . . ? N16 C18 S12 127.3(4) . . ? C110 C19 N15 107.1(5) . . ? N22 C21 N21 107.9(5) . . ? N22 C21 S21 128.4(4) . . ? N21 C21 S21 123.6(4) . . ? C23 C22 N21 109.3(6) . . ? C22 C23 N22 108.1(5) . . ? N22 C24 C25 108.8(5) . . ? N22 C24 C27 109.1(6) . . ? C25 C24 C27 113.6(6) . . ? N22 C24 C26 107.4(5) . . ? C25 C24 C26 108.9(6) . . ? C27 C24 C26 108.9(6) . . ? N24 C28 N23 107.8(5) . . ? N24 C28 S22 127.4(4) . . ? N23 C28 S22 124.7(4) . . ? C210 C29 N23 106.8(5) . . ? C19 C110 N16 108.4(5) . . ? C113 C111 C114 110.2(6) . . ? C113 C111 N16 109.8(5) . . ? C114 C111 N16 108.0(5) . . ? C113 C111 C112 113.5(6) . . ? C114 C111 C112 108.8(5) . . ? N16 C111 C112 106.3(5) . . ? N14 C115 N13 106.6(4) . . ? N14 C115 S13 127.5(4) . . ? N13 C115 S13 125.7(4) . . ? C117 C116 N13 108.5(5) . . ? C116 C117 N14 107.9(5) . . ? C121 C118 C120 112.3(7) . . ? C121 C118 N14 108.8(5) . . ? C120 C118 N14 107.9(6) . . ? C121 C118 C119 109.9(7) . . ? C120 C118 C119 109.7(6) . . ? N14 C118 C119 108.2(5) . . ? C29 C210 N24 108.2(5) . . ? C212 C211 N24 107.4(6) . . ? C212 C211 C213 108.4(6) . . ? N24 C211 C213 108.3(5) . . ? C212 C211 C214 109.6(7) . . ? N24 C211 C214 108.2(5) . . ? C213 C211 C214 114.7(7) . . ? N25 C215 N26 106.9(5) . . ? N25 C215 S23 124.6(4) . . ? N26 C215 S23 128.4(4) . . ? C217 C216 N25 106.8(6) . . ? C216 C217 N26 107.4(5) . . ? N26 C218 C219 107.6(6) . . ? N26 C218 C220 109.1(7) . . ? C219 C218 C220 108.2(8) . . ? N26 C218 C221 105.8(6) . . ? C219 C218 C221 117.8(9) . . ? C220 C218 C221 108.1(8) . . ? F1 P F4 170.2(16) . . ? F1 P F5 93.9(6) . . ? F4 P F5 90.6(7) . . ? F1 P F2 85.0(7) . . ? F4 P F2 91.4(7) . . ? F5 P F2 174.4(14) . . ? F1 P F6 77.3(13) . . ? F4 P F6 96.1(13) . . ? F5 P F6 70.8(18) . . ? F2 P F6 114(2) . . ? F1 P F3 104.2(16) . . ? F4 P F3 84.8(8) . . ? F5 P F3 85.4(8) . . ? F2 P F3 89.5(9) . . ? F6 P F3 156.2(19) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.709 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.116 data_danr005 _database_code_depnum_ccdc_archive 'CCDC 229400' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H51 B Co F9 N6.50 P2.50 S3' _chemical_formula_weight 1025.21 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 11.460(2) _cell_length_b 11.460(2) _cell_length_c 44.773(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5092.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 862 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 18.92 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9200 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. Data processed with SQUEEZE from Platon [Spek, A.L. (1990), Acta Cryst. A46, C-34] with void space 410.6 Ang^3 and 121 e/cell consistent with disordered PF6- counterion and cocrystallized half NH4PF6 found in initial solution. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 14167 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 20.00 _reflns_number_total 1597 _reflns_number_gt 1377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.1253P)^2^+79.7191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1597 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.2735 _refine_ls_wR_factor_gt 0.2691 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 1.0000 1.0000 0.11964(5) 0.0194(9) Uani 1 3 d S . . B1 B 1.0000 1.0000 0.1959(6) 0.031(6) Uani 1 3 d S . . H10A H 1.0000 1.0000 0.2182 0.037 Uiso 1 3 calc SR . . S1 S 0.7848(3) 0.9130(3) 0.13572(6) 0.0263(9) Uani 1 1 d . . . P1 P 1.0000 1.0000 0.06767(11) 0.0252(14) Uani 1 3 d S . . N1 N 0.7091(9) 0.6787(9) 0.1670(2) 0.033(3) Uani 1 1 d . . . N2 N 0.8818(10) 0.8596(9) 0.1868(2) 0.035(3) Uani 1 1 d . . . C1 C 0.8138(14) 0.7781(14) 0.0331(3) 0.056(4) Uani 1 1 d . . . H1A H 0.7767 0.8326 0.0274 0.067 Uiso 1 1 calc R . . C2 C 0.7593(15) 0.6490(17) 0.0227(4) 0.075(5) Uani 1 1 d . . . H2A H 0.6855 0.6134 0.0092 0.091 Uiso 1 1 calc R . . C3 C 0.8144(15) 0.5709(14) 