# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Damir Safin' _publ_contact_author_email damir.safin@ksu.ru _publ_author_name M.Babashkina data_CoL2-100K _database_code_depnum_ccdc_archive 'CCDC 893875' #TrackingRef '[CoL2]100K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 Co N4 O8 P2 S4' _chemical_formula_sum 'C30 H44 Co N4 O8 P2 S4' _chemical_formula_weight 837.80 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.459(3) _cell_length_b 11.329(3) _cell_length_c 17.261(4) _cell_angle_alpha 78.15(2) _cell_angle_beta 84.00(2) _cell_angle_gamma 85.35(2) _cell_volume 1987.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21600 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 36.78 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.8893 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2009)' _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 'Kuma KM4CCD \k-axis diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25353 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9119 _reflns_number_gt 8018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0491P)^2^+0.4358P] 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 9119 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.977815(18) 0.142150(17) 0.234265(11) 0.01749(6) Uani 1 1 d . . . S1 S 1.03542(3) 0.20662(3) 0.09898(2) 0.02091(8) Uani 1 1 d . . . S2 S 0.80127(4) 0.03235(4) 0.24661(2) 0.02326(8) Uani 1 1 d . . . P1 P 0.85950(3) 0.20627(3) 0.06404(2) 0.01615(8) Uani 1 1 d . . . O1 O 0.75913(9) 0.30044(9) 0.09577(6) 0.0187(2) Uani 1 1 d . . . O2 O 0.86325(10) 0.25020(9) -0.02865(6) 0.0203(2) Uani 1 1 d . . . O3 O 0.45464(12) -0.37200(11) 0.24004(8) 0.0364(3) Uani 1 1 d . . . O4 O 0.58179(14) -0.24768(12) 0.27517(7) 0.0416(3) Uani 1 1 d . . . N1 N 0.79213(12) 0.07930(11) 0.08369(7) 0.0195(2) Uani 1 1 d . . . N2 N 0.69290(13) -0.08530(11) 0.16200(7) 0.0232(3) Uani 1 1 d . . . H2 H 0.6839 -0.1269 0.2097 0.028 Uiso 1 1 calc R . . C1 C 0.76390(13) 0.01270(13) 0.15387(8) 0.0184(3) Uani 1 1 d . . . C2 C 0.78514(15) 0.42818(13) 0.09084(9) 0.0235(3) Uani 1 1 d . . . H2A H 0.8769 0.4347 0.0951 0.028 Uiso 1 1 calc R . . C3 C 0.70648(16) 0.46737(15) 0.16030(9) 0.0271(3) Uani 1 1 d . . . H3A H 0.7337 0.4191 0.2089 0.041 Uiso 1 1 calc R . . H3B H 0.6171 0.4572 0.1572 0.041 Uiso 1 1 calc R . . H3C H 0.7185 0.5509 0.1591 0.041 Uiso 1 1 calc R . . C4 C 0.7476(2) 0.50152(16) 0.01184(11) 0.0426(5) Uani 1 1 d . . . H4A H 0.8000 0.4736 -0.0307 0.064 Uiso 1 1 calc R . . H4B H 0.7604 0.5852 0.0092 0.064 Uiso 1 1 calc R . . H4C H 0.6586 0.4921 0.0069 0.064 Uiso 1 1 calc R . . C5 C 0.95294(16) 0.19648(14) -0.08526(9) 0.0261(3) Uani 1 1 d . . . H5 H 0.9961 0.1223 -0.0573 0.031 Uiso 1 1 calc R . . C6 C 1.05090(17) 0.28765(19) -0.11997(10) 0.0358(4) Uani 1 1 d . . . H6A H 1.0984 0.3021 -0.0785 0.054 Uiso 1 1 calc R . . H6B H 1.0078 0.3619 -0.1445 0.054 Uiso 1 1 calc R . . H6C H 1.1091 0.2571 -0.1591 0.054 Uiso 1 1 calc R . . C7 C 0.8737(2) 0.16688(19) -0.14603(10) 0.0405(4) Uani 1 1 d . . . H7A H 0.8137 0.1081 -0.1203 0.061 Uiso 1 1 calc R . . H7B H 0.9295 0.1347 -0.1855 0.061 Uiso 1 1 calc R . . H7C H 0.8274 0.2389 -0.1710 0.061 Uiso 1 1 calc R . . C8 C 0.63171(14) -0.13089(13) 0.10664(9) 0.0221(3) Uani 1 1 d . . . C9 C 0.54611(14) -0.22437(14) 0.13696(10) 0.0248(3) Uani 1 1 d . . . C10 C 0.47968(15) -0.26855(15) 0.08363(11) 0.0299(3) Uani 1 1 d . . . H10 H 0.4225 -0.3287 0.1030 0.036 Uiso 1 1 calc R . . C11 C 0.49758(16) -0.22450(16) 0.00284(11) 0.0321(4) Uani 1 1 d . . . H11 H 0.4512 -0.2531 -0.0318 0.038 Uiso 1 1 calc R . . C12 C 0.58562(17) -0.13697(15) -0.02617(10) 0.0305(3) Uani 1 1 d . . . H12 H 0.6000 -0.1094 -0.0808 0.037 Uiso 1 1 calc