0.0322(3) 0.055(4) Uani 1 1 d . . . H3A H 0.7764 0.4812 0.0250 0.066 Uiso 1 1 calc R . . C4 C 0.9211(16) 0.6185(13) 0.0515(3) 0.054(4) Uani 1 1 d . . . H4A H 0.9561 0.5629 0.0577 0.065 Uiso 1 1 calc R . . C5 C 0.9755(15) 0.7466(15) 0.0615(3) 0.053(4) Uani 1 1 d . . . H5A H 1.0494 0.7808 0.0750 0.064 Uiso 1 1 calc R . . C6 C 0.9253(10) 0.8292(10) 0.0526(2) 0.027(3) Uani 1 1 d . . . C7 C 0.7510(14) 0.6414(13) 0.1924(3) 0.041(3) Uani 1 1 d . . . H7A H 0.7111 0.5526 0.2002 0.050 Uiso 1 1 calc R . . C8 C 0.8554(12) 0.7489(12) 0.2042(2) 0.029(3) Uani 1 1 d . . . H8A H 0.9038 0.7500 0.2215 0.035 Uiso 1 1 calc R . . C9 C 0.7920(10) 0.8163(11) 0.1640(2) 0.023(3) Uani 1 1 d . . . C10 C 0.6008(11) 0.5833(12) 0.1462(3) 0.051(4) Uani 1 1 d . . . C11 C 0.6612(16) 0.5839(14) 0.1165(3) 0.063(4) Uani 1 1 d . . . H11A H 0.7266 0.5532 0.1190 0.094 Uiso 1 1 calc R . . H11B H 0.7067 0.6755 0.1084 0.094 Uiso 1 1 calc R . . H11C H 0.5898 0.5234 0.1028 0.094 Uiso 1 1 calc R . . C12 C 0.4954(12) 0.6336(13) 0.1440(4) 0.056(4) Uani 1 1 d . . . H12A H 0.4217 0.5740 0.1307 0.084 Uiso 1 1 calc R . . H12B H 0.5399 0.7257 0.1361 0.084 Uiso 1 1 calc R . . H12C H 0.4591 0.6322 0.1639 0.084 Uiso 1 1 calc R . . C13 C 0.5304(13) 0.4449(11) 0.1596(4) 0.062(4) Uani 1 1 d . . . H13A H 0.5938 0.4113 0.1612 0.094 Uiso 1 1 calc R . . H13B H 0.4547 0.3844 0.1468 0.094 Uiso 1 1 calc R . . H13C H 0.4967 0.4484 0.1795 0.094 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 Co 0.0173(11) 0.0173(11) 0.0236(15) 0.000 0.000 0.0087(5) B1 0.027(9) 0.027(9) 0.039(14) 0.000 0.000 0.013(4) S1 0.0189(16) 0.0257(18) 0.0330(18) 0.0036(13) 0.0019(13) 0.0101(14) P1 0.0231(19) 0.0231(19) 0.029(3) 0.000 0.000 0.0116(10) N1 0.024(6) 0.017(6) 0.064(7) 0.008(5) 0.007(5) 0.014(5) N2 0.049(7) 0.025(6) 0.036(6) 0.001(5) 0.007(6) 0.023(5) C1 0.047(9) 0.044(10) 0.077(10) -0.016(8) -0.008(8) 0.023(8) C2 0.048(10) 0.067(13) 0.090(12) -0.013(10) -0.027(9) 0.012(10) C3 0.060(10) 0.033(9) 0.067(10) -0.012(8) -0.006(9) 0.020(8) C4 0.090(12) 0.025(9) 0.056(9) 0.001(7) 0.014(9) 0.036(8) C5 0.074(10) 0.061(11) 0.047(8) -0.005(8) -0.008(7) 0.051(10) C6 0.008(6) 0.020(7) 0.034(7) 0.004(5) -0.003(5) -0.008(5) C7 0.056(9) 0.026(8) 0.052(8) 0.009(7) 0.007(7) 0.028(8) C8 0.030(7) 0.030(8) 0.032(7) 0.014(6) 0.013(6) 0.018(7) C9 0.019(6) 0.032(8) 0.032(7) 0.003(6) 0.009(6) 0.023(6) C10 0.010(7) 0.028(8) 0.101(12) 0.011(8) -0.015(7) 0.000(6) C11 0.067(10) 0.046(9) 0.068(10) -0.012(8) 0.001(9) 0.023(8) C12 0.019(7) 0.036(8) 0.115(12) 0.012(8) -0.013(7) 0.015(6) C13 0.043(9) 0.011(7) 0.126(14) 0.015(8) 0.000(9) 0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co S1 2.266(3) 3_675 ? Co S1 2.266(3) 2_765 ? Co S1 2.266(3) . ? Co P1 2.327(5) . ? B1 N2 1.552(12) 2_765 ? B1 N2 1.552(12) . ? B1 N2 1.552(12) 3_675 ? S1 C9 1.711(11) . ? P1 C6 1.829(11) 2_765 ? P1 C6 1.829(11) . ? P1 C6 1.829(11) 3_675 ? N1 C9 1.382(14) . ? N1 C7 1.383(14) . ? N1 C10 1.498(15) . ? N2 C9 1.355(14) . ? N2 C8 1.387(14) . ? C1 C2 1.37(2) . ? C1 C6 1.409(17) . ? C2 C3 1.39(2) . ? C3 C4 1.368(19) . ? C4 C5 1.353(18) . ? C5 C6 1.390(17) . ? C7 C8 1.323(16) . ? C10 C11 1.498(19) . ? C10 C13 1.498(17) . ? C10 C12 1.580(17) . ? 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 S1 Co S1 110.41(8) 3_675 2_765 ? S1 Co S1 110.41(8) 3_675 . ? S1 Co S1 110.41(8) 2_765 . ? S1 Co P1 108.52(9) 3_675 . ? S1 Co P1 108.52(9) 2_765 . ? S1 Co P1 108.52(9) . . ? N2 B1 N2 113.3(8) 2_765 . ? N2 B1 N2 113.3(8) 2_765 3_675 ? N2 B1 N2 113.3(8) . 3_675 ? C9 S1 Co 97.2(4) . . ? C6 P1 C6 107.2(4) 2_765 . ? C6 P1 C6 107.2(4) 2_765 3_675 ? C6 P1 C6 107.2(4) . 3_675 ? C6 P1 Co 111.7(4) 2_765 . ? C6 P1 Co 111.7(4) . . ? C6 P1 Co 111.7(4) 3_675 . ? C9 N1 C7 106.6(10) . . ? C9 N1 C10 128.2(10) . . ? C7 N1 C10 125.0(10) . . ? C9 N2 C8 108.0(9) . . ? C9 N2 B1 133.4(11) . . ? C8 N2 B1 118.6(11) . . ? C2 C1 C6 119.3(13) . . ? C1 C2 C3 118.7(14) . . ? C4 C3 C2 122.5(13) . . ? C5 C4 C3 118.6(13) . . ? C4 C5 C6 121.3(13) . . ? C5 C6 C1 119.6(11) . . ? C5 C6 P1 119.4(9) . . ? C1 C6 P1 121.0(9) . . ? C8 C7 N1 109.4(10) . . ? C7 C8 N2 108.1(10) . . ? N2 C9 N1 107.9(9) . . ? N2 C9 S1 126.4(9) . . ? N1 C9 S1 125.7(9) . . ? C11 C10 N1 109.6(10) . . ? C11 C10 C13 111.2(12) . . ? N1 C10 C13 109.7(11) . . ? C11 C10 C12 112.3(12) . . ? N1 C10 C12 106.1(11) . . ? C13 C10 C12 107.8(10) . . ? 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 S1 Co S1 C9 -103.1(4) 3_675 . . . ? S1 Co S1 C9 19.2(4) 2_765 . . . ? P1 Co S1 C9 138.1(4) . . . . ? S1 Co P1 C6 49.5(4) 3_675 . . 2_765 ? S1 Co P1 C6 -70.5(4) 2_765 . . 2_765 ? S1 Co P1 C6 169.5(4) . . . 2_765 ? S1 Co P1 C6 169.5(4) 3_675 . . . ? S1 Co P1 C6 49.5(4) 2_765 . . . ? S1 Co P1 C6 -70.5(4) . . . . ? S1 Co P1 C6 -70.5(4) 3_675 . . 3_675 ? S1 Co P1 C6 169.5(4) 2_765 . . 3_675 ? S1 Co P1 C6 49.5(4) . . . 3_675 ? N2 B1 N2 C9 -100.8(11) 2_765 . . . ? N2 B1 N2 C9 30(2) 3_675 . . . ? N2 B1 N2 C8 78.7(19) 2_765 . . . ? N2 B1 N2 C8 -150.3(12) 3_675 . . . ? C6 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C1 1.4(19) . . . . ? C4 C5 C6 P1 178.3(10) . . . . ? C2 C1 C6 C5 -2(2) . . . . ? C2 C1 C6 P1 -179.0(11) . . . . ? C6 P1 C6 C5 68.2(13) 2_765 . . . ? C6 P1 C6 C5 -177.1(9) 3_675 . . . ? Co P1 C6 C5 -54.5(10) . . . . ? C6 P1 C6 C1 -115.0(7) 2_765 . . . ? C6 P1 C6 C1 -0.2(12) 3_675 . . . ? Co P1 C6 C1 122.4(9) . . . . ? C9 N1 C7 C8 -1.2(12) . . . . ? C10 N1 C7 C8 174.8(10) . . . . ? N1 C7 C8 N2 1.2(13) . . . . ? C9 N2 C8 C7 -0.8(12) . . . . ? B1 N2 C8 C7 179.6(10) . . . . ? C8 N2 C9 N1 0.0(11) . . . . ? B1 N2 C9 N1 179.6(11) . . . . ? C8 N2 C9 S1 -178.1(7) . . . . ? B1 N2 C9 S1 1.5(17) . . . . ? C7 N1 C9 N2 0.7(11) . . . . ? C10 N1 C9 N2 -175.2(10) . . . . ? C7 N1 C9 S1 178.8(8) . . . . ? C10 N1 C9 S1 3.0(15) . . . . ? Co S1 C9 N2 55.1(9) . . . . ? Co S1 C9 N1 -122.7(8) . . . . ? C9 N1 C10 C11 61.6(14) . . . . ? C7 N1 C10 C11 -113.5(12) . . . . ? C9 N1 C10 C13 -176.1(10) . . . . ? C7 N1 C10 C13 8.8(16) . . . . ? C9 N1 C10 C12 -59.9(15) . . . . ? C7 N1 C10 C12 125.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.533 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.113 data_drjs30 _database_code_depnum_ccdc_archive 'CCDC 229401' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H71 B2 Co N7 P S3' _chemical_formula_weight 1157.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 10.7637(18) _cell_length_b 17.534(3) _cell_length_c 18.649(3) _cell_angle_alpha 62.397(3) _cell_angle_beta 82.260(3) _cell_angle_gamma 83.717(3) _cell_volume 3086.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9232 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21220 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 28.34 _reflns_number_total 13531 _reflns_number_gt 7937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0650P)^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 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13531 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.006 _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 0.17655(4) 0.68463(2) 0.27459(2) 0.03065(13) Uani 1 1 d . . . S1 S 0.29191(9) 0.57544(5) 0.36223(5) 0.0450(2) Uani 1 1 d . . . S2 S -0.03101(8) 0.68074(6) 0.28167(5) 0.0428(2) Uani 1 1 d . . . S3 S 0.27035(10) 0.79163(5) 0.16510(5) 0.0453(2) Uani 1 1 d . . . P P 0.15175(8) 0.76144(5) 0.35163(5) 0.0315(2) Uani 1 1 d . . . B1 B 0.1916(4) 0.6151(2) 0.2053(2) 0.0332(8) Uani 1 1 d . . . B2 B 0.0516(4) 0.2479(2) 0.1714(2) 0.0388(9) Uani 1 1 d . . . N11 N 0.2495(3) 0.52229(15) 0.25493(16) 0.0361(7) Uani 1 1 d . . . N12 N 0.3444(3) 0.41890(16) 0.35529(17) 0.0434(7) Uani 1 1 d . . . N13 N 0.0585(3) 0.60978(16) 0.18425(15) 0.0353(6) Uani 1 1 d . . . N14 N -0.1469(3) 0.63199(17) 0.18446(17) 0.0400(7) Uani 1 1 d . . . N15 N 0.2754(3) 0.66375(15) 0.12497(15) 0.0357(6) Uani 1 1 d . . . N16 