R . . C13 C 0.65232(16) -0.08994(14) 0.02461(9) 0.0267(3) Uani 1 1 d . . . H13 H 0.7107 -0.0312 0.0041 0.032 Uiso 1 1 calc R . . C14 C 0.53029(16) -0.27849(15) 0.22328(10) 0.0297(3) Uani 1 1 d . . . C15 C 0.4464(2) -0.43403(19) 0.32270(12) 0.0474(5) Uani 1 1 d . . . H15A H 0.3910 -0.4997 0.3299 0.071 Uiso 1 1 calc R . . H15B H 0.4120 -0.3785 0.3559 0.071 Uiso 1 1 calc R . . H15C H 0.5308 -0.4649 0.3370 0.071 Uiso 1 1 calc R . . S3 S 1.14453(4) 0.02094(3) 0.29313(2) 0.02337(8) Uani 1 1 d . . . S4 S 0.93856(4) 0.30192(3) 0.29681(2) 0.02364(9) Uani 1 1 d . . . P2 P 1.19618(3) 0.13134(3) 0.35926(2) 0.01611(8) Uani 1 1 d . A . O5 O 1.26950(10) 0.24242(9) 0.31089(6) 0.0207(2) Uani 1 1 d . . . O6 O 1.29862(9) 0.06088(9) 0.41515(6) 0.0186(2) Uani 1 1 d . . . O7 O 0.72602(10) 0.60240(10) 0.53536(6) 0.0249(2) Uani 1 1 d . . . O8 O 0.71110(11) 0.47646(10) 0.45261(7) 0.0279(2) Uani 1 1 d . . . N3 N 1.08455(11) 0.18435(11) 0.41694(7) 0.0185(2) Uani 1 1 d . . . N4 N 0.90803(12) 0.31004(11) 0.44665(7) 0.0201(2) Uani 1 1 d . . . H4 H 0.8325 0.3351 0.4325 0.024 Uiso 1 1 calc R A . C16 C 0.98603(13) 0.25667(12) 0.39362(8) 0.0182(3) Uani 1 1 d . A . C17 C 1.35612(19) 0.23826(16) 0.23853(11) 0.0369(6) Uani 0.549(6) 1 d P A 1 H17A H 1.3440 0.1687 0.2149 0.044 Uiso 0.549(6) 1 calc PR A 1 C17A C 1.35612(19) 0.23826(16) 0.23853(11) 0.0369(6) Uani 0.45 1 d P A 2 H17B H 1.3226 0.1779 0.2140 0.044 Uiso 0.451(6) 1 calc PR A 2 C18 C 1.3331(2) 0.35657(19) 0.18301(11) 0.0418(5) Uani 1 1 d . . . H18A H 1.2453 0.3651 0.1702 0.063 Uiso 1 1 calc R A 1 H18B H 1.3896 0.3591 0.1352 0.063 Uiso 1 1 calc R A 1 H18C H 1.3496 0.4214 0.2080 0.063 Uiso 1 1 calc R A 1 C19A C 1.4997(4) 0.2321(4) 0.2725(2) 0.0396(9) Uiso 0.549(6) 1 d P A 1 H19A H 1.5139 0.1561 0.3081 0.059 Uiso 0.549(6) 1 calc PR A 1 H19B H 1.5030 0.2968 0.3003 0.059 Uiso 0.549(6) 1 calc PR A 1 H19C H 1.5651 0.2398 0.2288 0.059 Uiso 0.549(6) 1 calc PR A 1 C19B C 1.4828(4) 0.1997(4) 0.2490(2) 0.0269(10) Uiso 0.451(6) 1 d P A 2 H19D H 1.5090 0.1384 0.2186 0.040 Uiso 0.451(6) 1 calc PR A 2 H19E H 1.4912 0.1672 0.3042 0.040 Uiso 0.451(6) 1 calc PR A 2 H19F H 1.5363 0.2668 0.2313 0.040 Uiso 0.451(6) 1 calc PR A 2 C20 C 1.27025(14) -0.05647(13) 0.46795(8) 0.0208(3) Uani 1 1 d . A . H20 H 1.1787 -0.0702 0.4690 0.025 Uiso 1 1 calc R . . C21 C 1.30112(19) -0.04772(17) 0.54988(9) 0.0341(4) Uani 1 1 d . . . H21A H 1.2467 0.0154 0.5679 0.051 Uiso 1 1 calc R A . H21B H 1.3897 -0.0298 0.5481 0.051 Uiso 1 1 calc R . . H21C H 1.2867 -0.1232 0.5858 0.051 Uiso 1 1 calc R . . C22 C 1.35112(16) -0.15381(15) 0.43386(10) 0.0303(3) Uani 1 1 d . . . H22A H 1.3265 -0.1548 0.3820 0.045 Uiso 1 1 calc R A . H22B H 1.3378 -0.2309 0.4680 0.045 Uiso 1 1 calc R . . H22C H 1.4405 -0.1375 0.4300 0.045 Uiso 1 1 calc R . . C23 C 0.93387(13) 0.32992(13) 0.52131(8) 0.0185(3) Uani 1 1 d . A . C24 C 0.86669(13) 0.42866(13) 0.54959(8) 0.0186(3) Uani 1 1 d . . . C25 C 0.89979(15) 0.45730(14) 0.61986(9) 0.0228(3) Uani 1 1 d . A . H25 H 0.8580 0.5237 0.6377 0.027 Uiso 1 1 calc R . . C26 C 0.99312(16) 0.38895(15) 0.66299(9) 0.0276(3) Uani 1 1 d . . . H26 H 1.0156 0.4101 0.7089 0.033 Uiso 1 1 calc R A . C27 C 1.05342(16) 0.28796(15) 0.63719(9) 0.0268(3) Uani 1 1 d . A . H27 H 1.1140 0.2398 0.6673 0.032 Uiso 1 1 calc R . . C28 C 1.02457(15) 0.25814(14) 0.56744(8) 0.0228(3) Uani 1 1 d . . . H28 H 1.0655 0.1902 0.5511 0.027 Uiso 1 1 calc R A . C29 C 0.76220(14) 0.50249(13) 0.50656(8) 0.0206(3) Uani 1 1 d . A . C30 C 0.62253(17) 0.67809(16) 0.49804(11) 0.0322(4) Uani 1 1 d . . . H30A H 0.6038 0.7470 0.5226 0.048 Uiso 1 1 calc R . . H30B H 0.5472 0.6328 0.5042 0.048 Uiso 1 1 calc R . . H30C H 0.6479 0.7048 0.4425 0.048 