N 0.3606(3) 0.77714(16) 0.02388(15) 0.0385(7) Uani 1 1 d . . . C11 C 0.2982(3) 0.50195(19) 0.3239(2) 0.0373(8) Uani 1 1 d . . . C12 C 0.2643(4) 0.4508(2) 0.2413(2) 0.0483(9) Uani 1 1 d . . . H12A H 0.2384 0.4473 0.1968 0.058 Uiso 1 1 calc R . . C13 C 0.3212(4) 0.3880(2) 0.3019(2) 0.0503(10) Uani 1 1 d . . . H13A H 0.3424 0.3320 0.3079 0.060 Uiso 1 1 calc R . . C14 C 0.3996(4) 0.3672(2) 0.4349(2) 0.0508(10) Uani 1 1 d . . . C15 C 0.4427(5) 0.2765(2) 0.4436(3) 0.0798(15) Uani 1 1 d . . . H15A H 0.5059 0.2817 0.3995 0.120 Uiso 1 1 calc R . . H15B H 0.3713 0.2485 0.4416 0.120 Uiso 1 1 calc R . . H15C H 0.4778 0.2424 0.4952 0.120 Uiso 1 1 calc R . . C16 C 0.5142(4) 0.4111(3) 0.4359(3) 0.0836(16) Uani 1 1 d . . . H16A H 0.5760 0.4151 0.3915 0.125 Uiso 1 1 calc R . . H16B H 0.5505 0.3775 0.4872 0.125 Uiso 1 1 calc R . . H16C H 0.4888 0.4684 0.4297 0.125 Uiso 1 1 calc R . . C17 C 0.3000(5) 0.3590(3) 0.5034(3) 0.0785(14) Uani 1 1 d . . . H17A H 0.2748 0.4157 0.4990 0.118 Uiso 1 1 calc R . . H17B H 0.3338 0.3233 0.5551 0.118 Uiso 1 1 calc R . . H17C H 0.2278 0.3327 0.4998 0.118 Uiso 1 1 calc R . . C18 C -0.0438(3) 0.63939(18) 0.21513(19) 0.0336(7) Uani 1 1 d . . . C19 C 0.0196(4) 0.5824(2) 0.1326(2) 0.0471(9) Uani 1 1 d . . . H19A H 0.0718 0.5582 0.1030 0.057 Uiso 1 1 calc R . . C21 C 0.0175(3) 0.84013(18) 0.32629(19) 0.0329(7) Uani 1 1 d . . . C22 C 0.0112(3) 0.9005(2) 0.2460(2) 0.0475(9) Uani 1 1 d . . . H22A H 0.0732 0.8982 0.2063 0.057 Uiso 1 1 calc R . . C23 C -0.0834(4) 0.9637(2) 0.2230(2) 0.0542(10) Uani 1 1 d . . . H23A H -0.0855 1.0050 0.1683 0.065 Uiso 1 1 calc R . . C24 C -0.1766(4) 0.9660(2) 0.2816(3) 0.0573(11) Uani 1 1 d . . . H24A H -0.2418 1.0092 0.2665 0.069 Uiso 1 1 calc R . . C25 C -0.1734(4) 0.9060(2) 0.3606(2) 0.0588(11) Uani 1 1 d . . . H25A H -0.2376 0.9070 0.3997 0.071 Uiso 1 1 calc R . . C26 C -0.0766(3) 0.8436(2) 0.3838(2) 0.0456(9) Uani 1 1 d . . . H26A H -0.0742 0.8031 0.4387 0.055 Uiso 1 1 calc R . . C27 C 0.2825(3) 0.82642(19) 0.33897(18) 0.0353(8) Uani 1 1 d . . . C28 C 0.4054(3) 0.7951(2) 0.3302(2) 0.0454(9) Uani 1 1 d . . . H28A H 0.4198 0.7413 0.3300 0.054 Uiso 1 1 calc R . . C29 C 0.5058(4) 0.8415(3) 0.3220(2) 0.0579(11) Uani 1 1 d . . . H29A H 0.5881 0.8197 0.3159 0.069 Uiso 1 1 calc R . . C31 C 0.0833(3) 0.1901(2) 0.2664(2) 0.0412(8) Uani 1 1 d . . . C32 C 0.0617(4) 0.1031(2) 0.3123(2) 0.0515(10) Uani 1 1 d . . . H32A H 0.0345 0.0736 0.2866 0.062 Uiso 1 1 calc R . . C33 C 0.0784(4) 0.0576(2) 0.3947(2) 0.0658(12) Uani 1 1 d . . . H33A H 0.0630 -0.0014 0.4234 0.079 Uiso 1 1 calc R . . C34 C 0.1174(4) 0.0989(3) 0.4340(2) 0.0689(13) Uani 1 1 d . . . H34A H 0.1310 0.0682 0.4893 0.083 Uiso 1 1 calc R . . C35 C 0.1361(5) 0.1845(3) 0.3923(2) 0.0726(13) Uani 1 1 d . . . H35A H 0.1600 0.2139 0.4191 0.087 Uiso 1 1 calc R . . C36 C 0.1200(4) 0.2284(3) 0.3104(2) 0.0618(11) Uani 1 1 d . . . H36A H 0.1346 0.2875 0.2828 0.074 Uiso 1 1 calc R . . C37 C -0.0925(3) 0.2854(2) 0.17995(19) 0.0402(8) Uani 1 1 d . . . C38 C -0.1975(4) 0.2402(3) 0.1878(2) 0.0574(10) Uani 1 1 d . . . H38A H -0.1844 0.1896 0.1816 0.069 Uiso 1 1 calc R . . C39 C -0.3205(4) 0.2670(3) 0.2043(3) 0.0720(13) Uani 1 1 d . . . H39A H -0.3880 0.2347 0.2089 0.086 Uiso 1 1 calc R . . C110 C -0.1060(4) 0.5963(2) 0.1321(2) 0.0500(10) Uani 1 1 d . . . H11A H -0.1567 0.5840 0.1018 0.060 Uiso 1 1 calc R . . C111 C -0.2802(3) 0.6584(2) 0.2020(2) 0.0493(9) Uani 1 1 d . . . C112 C -0.2891(4) 0.7552(2) 0.1786(3) 0.0589(11) Uani 1 1 d . . . H11B H -0.2570 0.7875 0.1221 0.088 Uiso 1 1 calc R . . H11C H -0.2399 0.7654 0.2129 0.088 Uiso 1 1 calc R . . H11D H -0.3762 0.7736 0.1859 0.088 Uiso 1 1 calc R . . C113 C -0.3639(4) 0.6426(3) 0.1508(3) 0.0825(15) Uani 1 1 d . . . H11E H -0.3340 0.6737 0.0938 0.124 Uiso 1 1 calc R . . H11F H -0.4495 0.6626 0.1595 0.124 Uiso 1 1 calc R . . H11G H -0.3612 0.5814 0.1666 0.124 Uiso 1 1 calc R . . C114 C -0.3182(4) 