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 0.01993(10) 0.01792(10) 0.01624(10) -0.00531(7) -0.00527(7) -0.00109(7) S1 0.01794(16) 0.02719(19) 0.01809(16) -0.00429(13) -0.00303(12) -0.00310(13) S2 0.02618(18) 0.0288(2) 0.01630(16) -0.00476(14) -0.00220(13) -0.00954(15) P1 0.01843(16) 0.01644(17) 0.01415(16) -0.00316(12) -0.00272(12) -0.00259(13) O1 0.0194(5) 0.0164(5) 0.0201(5) -0.0029(4) -0.0010(4) -0.0029(4) O2 0.0251(5) 0.0209(5) 0.0145(4) -0.0030(4) -0.0022(4) -0.0002(4) O3 0.0363(6) 0.0314(6) 0.0428(7) -0.0134(5) 0.0133(5) -0.0168(5) O4 0.0594(9) 0.0366(7) 0.0306(6) -0.0053(5) 0.0026(6) -0.0254(6) N1 0.0234(6) 0.0179(6) 0.0185(6) -0.0039(4) -0.0053(5) -0.0038(5) N2 0.0299(7) 0.0199(6) 0.0208(6) -0.0023(5) -0.0049(5) -0.0079(5) C1 0.0181(6) 0.0171(7) 0.0213(6) -0.0061(5) -0.0036(5) -0.0004(5) C2 0.0259(7) 0.0148(7) 0.0302(8) -0.0060(6) 0.0008(6) -0.0039(5) C3 0.0286(8) 0.0234(8) 0.0299(8) -0.0093(6) -0.0027(6) 0.0040(6) C4 0.0716(14) 0.0222(8) 0.0289(9) 0.0018(7) 0.0017(9) 0.0014(8) C5 0.0359(8) 0.0245(8) 0.0172(7) -0.0062(6) 0.0006(6) 0.0035(6) C6 0.0296(8) 0.0543(12) 0.0227(8) -0.0060(7) 0.0006(6) -0.0067(8) C7 0.0601(12) 0.0424(11) 0.0239(8) -0.0148(7) 0.0009(8) -0.0181(9) C8 0.0212(7) 0.0175(7) 0.0301(8) -0.0094(6) -0.0049(6) -0.0009(5) C9 0.0204(7) 0.0208(7) 0.0357(8) -0.0114(6) -0.0016(6) -0.0011(6) C10 0.0205(7) 0.0268(8) 0.0469(10) -0.0165(7) -0.0035(7) -0.0033(6) C11 0.0265(8) 0.0287(8) 0.0482(10) -0.0194(7) -0.0164(7) 0.0023(6) C12 0.0378(9) 0.0269(8) 0.0303(8) -0.0099(6) -0.0128(7) 0.0011(7) C13 0.0327(8) 0.0206(7) 0.0292(8) -0.0065(6) -0.0093(6) -0.0033(6) C14 0.0275(8) 0.0239(8) 0.0380(9) -0.0100(7) 0.0087(7) -0.0081(6) C15 0.0633(13) 0.0373(10) 0.0410(10) -0.0119(8) 0.0228(10) -0.0258(10) S3 0.02840(19) 0.02001(18) 0.02554(18) -0.01034(14) -0.01259(14) 0.00370(14) S4 0.0324(2) 0.01999(18) 0.02084(17) -0.00795(13) -0.01036(14) 0.00508(14) P2 0.01807(16) 0.01621(17) 0.01490(16) -0.00427(12) -0.00331(12) -0.00066(13) O5 0.0238(5) 0.0193(5) 0.0183(5) -0.0030(4) 0.0008(4) -0.0025(4) O6 0.0195(5) 0.0181(5) 0.0182(5) -0.0019(4) -0.0042(4) -0.0021(4) O7 0.0269(5) 0.0201(5) 0.0289(6) -0.0091(4) -0.0027(4) 0.0026(4) O8 0.0270(6) 0.0278(6) 0.0322(6) -0.0127(5) -0.0086(5) 0.0040(5) N3 0.0194(6) 0.0193(6) 0.0178(5) -0.0056(4) -0.0019(4) -0.0015(4) N4 0.0187(6) 0.0220(6) 0.0207(6) -0.0066(5) -0.0034(4) 0.0011(5) C16 0.0203(6) 0.0161(6) 0.0192(6) -0.0046(5) -0.0027(5) -0.0038(5) C17 0.0464(11) 0.0282(10) 0.0312(9) -0.0053(7) 0.0194(8) -0.0047(7) C17A 0.0464(11) 0.0282(10) 0.0312(9) -0.0053(7) 0.0194(8) -0.0047(7) C18 0.0458(11) 0.0513(12) 0.0246(8) 0.0059(8) -0.0034(7) -0.0144(9) C20 0.0218(7) 0.0179(7) 0.0213(7) 0.0005(5) -0.0041(5) -0.0018(5) C21 0.0459(10) 0.0346(9) 0.0209(7) -0.0003(6) -0.0075(7) -0.0053(8) C22 0.0318(8) 0.0215(8) 0.0356(9) -0.0030(6) -0.0045(7) 0.0053(6) C23 0.0190(6) 0.0185(7) 0.0179(6) -0.0036(5) 0.0019(5) -0.0049(5) C24 0.0192(6) 0.0181(7) 0.0185(6) -0.0038(5) 0.0026(5) -0.0053(5) C25 0.0281(7) 0.0210(7) 0.0193(7) -0.0057(5) 0.0029(6) -0.0043(6) C26 0.0379(9) 0.0287(8) 0.0175(7) -0.0061(6) -0.0034(6) -0.0044(7) C27 0.0319(8) 0.0274(8) 0.0194(7) -0.0011(6) -0.0038(6) 0.0009(6) C28 0.0267(7) 0.0214(7) 0.0193(7) -0.0034(5) 0.0000(6) 0.0005(6) C29 0.0200(6) 0.0184(7) 0.0226(7) -0.0047(5) 0.0043(5) -0.0033(5) C30 0.0321(8) 0.0257(8) 0.0397(9) -0.0103(7) -0.0071(7) 0.0080(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 Co1 S2 2.2767(7) . ? Co1 S4 2.2803(7) . ? Co1 S3 2.3168(8) . ? Co1 S1 2.3294(7) . ? S1 P1 1.9959(7) . ? S2 C1 1.7482(15) . ? P1 O2 1.5722(11) . ? P1 O1 1.5743(11) . ? P1 N1 1.6108(13) . ? O1 C2 1.4778(17) . ? O2 C5 1.4715(18) . ? O3 C14 1.3395(19) . ? O3 C15 1.452(2) . ? O4 