0.6047(3) 0.2918(3) 0.0806(15) Uani 1 1 d . . . H11H H -0.2711 0.6205 0.3233 0.121 Uiso 1 1 calc R . . H11I H -0.3006 0.5441 0.3063 0.121 Uiso 1 1 calc R . . H11J H -0.4073 0.6151 0.3033 0.121 Uiso 1 1 calc R . . C115 C 0.3030(3) 0.74510(19) 0.10051(18) 0.0325(7) Uani 1 1 d . . . C116 C 0.3172(4) 0.6430(2) 0.0622(2) 0.0529(10) Uani 1 1 d . . . H11K H 0.3103 0.5898 0.0626 0.064 Uiso 1 1 calc R . . C117 C 0.3692(4) 0.7123(2) 0.0010(2) 0.0574(11) Uani 1 1 d . . . H11L H 0.4055 0.7162 -0.0493 0.069 Uiso 1 1 calc R . . C118 C 0.4044(4) 0.8675(2) -0.0290(2) 0.0451(9) Uani 1 1 d . . . C119 C 0.2929(4) 0.9308(2) -0.0390(3) 0.0726(14) Uani 1 1 d . . . H11M H 0.2598 0.9265 0.0137 0.109 Uiso 1 1 calc R . . H11N H 0.2284 0.9178 -0.0627 0.109 Uiso 1 1 calc R . . H11O H 0.3190 0.9889 -0.0744 0.109 Uiso 1 1 calc R . . C120 C 0.5055(4) 0.8823(2) 0.0116(2) 0.0635(12) Uani 1 1 d . . . H12B H 0.4704 0.8787 0.0637 0.095 Uiso 1 1 calc R . . H12C H 0.5374 0.9390 -0.0227 0.095 Uiso 1 1 calc R . . H12D H 0.5734 0.8388 0.0197 0.095 Uiso 1 1 calc R . . C121 C 0.4609(5) 0.8745(3) -0.1111(2) 0.0842(16) Uani 1 1 d . . . H12E H 0.3965 0.8663 -0.1383 0.126 Uiso 1 1 calc R . . H12F H 0.5282 0.8305 -0.1030 0.126 Uiso 1 1 calc R . . H12G H 0.4939 0.9310 -0.1442 0.126 Uiso 1 1 calc R . . C210 C 0.4854(4) 0.9203(3) 0.3225(3) 0.0645(12) Uani 1 1 d . . . H21A H 0.5540 0.9515 0.3183 0.077 Uiso 1 1 calc R . . C211 C 0.3646(4) 0.9534(2) 0.3293(3) 0.0670(12) Uani 1 1 d . . . H21B H 0.3508 1.0077 0.3283 0.080 Uiso 1 1 calc R . . C212 C 0.2637(4) 0.9065(2) 0.3374(2) 0.0517(10) Uani 1 1 d . . . H21C H 0.1814 0.9293 0.3419 0.062 Uiso 1 1 calc R . . C213 C 0.1235(3) 0.69600(19) 0.46189(19) 0.0350(8) Uani 1 1 d . . . C214 C 0.1599(4) 0.7197(2) 0.5162(2) 0.0549(10) Uani 1 1 d . . . H21D H 0.2045 0.7698 0.4967 0.066 Uiso 1 1 calc R . . C215 C 0.1319(4) 0.6711(3) 0.5995(2) 0.0668(12) Uani 1 1 d . . . H21E H 0.1563 0.6885 0.6360 0.080 Uiso 1 1 calc R . . C216 C 0.0681(4) 0.5974(3) 0.6277(2) 0.0632(12) Uani 1 1 d . . . H21F H 0.0492 0.5641 0.6840 0.076 Uiso 1 1 calc R . . C217 C 0.0319(4) 0.5718(2) 0.5753(2) 0.0620(12) Uani 1 1 d . . . H21G H -0.0119 0.5213 0.5954 0.074 Uiso 1 1 calc R . . C218 C 0.0599(4) 0.6208(2) 0.4917(2) 0.0520(10) Uani 1 1 d . . . H21H H 0.0356 0.6029 0.4555 0.062 Uiso 1 1 calc R . . C310 C -0.3422(4) 0.3409(3) 0.2137(2) 0.0671(13) Uani 1 1 d . . . H31A H -0.4248 0.3600 0.2236 0.081 Uiso 1 1 calc R . . C311 C -0.2431(4) 0.3865(3) 0.2086(2) 0.0607(11) Uani 1 1 d . . . H31B H -0.2571 0.4362 0.2163 0.073 Uiso 1 1 calc R . . C312 C -0.1215(4) 0.3587(2) 0.1920(2) 0.0474(9) Uani 1 1 d . . . H31C H -0.0549 0.3911 0.1888 0.057 Uiso 1 1 calc R . . C313 C 0.1528(3) 0.32529(19) 0.12116(19) 0.0361(8) Uani 1 1 d . . . C314 C 0.2787(4) 0.3125(2) 0.1351(2) 0.0494(9) Uani 1 1 d . . . H31D H 0.3054 0.2600 0.1775 0.059 Uiso 1 1 calc R . . C315 C 0.3668(4) 0.3727(2) 0.0900(2) 0.0540(10) Uani 1 1 d . . . H31E H 0.4509 0.3611 0.1020 0.065 Uiso 1 1 calc R . . C316 C 0.3298(4) 0.4516(2) 0.0262(2) 0.0505(10) Uani 1 1 d . . . H31F H 0.3888 0.4931 -0.0057 0.061 Uiso 1 1 calc R . . C317 C 0.2059(4) 0.4671(2) 0.0113(2) 0.0457(9) Uani 1 1 d . . . H31G H 0.1789 0.5198 -0.0307 0.055 Uiso 1 1 calc R . . C318 C 0.1201(3) 0.4047(2) 0.05852(19) 0.0413(8) Uani 1 1 d . . . H31H H 0.0356 0.4170 0.0474 0.050 Uiso 1 1 calc R . . C319 C 0.0667(3) 0.1931(2) 0.1189(2) 0.0387(8) Uani 1 1 d . . . C320 C -0.0018(4) 0.2161(2) 0.0527(2) 0.0490(9) Uani 1 1 d . . . H32B H -0.0619 0.2625 0.0402 0.059 Uiso 1 1 calc R . . C321 C 0.0139(4) 0.1741(3) 0.0045(2) 0.0578(11) Uani 1 1 d . . . H32C H -0.0340 0.1929 -0.0399 0.069 Uiso 1 1 calc R . . C322 C 0.0995(4) 0.1048(3) 0.0213(3) 0.0608(12) Uani 1 1 d . . . H32D H 0.1087 0.0752 -0.0102 0.073 Uiso 1 1 calc R . . C323 C 0.1717(4) 0.0798(2) 0.0854(3) 0.0596(11) Uani 1 1 d . . . H32E H 0.2310 0.0330 0.0974 0.072 Uiso 1 1 calc R . . C324 C 