C14 1.214(2) . ? N1 C1 1.3076(19) . ? N2 C1 1.3607(19) . ? N2 C8 1.4049(19) . ? N2 H2 0.8600 . ? C2 C3 1.505(2) . ? C2 C4 1.516(2) . ? C2 H2A 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.505(2) . ? C5 C7 1.507(2) . ? C5 H5 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C13 1.396(2) . ? C8 C9 1.423(2) . ? C9 C10 1.400(2) . ? C9 C14 1.488(2) . ? C10 C11 1.380(3) . ? C10 H10 0.9300 . ? C11 C12 1.389(3) . ? C11 H11 0.9300 . ? C12 C13 1.385(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? S3 P2 1.9959(7) . ? S4 C16 1.7556(15) . ? P2 O5 1.5684(11) . ? P2 O6 1.5739(11) . ? P2 N3 1.6137(13) . ? O5 C17 1.4709(19) . ? O6 C20 1.4819(17) . ? O7 C29 1.3394(18) . ? O7 C30 1.4458(19) . ? O8 C29 1.2175(19) . ? N3 C16 1.3074(19) . ? N4 C16 1.3638(19) . ? N4 C23 1.4094(18) . ? N4 H4 0.8600 . ? C17 C18 1.497(3) . ? C17 C19A 1.659(5) . ? C17 H17A 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20 C21 1.507(2) . ? C20 C22 1.513(2) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.401(2) . ? C23 C24 1.417(2) . ? C24 C25 1.401(2) . ? C24 C29 1.487(2) . ? C25 C26 1.378(2) . ? C25 H25 0.9300 . ? C26 C27 1.392(2) . ? C26 H26 0.9300 . ? C27 C28 1.383(2) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? 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 S4 111.55(2) . . ? S2 Co1 S3 109.29(3) . . ? S4 Co1 S3 107.36(2) . . ? S2 Co1 S1 107.52(2) . . ? S4 Co1 S1 111.19(2) . . ? S3 Co1 S1 109.93(3) . . ? P1 S1 Co1 96.30(3) . . ? C1 S2 Co1 111.05(5) . . ? O2 P1 O1 102.65(6) . . ? O2 P1 N1 105.87(6) . . ? O1 P1 N1 106.32(6) . . ? O2 P1 S1 109.77(5) . . ? O1 P1 S1 113.77(5) . . ? N1 P1 S1 117.20(5) . . ? C2 O1 P1 123.42(9) . . ? C5 O2 P1 123.36(9) . . ? C14 O3 C15 114.45(15) . . ? C1 N1 P1 127.14(11) . . ? C1 N2 C8 131.67(13) . . ? C1 N2 H2 114.2 . . ? C8 N2 H2 114.2 . . ? N1 C1 N2 120.49(13) . . ? N1 C1 S2 128.85(11) . . ? N2 C1 S2 110.63(10) . . ? O1 C2 C3 106.19(12) . . ? O1 C2 C4 108.98(13) . . ? C3 C2 C4 112.26(14) . . ? O1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C4 C2 H2A 109.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C6 107.08(13) . . ? O2 C5 C7 106.97(14) . . ? C6 C5 C7 113.55(14) . . ? O2 C5 H5 109.7 . . ? C6 C5 H5 109.7 . . ? C7 C5 H5 109.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 N2 123.22(14) . . ? C13 C8 C9 119.41(14) . . ? N2 C8 C9 117.37(14) . . ? C10 C9 C8 118.83(15) . . ? C10 C9 C14 119.90(14) . . ? C8 C9 C14 121.23(14) . . ? C11 C10 C9 121.19(15) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.33(15) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 121.28(16) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 119.86(15) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? O4 C14 O3 120.99(16) . . ? O4 C14 C9 126.03(14) . . ? O3 C14 C9 112.93(15) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 S3 Co1 98.77(3) . . ? C16 S4 Co1 108.26(5) . . ? O5 P2 O6 103.08(6) . . ? O5 P2 N3 106.44(6) . . ? O6 P2 N3 105.82(6) . . ? O5 P2 S3 114.40(5) . . ? O6 P2 S3 108.53(5) . . ? N3 P2 S3 117.32(5) . . ? C17 O5 P2 123.52(10) . . ? C20 O6 P2 120.56(9) . . ? C29 O7 C30 115.75(13) . . ? C16 N3 P2 125.54(10) . . ? C16 N4 C23 129.09(12) . . ? C16 N4 H4 115.5 . . ? C23 N4 H4 115.5 . . ? N3 C16 N4 120.41(13) . . ? N3 C16 S4 127.76(11) . . ? N4 C16 S4 111.79(10) . . ? O5 C17 C18 106.38(15) . . ? O5 C17 C19A 101.62(19) . . ? C18 C17 C19A 109.84(19) . . ? O5 C17 H17A 112.8 . . ? C18 C17 H17A 112.8 . . ? C19A C17 H17A 112.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19A H19A 109.5 . . ? C17 C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17 C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? H19D C19B H19E 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O6 C20 C21 106.74(12) . . ? O6 C20 C22 107.31(12) . . ? C21 C20 C22 113.73(14) . . ? O6 C20 H20 109.6 . . ? C21 C20 H20 109.6 . . ? C22 C20 H20 109.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 N4 122.84(13) . . ? C28 C23 C24 119.05(13) . . ? N4 C23 C24 118.09(13) . . ? C25 C24 C23 119.05(13) . . ? C25 C24 C29 119.29(13) . . ? C23 C24 C29 121.66(13) . . ? C26 C25 C24 121.22(14) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.31(15) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 120.98(15) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C23 120.20(14) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? O8 C29 O7 122.33(14) . . ? O8 C29 C24 125.51(14) . . ? O7 C29 C24 112.13(13) . . ? O7 C30 H30A 109.5 . . ? O7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Co1 S1 P1 26.95(2) . . . . ? S4 Co1 S1 P1 -95.43(3) . . . . ? S3 Co1 S1 P1 145.82(2) . . . . ? S4 Co1 S2 C1 127.67(5) . . . . ? S3 Co1 S2 C1 -113.77(6) . . . . ? S1 Co1 S2 C1 5.52(5) . . . . ? Co1 S1 P1 O2 178.74(4) . . . . ? Co1 S1 P1 O1 64.37(5) . . . . ? Co1 S1 P1 N1 -60.50(6) . . . . ? O2 P1 O1 C2 -70.47(11) . . . . ? N1 P1 O1 C2 178.57(10) . . . . ? S1 P1 O1 C2 48.07(11) . . . . ? O1 P1 O2 C5 174.43(11) . . . . ? N1 P1 O2 C5 -74.27(12) . . . . ? S1 P1 O2 C5 53.12(12) . . . . ? O2 P1 N1 C1 -176.81(12) . . . . ? O1 P1 N1 C1 -68.11(14) . . . . ? S1 P1 N1 C1 60.40(14) . . . . ? P1 N1 C1 N2 171.99(11) . . . . ? P1 N1 C1 S2 -5.9(2) . . . . ? C8 N2 C1 N1 -4.4(2) . . . . ? C8 N2 C1 S2 173.83(13) . . . . ? Co1 S2 C1 N1 -24.27(15) . . . . ? Co1 S2 C1 N2 157.67(9) . . . . ? P1 O1 C2 C3 -150.64(10) . . . . ? P1 O1 C2 C4 88.23(15) . . . . ? P1 O2 C5 C6 -108.55(13) . . . . ? P1 O2 C5 C7 129.40(12) . . . . ? C1 N2 C8 C13 11.3(3) . . . . ? C1 N2 C8 C9 -169.48(15) . . . . ? C13 C8 C9 C10 -3.2(2) . . . . ? N2 C8 C9 C10 177.53(14) . . . . ? C13 C8 C9 C14 174.39(14) . . . . ? N2 C8 C9 C14 -4.9(2) . . . . ? C8 C9 C10 C11 1.1(2) . . . . ? C14 C9 C10 C11 -176.57(15) . . . . ? C9 C10 C11 C12 1.7(2) . . . . ? C10 C11 C12 C13 -2.4(2) . . . . ? C11 C12 C13 C8 0.2(2) . . . . ? N2 C8 C13 C12 -178.18(15) . . . . ? C9 C8 C13 C12 2.6(2) . . . . ? C15 O3 C14 O4 -2.9(2) . . . . ? C15 O3 C14 C9 174.67(15) . . . . ? C10 C9 C14 O4 -179.49(17) . . . . ? C8 C9 C14 O4 2.9(3) . . . . ? C10 C9 C14 O3 3.0(2) . . . . ? C8 C9 C14 O3 -174.54(14) . . . . ? S2 Co1 S3 P2 -130.77(2) . . . . ? S4 Co1 S3 P2 -9.63(2) . . . . ? S1 Co1 S3 P2 111.45(3) . . . . ? S2 Co1 S4 C16 93.20(6) . . . . ? S3 Co1 S4 C16 -26.50(5) . . . . ? S1 Co1 S4 C16 -146.79(5) . . . . ? Co1 S3 P2 O5 -73.14(5) . . . . ? Co1 S3 P2 O6 172.40(4) . . . . ? Co1 S3 P2 N3 52.60(6) . . . . ? O6 P2 O5 C17 84.60(13) . . . . ? N3 P2 O5 C17 -164.27(13) . . . . ? S3 P2 O5 C17 -33.02(14) . . . . ? O5 P2 O6 C20 -175.94(10) . . . . ? N3 P2 O6 C20 72.47(11) . . . . ? S3 P2 O6 C20 -54.27(10) . . . . ? O5 P2 N3 C16 65.12(13) . . . . ? O6 P2 N3 C16 174.32(12) . . . . ? S3 P2 N3 C16 -64.47(13) . . . . ? P2 N3 C16 N4 -170.28(10) . . . . ? P2 N3 C16 S4 7.6(2) . . . . ? C23 N4 C16 N3 20.7(2) . . . . ? C23 N4 C16 S4 -157.42(12) . . . . ? Co1 S4 C16 N3 36.55(14) . . . . ? Co1 S4 C16 N4 -145.46(9) . . . . ? P2 O5 C17 C18 141.11(13) . . . . ? P2 O5 C17 C19A -103.95(19) . . . . ? P2 O6 C20 C21 -129.72(12) . . . . ? P2 O6 C20 C22 108.01(12) . . . . ? C16 N4 C23 C28 -25.9(2) . . . . ? C16 N4 C23 C24 152.70(14) . . . . ? C28 C23 C24 C25 4.8(2) . . . . ? N4 C23 C24 C25 -173.82(13) . . . . ? C28 C23 C24 C29 -175.22(13) . . . . ? N4 C23 C24 C29 6.14(19) . . . . ? C23 C24 C25 C26 -2.1(2) . . . . ? C29 C24 C25 C26 177.88(14) . . . . ? C24 C25 C26 C27 -1.5(2) . . . . ? C25 C26 C27 C28 2.5(2) . . . . ? C26 C27 C28 C23 