0.1564(4) 0.1241(2) 0.1328(2) 0.0473(9) Uani 1 1 d . . . H32F H 0.2079 0.1071 0.1751 0.057 Uiso 1 1 calc R . . C2S C 0.2804(12) 0.8794(7) 0.5828(6) 0.212(5) Uani 1 1 d . . . H2SA H 0.2193 0.8526 0.6293 0.318 Uiso 1 1 calc R . . H2SB H 0.3175 0.8370 0.5654 0.318 Uiso 1 1 calc R . . H2SC H 0.2392 0.9263 0.5387 0.318 Uiso 1 1 calc R . . C1S C 0.3822(12) 0.9142(7) 0.6063(8) 0.191(5) Uani 1 1 d . . . N1S N 0.4558(16) 0.9442(13) 0.5860(18) 0.58(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0346(3) 0.0292(2) 0.0274(2) -0.01261(17) -0.00118(19) -0.00230(18) S1 0.0555(6) 0.0396(4) 0.0418(5) -0.0194(4) -0.0153(4) 0.0072(4) S2 0.0366(5) 0.0578(5) 0.0461(5) -0.0347(4) -0.0010(4) -0.0019(4) S3 0.0659(7) 0.0352(4) 0.0368(5) -0.0197(4) 0.0100(5) -0.0141(4) P 0.0358(5) 0.0301(4) 0.0278(4) -0.0125(3) -0.0023(4) -0.0020(4) B1 0.036(2) 0.0317(18) 0.034(2) -0.0168(16) -0.0010(17) -0.0020(16) B2 0.044(2) 0.0341(19) 0.039(2) -0.0169(17) -0.0058(19) -0.0009(18) N11 0.0436(18) 0.0299(13) 0.0337(15) -0.0141(12) -0.0024(13) 0.0003(12) N12 0.0449(19) 0.0313(14) 0.0473(18) -0.0136(13) -0.0041(15) 0.0045(13) N13 0.0385(17) 0.0359(14) 0.0354(15) -0.0194(12) -0.0024(13) -0.0040(12) N14 0.0364(17) 0.0405(15) 0.0483(18) -0.0235(14) -0.0074(14) -0.0021(13) N15 0.0417(17) 0.0328(13) 0.0309(14) -0.0149(12) 0.0041(13) -0.0031(12) N16 0.0454(18) 0.0406(15) 0.0264(14) -0.0137(12) 0.0054(13) -0.0091(13) C11 0.035(2) 0.0314(16) 0.0393(19) -0.0133(15) 0.0058(16) -0.0044(15) C12 0.061(3) 0.0385(18) 0.050(2) -0.0245(17) -0.007(2) 0.0022(18) C13 0.061(3) 0.0321(17) 0.056(2) -0.0202(17) -0.001(2) 0.0047(17) C14 0.048(2) 0.0421(19) 0.047(2) -0.0067(17) -0.0095(19) 0.0018(18) C15 0.099(4) 0.043(2) 0.075(3) -0.009(2) -0.025(3) 0.023(2) C16 0.063(3) 0.062(3) 0.103(4) -0.012(3) -0.035(3) 0.000(2) C17 0.079(3) 0.072(3) 0.054(3) -0.008(2) 0.000(3) 0.008(3) C18 0.035(2) 0.0317(16) 0.0349(18) -0.0159(14) -0.0009(15) -0.0037(14) C19 0.052(3) 0.053(2) 0.052(2) -0.0372(19) -0.0045(19) -0.0032(19) C21 0.0339(19) 0.0311(15) 0.0363(18) -0.0166(14) -0.0035(15) -0.0049(14) C22 0.044(2) 0.049(2) 0.038(2) -0.0118(17) -0.0024(17) -0.0001(18) C23 0.043(2) 0.049(2) 0.051(2) -0.0052(18) -0.011(2) 0.0018(18) C24 0.037(2) 0.048(2) 0.071(3) -0.014(2) -0.011(2) 0.0067(18) C25 0.044(2) 0.061(2) 0.061(3) -0.023(2) 0.004(2) 0.001(2) C26 0.041(2) 0.0454(19) 0.045(2) -0.0167(17) -0.0022(18) 0.0009(17) C27 0.041(2) 0.0367(17) 0.0286(17) -0.0146(14) -0.0052(15) -0.0042(15) C28 0.043(2) 0.050(2) 0.046(2) -0.0245(17) -0.0049(17) 0.0003(18) C29 0.036(2) 0.076(3) 0.064(3) -0.034(2) -0.006(2) -0.005(2) C31 0.046(2) 0.0357(17) 0.040(2) -0.0162(15) -0.0040(17) -0.0007(16) C32 0.062(3) 0.0429(19) 0.045(2) -0.0181(17) 0.005(2) -0.0048(18) C33 0.085(3) 0.045(2) 0.046(2) -0.0067(19) 0.004(2) 0.002(2) C34 0.084(3) 0.076(3) 0.034(2) -0.014(2) -0.012(2) 0.006(3) C35 0.103(4) 0.074(3) 0.044(2) -0.025(2) -0.012(2) -0.020(3) C36 0.083(3) 0.053(2) 0.046(2) -0.0175(19) -0.010(2) -0.010(2) C37 0.045(2) 0.0415(18) 0.0287(18) -0.0112(15) -0.0055(16) -0.0010(16) C38 0.054(3) 0.064(2) 0.064(3) -0.038(2) -0.002(2) -0.006(2) C39 0.047(3) 0.108(4) 0.067(3) -0.044(3) -0.002(2) -0.012(3) C110 0.054(3) 0.053(2) 0.057(2) -0.0344(19) -0.012(2) -0.0054(19) C111 0.034(2) 0.053(2) 0.063(3) -0.0266(19) -0.0096(19) -0.0003(17) C112 0.054(3) 0.056(2) 0.068(3) -0.030(2) -0.014(2) 0.008(2) C113 0.050(3) 0.085(3) 0.140(5) -0.071(3) -0.038(3) 0.012(2) C114 0.042(3) 0.081(3) 0.084(3) -0.012(3) 0.014(2) -0.008(2) C115 0.0319(19) 0.0323(16) 0.0312(17) -0.0131(14) -0.0023(14) -0.0005(14) C116 0.069(3) 0.051(2) 0.051(2) -0.0350(19) 0.013(2) -0.017(2) C117 0.080(3) 0.056(2) 0.042(2) -0.0309(19) 0.023(2) -0.021(2) C118 0.051(2) 0.0398(18) 0.0347(19) -0.0085(15) 0.0006(17) -0.0102(17) C119 0.066(3) 0.046(2) 0.071(3) 0.002(2) -0.008(2) 0.001(2) C120 0.061(3) 0.056(2) 0.063(3) -0.014(2) -0.006(2) -0.022(2) C121 0.130(5) 0.074(3) 