0.2(2) . . . . ? N4 C23 C28 C27 174.69(14) . . . . ? C24 C23 C28 C27 -3.9(2) . . . . ? C30 O7 C29 O8 -0.3(2) . . . . ? C30 O7 C29 C24 -178.61(12) . . . . ? C25 C24 C29 O8 -167.98(14) . . . . ? C23 C24 C29 O8 12.1(2) . . . . ? C25 C24 C29 O7 10.28(18) . . . . ? C23 C24 C29 O7 -169.69(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O4 0.86 1.91 2.6356(19) 141.5 . N4 H4 O8 0.86 2.03 2.6857(18) 132.9 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.759 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.065 # Attachment '[CoL2]173K.cif' data_CoL2-173K _database_code_depnum_ccdc_archive 'CCDC 893876' #TrackingRef '[CoL2]173K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 Co N4 O8 P2 S4' _chemical_formula_sum 'C30 H44 Co N4 O8 P2 S4' _chemical_formula_weight 837.80 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4743(8) _cell_length_b 11.3943(9) _cell_length_c 17.3391(14) _cell_angle_alpha 78.149(6) _cell_angle_beta 84.676(6) _cell_angle_gamma 85.234(6) _cell_volume 2012.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30814 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7980 _exptl_absorpt_correction_T_max 0.9141 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 33235 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7092 _reflns_number_gt 5643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^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 7092 _refine_ls_number_parameters 452 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 0.47423(4) 0.14473(4) 0.23472(3) 0.03237(15) Uani 1 1 d . . . P1 P 0.35832(8) 0.20806(7) 0.06337(5) 0.0300(2) Uani 1 1 d . . . P2 P 0.69313(8) 0.13233(7) 0.36031(5) 0.0302(2) Uani 1 1 d . . . S1 S 0.53253(8) 0.20934(8) 0.10051(5) 0.0371(2) Uani 1 1 d . . . S2 S 0.29814(9) 0.03658(9) 0.24504(5) 0.0427(2) Uani 1 1 d . . . S3 S 0.64084(9) 0.02347(8) 0.29394(6) 0.0431(2) Uani 1 1 d . . . S4 S 0.43444(9) 0.30271(8) 0.29752(5) 0.0425(2) Uani 1 1 d . . . N1 N 0.2920(3) 0.0826(2) 0.08275(17) 0.0352(6) Uani 1 1 d . . . N2 N 0.1929(3) -0.0813(3) 0.15979(19) 0.0409(7) Uani 1 1 d D . . H2 H 0.175(4) -0.120(3) 0.2077(11) 0.052(12) Uiso 1 1 d D . . N3 N 0.5827(3) 0.1856(2) 0.41687(16) 0.0329(6) Uani 1 1 d . . . N4 N 0.4076(3) 0.3114(3) 0.44697(17) 0.0349(6) Uani 1 1 d . . . H4 H 0.342(4) 0.362(3) 0.426(2) 0.033(9) Uiso 1 1 d . . . O1 O 0.2571(2) 0.30212(19) 0.09302(13) 0.0333(5) Uani 1 1 d . . . O2 O 0.3634(2) 0.2507(2) -0.02892(13) 0.0349(5) Uani 1 1 d . . . O4 O 0.0784(4) -0.2402(3) 0.2714(2) 0.0790(11) Uani 1 1 d . . . O3 O -0.0474(3) -0.3623(3) 0.2353(2) 0.0733(11) Uani 1 1 d . . . O5 O 0.7662(2) 0.2421(2) 0.31278(13) 0.0376(5) Uani 1 1 d . . . O6 O 0.7949(2) 0.0616(2) 0.41650(13) 0.0330(5) Uani 1 1 d . . . O8 O 0.2122(3) 0.4763(2) 0.45295(17) 0.0498(7) Uani 1 1 d . . . O7 O 0.2256(3) 0.5985(2) 0.53732(16) 0.0466(6) Uani 1 1 d . . . C1 C 0.2630(3) 0.0165(3) 0.1520(2) 0.0341(7) Uani 1 1 d . . . C2 C 0.2830(4) 0.4291(3) 0.0885(2) 0.0411(8) Uani 1 1 d . . . H2A H 0.3762 0.4356 0.0939 0.049 Uiso 1 1 calc R . . C3 C 0.2037(4) 0.4683(4) 0.1561(2) 0.0500(10) Uani 1 1 d . . . H3A H 0.2322 0.4208 0.2061 0.075 Uiso 1 1 calc R . . H3B H 0.1131 0.4563 0.1525 0.075 Uiso 1 1 calc R . . H3C H 0.2139 0.5536 0.1542 0.075 Uiso 1 1 calc R . . C4 C 0.2458(6) 0.5015(4) 0.0100(3) 0.0786(17) Uani 1 1 d . . . H4A H 0.3004 0.4740 -0.0327 0.118 Uiso 1 1 calc R . . H4B H 0.2572 0.5867 0.0078 0.118 Uiso 1 1 calc R . . H4C H 0.1556 0.4910 0.0038 0.118 Uiso 1 1 calc R . . C5 C 0.4539(4) 0.1962(4) -0.0841(2) 0.0467(9) Uani 1 1 d . . . H5 H 0.4982 0.1214 -0.0550 0.056 Uiso 1 1 calc R . . C6 C 0.5497(4) 0.2853(5) -0.1189(3) 0.0646(12) Uani 1 1 d . . . H6A H 0.5997 0.2999 -0.0771 0.097 Uiso 1 1 calc R . . H6B H 0.5052 0.3608 -0.1436 0.097 Uiso 1 1 calc R . . H6C H 0.6075 0.2540 -0.1588 0.097 Uiso 1 1 calc R . . C7 C 0.3747(6) 0.1657(5) -0.1447(3) 0.0754(15) Uani 1 1 d . . . H7A H 0.3146 0.1057 -0.1187 0.113 Uiso 1 1 calc R . . H7B H 0.4316 0.1331 -0.1845 0.113 Uiso 1 1 calc R . . H7C H 0.3266 0.2384 -0.1705 0.113 Uiso 1 1 calc R . . C8 C 0.1334(3) -0.1261(3) 0.1039(2) 0.0379(8) Uani 1 1 d . . . C9 C 0.0473(3) -0.2177(3) 0.1327(3) 0.0479(9) Uani 1 1 d . . . C10 C -0.0167(4) -0.2617(4) 0.0792(3) 0.0540(11) Uani 1 1 d . . . H10 H -0.0752 -0.3224 0.0983 0.065 Uiso 1 1 calc R . . C11 C 0.0029(4) -0.2193(4) -0.0007(3) 0.0592(12) Uani 1 1 d . . . H11 H -0.0441 -0.2483 -0.0365 0.071 Uiso 1 1 calc R . . C12 C 0.0917(4) -0.1337(4) -0.0290(3) 0.0567(11) Uani 1 1 d . . . H12 H 0.1083 -0.1075 -0.0844 0.068 Uiso 1 1 calc R . . C13 C 0.1566(4) -0.0860(3) 0.0221(3) 0.0485(9) Uani 1 1 d . . . H13 H 0.2163 -0.0267 0.0020 0.058 Uiso 1 1 calc R . . C14 C 0.0291(4) -0.2706(4) 0.2193(3) 0.0563(11) Uani 1 1 d . . . C15 C -0.0584(7) -0.4235(5) 0.3188(3) 0.091(2) Uani 1 1 d . . . H15C H 0.0266 -0.4569 0.3348 0.137 Uiso 1 1 calc R . . H15A H -0.1166 -0.4885 0.3257 0.137 Uiso 1 1 calc R . . H15B H -0.0924 -0.3657 0.3516 0.137 Uiso 1 1 calc R . . C16 C 0.4840(3) 0.2578(3) 0.39356(19) 0.0329(7) Uani 1 1 d . . . C17 C 0.8544(5) 0.2372(4) 0.2427(3) 0.0643(13) Uani 1 1 d . . . H17 H 0.8349 0.1686 0.2187 0.077 Uiso 1 1 calc R . . C19 C 0.9879(6) 0.2179(8) 0.2678(5) 0.161(5) Uani 1 1 d . . . H19A H 0.9976 0.1404 0.3044 0.242 Uiso 1 1 calc R . . H19B H 1.0053 0.2825 0.2942 0.242 Uiso 1 1 calc R . . H19C H 1.0488 0.2182 0.2213 0.242 Uiso 1 1 calc R . . C18 C 0.8312(5) 0.3533(5) 0.1852(3) 0.0742(14) Uani 1 1 d . . . H18A H 0.7425 0.3603 0.1702 0.111 Uiso 1 1 calc R . . H18B H 0.8906 0.3547 0.1379 0.111 Uiso 1 1 calc R . . H18C H 0.8454 0.4207 0.2098 0.111 Uiso 1 1 calc R . . C20 C 0.7684(3) -0.0552(3) 0.4688(2) 0.0377(8) Uani 1 1 d . . . H20 H 0.6759 -0.0704 0.4683 0.045 Uiso 1 1 calc R . . C22 C 0.8515(4) -0.1506(4) 0.4357(3) 0.0569(11) Uani 1 1 d . . . H22A H 0.8276 -0.1516 0.3825 0.085 Uiso 1 1 calc R . . H22B H 0.8388 -0.2293 0.4699 0.085 Uiso 1 1 calc R . . H22C H 0.9419 -0.1330 0.4331 0.085 Uiso 1 1 calc R . . C21 C 0.7954(5) -0.0461(4) 0.5504(2) 0.0620(12) Uani 1 1 d . . . H21A H 0.7376 0.0171 0.5679 0.093 Uiso 1 1 calc R . . H21B H 0.8847 -0.0264 0.5504 0.093 Uiso 1 1 calc R . . H21C H 0.7816 -0.1231 0.5865 0.093 Uiso 1 1 calc R . . C23 C 0.4346(3) 0.3303(3) 0.52087(19) 0.0330(7) Uani 1 1 d . . . C24 C 0.3682(3) 0.4284(3) 0.54927(19) 0.0331(7) Uani 1 1 d . . . C25 C 0.4023(4) 0.4549(3) 0.6195(2) 0.0408(8) Uani 1 1 d . . . H25 H 0.3587 0.5211 0.6384 0.049 Uiso 1 1 calc R . . C26 C 0.4973(4) 0.3878(3) 0.6621(2) 0.0471(9) Uani 1 1 d . . . H26 H 0.5222 0.4096 0.7083 0.057 Uiso 1 1 calc R . . C27 C 0.5560(4) 0.2874(4) 0.6359(2) 0.0482(9) Uani 1 1 d . . . H27 H 0.6179 0.2375 0.6665 0.058 Uiso 1 1 calc R . . C28 C 0.5260(3) 0.2591(3) 0.5666(2) 0.0395(8) Uani 1 1 d . . . H28 H 0.5678 0.1905 0.5496 0.047 Uiso 1 1 calc R . . C29 C 0.2626(3) 0.5012(3) 0.5071(2) 0.0372(8) Uani 1 1 d . . . C30 C 0.1220(4) 0.6744(4) 0.5000(3) 0.0592(11) Uani 1 1 d . . . H30C H 0.1472 0.7015 0.4437 0.089 Uiso 1 1 calc R . . H30A H 0.1034 0.7442 0.5251 0.089 Uiso 1 1 calc R . . H30B H 0.0452 0.6288 0.5060 0.089 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 0.0346(3) 0.0352(3) 0.0297(3) -0.01107(19) -0.00670(18) -0.00006(19) P1 0.0311(4) 0.0328(4) 0.0270(4) -0.0075(3) -0.0027(3) -0.0023(3) P2 0.0311(4) 0.0329(4) 0.0277(4) -0.0092(3) -0.0036(3) 0.0011(3) S1 0.0305(4) 0.0493(5) 0.0325(4) -0.0098(4) -0.0030(3) -0.0036(4) S2 0.0459(5) 0.0540(5) 