0.038(2) -0.019(2) 0.030(3) -0.045(3) C210 0.047(3) 0.070(3) 0.073(3) -0.024(2) -0.013(2) -0.019(2) C211 0.061(3) 0.047(2) 0.098(3) -0.032(2) -0.018(3) -0.012(2) C212 0.043(2) 0.048(2) 0.072(3) -0.0323(19) -0.012(2) -0.0028(18) C213 0.038(2) 0.0367(16) 0.0296(17) -0.0157(14) -0.0033(15) 0.0040(15) C214 0.068(3) 0.057(2) 0.037(2) -0.0180(18) -0.008(2) -0.009(2) C215 0.093(4) 0.075(3) 0.033(2) -0.023(2) -0.007(2) -0.016(3) C216 0.077(3) 0.062(3) 0.029(2) -0.0070(19) 0.004(2) 0.002(2) C217 0.080(3) 0.050(2) 0.040(2) -0.0088(18) 0.010(2) -0.012(2) C218 0.066(3) 0.046(2) 0.042(2) -0.0188(17) 0.0019(19) -0.0103(19) C310 0.051(3) 0.099(3) 0.047(2) -0.035(2) -0.005(2) 0.018(3) C311 0.068(3) 0.062(2) 0.044(2) -0.022(2) 0.000(2) 0.014(2) C312 0.057(3) 0.045(2) 0.036(2) -0.0162(16) -0.0012(18) -0.0015(18) C313 0.042(2) 0.0353(16) 0.0346(18) -0.0191(14) -0.0063(16) 0.0032(15) C314 0.052(3) 0.0406(19) 0.053(2) -0.0192(17) -0.011(2) 0.0054(18) C315 0.036(2) 0.064(2) 0.067(3) -0.035(2) -0.005(2) 0.0016(19) C316 0.050(3) 0.052(2) 0.057(2) -0.0323(19) 0.011(2) -0.0143(19) C317 0.053(3) 0.0442(19) 0.038(2) -0.0169(16) -0.0043(18) -0.0043(18) C318 0.038(2) 0.0488(19) 0.0357(19) -0.0182(16) -0.0046(16) -0.0021(17) C319 0.044(2) 0.0360(17) 0.0369(19) -0.0171(15) 0.0017(16) -0.0089(16) C320 0.057(3) 0.046(2) 0.047(2) -0.0245(17) -0.0025(19) -0.0013(18) C321 0.065(3) 0.064(2) 0.048(2) -0.028(2) 0.002(2) -0.014(2) C322 0.072(3) 0.068(3) 0.054(3) -0.040(2) 0.019(2) -0.027(2) C323 0.061(3) 0.047(2) 0.067(3) -0.028(2) 0.020(2) -0.006(2) C324 0.047(2) 0.0449(19) 0.051(2) -0.0239(17) 0.0046(18) -0.0076(18) C2S 0.258(14) 0.207(11) 0.145(8) -0.076(8) -0.070(9) 0.133(10) C1S 0.166(11) 0.130(7) 0.243(13) -0.067(8) 0.022(9) -0.011(7) N1S 0.33(2) 0.54(3) 1.11(6) -0.56(4) 0.05(3) -0.242(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co B1 2.132(4) . ? Co S2 2.2269(11) . ? Co S1 2.2372(10) . ? Co S3 2.2400(9) . ? Co P 2.3581(10) . ? S1 C11 1.731(3) . ? S2 C18 1.728(3) . ? S3 C115 1.725(3) . ? P C27 1.829(3) . ? P C21 1.833(3) . ? P C213 1.833(3) . ? B1 N15 1.551(4) . ? B1 N13 1.558(5) . ? B1 N11 1.559(4) . ? B2 C37 1.635(5) . ? B2 C319 1.644(5) . ? B2 C31 1.645(5) . ? B2 C313 1.665(5) . ? N11 C11 1.331(4) . ? N11 C12 1.378(4) . ? N12 C11 1.357(4) . ? N12 C13 1.394(5) . ? N12 C14 1.500(4) . ? N13 C18 1.339(4) . ? N13 C19 1.384(4) . ? N14 C18 1.359(4) . ? N14 C110 1.389(4) . ? N14 C111 1.500(4) . ? N15 C115 1.336(4) . ? N15 C116 1.387(4) . ? N16 C115 1.355(4) . ? N16 C117 1.378(4) . ? N16 C118 1.515(4) . ? C12 C13 1.323(5) . ? C14 C17 1.515(5) . ? C14 C16 1.530(6) . ? C14 C15 1.546(5) . ? C19 C110 1.347(5) . ? C21 C22 1.383(4) . ? C21 C26 1.390(4) . ? C22 C23 1.371(5) . ? C23 C24 1.392(5) . ? C24 C25 1.360(5) . ? C25 C26 1.380(5) . ? C27 C212 1.383(4) . ? C27 C28 1.395(5) . ? C28 C29 1.373(5) . ? C29 C210 1.380(5) . ? C31 C32 1.388(4) . ? C31 C36 1.392(5) . ? C32 C33 1.393(5) . ? C33 C34 1.369(6) . ? C34 C35 1.358(6) . ? C35 C36 1.381(5) . ? C37 C312 1.401(5) . ? C37 C38 1.404(5) . ? C38 C39 1.399(6) . ? C39 C310 1.378(6) . ? C111 C114 1.515(5) . ? C111 C113 1.528(5) . ? C111 C112 1.538(5) . ? C116 C117 1.336(5) . ? C118 C119 1.512(5) . ? C118 C120 1.513(5) . ? C118 C121 1.523(5) . ? C210 C211 1.379(6) . ? C211 C212 1.384(5) . ? C213 C214 1.373(5) . ? C213 C218 1.390(5) . ? C214 C215 1.390(5) . ? C215 C216 1.373(6) . ? C216 C217 1.362(6) . ? C217 C218 1.396(5) . ? C310 C311 1.370(6) . ? C311 C312 1.392(5) . ? C313 C318 1.387(4) . ? C313 C314 1.390(5) . ? C314 C315 1.379(5) . ? C315 C316 1.404(5) . ? C316 C317 1.372(5) . ? C317 C318 1.390(5) . ? C319 C320 1.396(5) . ? C319 C324 1.409(5) . ? C320 C321 1.388(5) . ? C321 C322 1.379(6) . ? C322 C323 1.384(6) . ? C323 C324 1.407(5) . ? C2S C1S 1.512(14) . ? C1S N1S 0.934(15) . ? 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 B1 Co S2 87.52(11) . . ? B1 Co S1 86.79(10) . . ? S2 Co S1 121.56(4) . . ? B1 Co S3 87.33(10) . . ? S2 Co S3 117.56(4) . . ? S1 Co S3 120.18(4) . . ? B1 Co P 177.88(11) . . ? S2 Co P 90.36(3) . . ? S1 Co P 94.30(4) . . ? S3 Co P 93.68(3) . . ? C11 S1 Co 101.12(12) . . ? C18 S2 Co 101.03(12) . . ? C115 S3 Co 100.89(10) . . ? C27 P C21 103.13(14) . . ? C27 P C213 104.24(15) . . ? C21 P C213 103.70(14) . . ? C27 P Co 115.92(11) . . ? C21 P Co 112.77(11) . . ? C213 P Co 115.57(11) . . ? N15 B1 N13 108.7(3) . . ? N15 B1 N11 110.2(3) . . ? N13 B1 N11 109.5(3) . . ? N15 B1 Co 109.1(2) . . ? N13 B1 Co 109.2(2) . . ? N11 B1 Co 110.0(2) . . ? C37 B2 C319 112.5(3) . . ? C37 B2 C31 103.2(3) . . ? C319 B2 C31 113.8(3) . . ? C37 B2 C313 113.0(3) . . ? C319 B2 C313 104.0(3) . . ? C31 B2 C313 110.6(3) . . ? C11 N11 C12 108.1(3) . . ? C11 N11 B1 119.8(3) . . ? C12 N11 B1 132.1(3) . . ? C11 N12 C13 106.3(3) . . ? C11 N12 C14 127.5(3) . . ? C13 N12 C14 126.0(3) . . ? C18 N13 C19 107.5(3) . . ? C18 N13 B1 120.5(3) . . ? C19 N13 B1 131.8(3) . . ? C18 N14 C110 107.2(3) . . ? C18 N14 C111 127.0(3) . . ? C110 N14 C111 125.8(3) . . ? C115 N15 C116 107.7(3) . . ? C115 N15 B1 120.5(3) . . ? C116 N15 B1 131.0(3) . . ? C115 N16 C117 107.0(3) . . ? C115 N16 C118 127.5(3) . . ? C117 N16 C118 125.5(3) . . ? N11 C11 N12 109.2(3) . . ? N11 C11 S1 121.1(2) . . ? N12 C11 S1 129.7(3) . . ? C13 C12 N11 108.1(3) . . ? C12 C13 N12 108.4(3) . . ? N12 C14 C17 109.0(3) . . ? N12 C14 C16 109.4(3) . . ? C17 C14 C16 111.6(4) . . ? N12 C14 C15 108.9(3) . . ? C17 C14 C15 109.4(3) . . ? C16 C14 C15 108.6(4) . . ? N13 C18 N14 109.4(3) . . ? N13 C18 S2 120.6(3) . . ? N14 C18 S2 130.0(3) . . ? C110 C19 N13 108.4(3) . . ? C22 C21 C26 118.4(3) . . ? C22 C21 P 118.1(3) . . ? C26 C21 P 123.5(2) . . ? C23 C22 C21 121.4(4) . . ? C22 C23 C24 119.3(3) . . ? C25 C24 C23 120.1(4) . . ? C24 C25 C26 120.4(4) . . ? C25 C26 C21 120.4(3) . . ? C212 C27 C28 118.4(3) . . ? C212 C27 P 122.1(3) . . ? C28 C27 P 119.5(2) . . ? C29 C28 C27 121.0(3) . . ? C28 C29 C210 119.8(4) . . ? C32 C31 C36 114.2(3) . . ? C32 C31 B2 124.2(3) . . ? C36 C31 B2 121.2(3) . . ? C31 C32 C33 123.0(4) . . ? C34 C33 C32 119.9(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 119.8(4) . . ? C35 C36 C31 123.7(4) . . ? C312 C37 C38 114.1(3) . . ? C312 C37 B2 122.6(3) . . ? C38 C37 B2 122.7(3) . . ? C39 C38 C37 123.1(4) . . ? C310 C39 C38 119.6(4) . . ? C19 C110 N14 107.5(3) . . ? N14 C111 C114 108.0(3) . . ? N14 C111 C113 109.0(3) . . ? C114 C111 C113 110.5(4) . . ? N14 C111 C112 109.1(3) . . ? C114 C111 C112 111.3(3) . . ? C113 C111 C112 108.9(3) . . ? N15 C115 N16 109.2(3) . . ? N15 C115 S3 120.7(2) . . ? N16 C115 S3 130.1(2) . . ? C117 C116 N15 107.6(3) . . ? C116 C117 N16 108.5(3) . . ? C119 C118 C120 111.6(3) . . ? C119 C118 N16 108.6(3) . . ? C120 C118 N16 108.3(3) . . ? C119 C118 C121 110.8(3) . . ? C120 C118 C121 108.7(3) . . ? N16 C118 C121 108.8(3) . . ? C211 C210 C29 120.1(4) . . ? C210 C211 C212 119.9(4) . . ? C27 C212 C211 120.7(4) . . ? C214 C213 C218 118.7(3) . . ? C214 C213 P 122.4(3) . . ? C218 C213 P 118.8(3) . . ? C213 C214 C215 121.3(4) . . ? C216 C215 C214 119.1(4) . . ? C217 C216 C215 120.9(4) . . ? C216 C217 C218 119.9(4) . . ? C213 C218 C217 120.1(4) . . ? C311 C310 C39 119.8(4) . . ? C310 C311 C312 119.5(4) . . ? C311 C312 C37 123.9(4) . . ? C318 C313 C314 115.0(3) . . ? C318 C313 B2 122.7(3) . . ? C314 C313 B2 122.1(3) . . ? C315 C314 C313 123.5(3) . . ? C314 C315 C316 119.5(4) . . ? C317 C316 C315 118.6(3) . . ? C316 C317 C318 119.9(3) . . ? C313 C318 C317 123.4(3) . . ? C320 C319 C324 114.8(3) . . ? C320 C319 B2 122.2(3) . . ? C324 C319 B2 122.8(3) . . ? C321 C320 C319 123.5(4) . . ? C322 C321 C320 120.3(4) . . ? C321 C322 C323 118.9(4) . . ? C322 C323 C324 120.1(4) . . ? C323 C324 C319 122.3(4) . . ? N1S C1S C2S 143(3) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.443 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.057