0.0309(4) -0.0108(4) -0.0009(4) -0.0154(4) S3 0.0505(5) 0.0387(5) 0.0463(5) -0.0202(4) -0.0205(4) 0.0101(4) S4 0.0550(5) 0.0385(5) 0.0374(5) -0.0160(4) -0.0154(4) 0.0107(4) N1 0.0395(15) 0.0346(14) 0.0340(15) -0.0104(12) -0.0057(12) -0.0050(12) N2 0.0460(17) 0.0371(16) 0.0419(18) -0.0092(13) -0.0018(14) -0.0139(13) N3 0.0325(14) 0.0368(15) 0.0300(14) -0.0102(12) 0.0000(11) 0.0005(12) N4 0.0321(15) 0.0375(15) 0.0371(15) -0.0145(12) -0.0023(12) 0.0030(12) O1 0.0304(11) 0.0324(11) 0.0369(12) -0.0078(9) 0.0004(9) -0.0009(9) O2 0.0391(13) 0.0391(12) 0.0261(11) -0.0069(9) -0.0015(10) 0.0004(10) O4 0.111(3) 0.072(2) 0.059(2) -0.0154(17) 0.0146(19) -0.051(2) O3 0.069(2) 0.065(2) 0.092(3) -0.0377(19) 0.0383(18) -0.0356(16) O5 0.0407(13) 0.0391(12) 0.0310(12) -0.0064(10) 0.0046(10) -0.0003(10) O6 0.0282(11) 0.0347(12) 0.0359(12) -0.0069(9) -0.0046(9) 0.0014(9) O8 0.0433(14) 0.0511(15) 0.0606(17) -0.0256(13) -0.0115(13) 0.0093(12) O7 0.0479(15) 0.0397(13) 0.0543(16) -0.0182(12) -0.0021(12) 0.0057(11) C1 0.0327(17) 0.0347(17) 0.0370(18) -0.0121(14) -0.0044(14) 0.0003(14) C2 0.0417(19) 0.0330(17) 0.049(2) -0.0108(15) 0.0028(16) -0.0052(15) C3 0.050(2) 0.045(2) 0.056(2) -0.0195(18) -0.0028(18) 0.0106(17) C4 0.124(5) 0.041(2) 0.060(3) 0.002(2) 0.009(3) 0.010(3) C5 0.059(2) 0.048(2) 0.0317(18) -0.0145(16) 0.0024(17) 0.0100(18) C6 0.053(3) 0.098(4) 0.041(2) -0.011(2) 0.0048(19) -0.011(2) C7 0.113(4) 0.081(3) 0.044(2) -0.031(2) 0.002(3) -0.032(3) C8 0.0327(17) 0.0342(17) 0.050(2) -0.0162(15) -0.0066(15) 0.0028(14) C9 0.0339(18) 0.042(2) 0.074(3) -0.0279(19) 0.0007(18) -0.0024(15) C10 0.0352(19) 0.056(2) 0.080(3) -0.036(2) -0.0028(19) -0.0028(17) C11 0.042(2) 0.052(2) 0.097(4) -0.039(2) -0.029(2) 0.0045(19) C12 0.062(3) 0.053(2) 0.063(3) -0.028(2) -0.022(2) 0.010(2) C13 0.053(2) 0.040(2) 0.058(2) -0.0186(18) -0.0175(19) -0.0031(17) C14 0.053(2) 0.049(2) 0.070(3) -0.025(2) 0.023(2) -0.0201(19) C15 0.122(5) 0.075(3) 0.079(4) -0.030(3) 0.053(4) -0.055(3) C16 0.0361(17) 0.0334(16) 0.0309(17) -0.0098(13) -0.0035(13) -0.0024(14) C17 0.077(3) 0.054(2) 0.054(3) -0.012(2) 0.035(2) -0.003(2) C19 0.052(3) 0.186(8) 0.166(7) 0.101(6) 0.048(4) 0.051(4) C18 0.078(3) 0.095(4) 0.042(2) 0.010(2) -0.001(2) -0.024(3) C20 0.0361(18) 0.0365(18) 0.0389(19) -0.0041(14) -0.0027(14) -0.0007(14) C22 0.059(3) 0.039(2) 0.068(3) -0.0077(19) -0.004(2) 0.0142(19) C21 0.085(3) 0.062(3) 0.036(2) 0.0011(19) -0.011(2) -0.008(2) C23 0.0326(16) 0.0328(16) 0.0333(17) -0.0078(13) 0.0054(13) -0.0053(13) C24 0.0328(17) 0.0338(16) 0.0326(17) -0.0089(13) 0.0069(13) -0.0060(14) C25 0.045(2) 0.0430(19) 0.0351(18) -0.0130(15) 0.0085(16) -0.0055(16) C26 0.065(2) 0.048(2) 0.0299(18) -0.0112(16) -0.0018(17) -0.0033(19) C27 0.055(2) 0.054(2) 0.0333(19) -0.0034(16) -0.0059(17) 0.0010(18) C28 0.0443(19) 0.0386(18) 0.0333(18) -0.0073(14) 0.0024(15) 0.0037(15) C29 0.0331(17) 0.0352(17) 0.044(2) -0.0152(15) 0.0097(15) -0.0045(14) C30 0.055(2) 0.048(2) 0.077(3) -0.023(2) -0.012(2) 0.0174(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 Co1 S2 2.2756(10) . ? Co1 S4 2.2795(9) . ? Co1 S3 2.3147(10) . ? Co1 S1 2.3319(10) . ? P1 O1 1.573(2) . ? P1 O2 1.571(2) . ? P1 N1 1.601(3) . ? P1 S1 1.9926(12) . ? P2 O5 1.565(2) . ? P2 O6 1.569(2) . ? P2 N3 1.608(3) . ? P2 S3 1.9947(12) . ? S2 C1 1.752(3) . ? S4 C16 1.752(3) . ? N1 C1 1.304(4) . ? N2 C1 1.361(5) . ? N2 C8 1.399(5) . ? N2 H2 0.866(10) . ? N3 C16 1.307(4) . ? N4 C16 1.373(4) . ? N4 C23 1.400(4) . ? N4 H4 0.91(4) . ? O1 C2 1.479(4) . ? O2 C5 1.476(4) . ? O4 C14 1.202(6) . ? O3 C14 1.337(5) . ? O3 C15 1.471(7) . ? O5 C17 1.465(4) . ? O6 C20 1.480(4) . ? O8 C29 1.211(4) . ? O7 C29 1.335(4) . ? O7 C30 1.445(5) . ? C2 C3 1.497(5) . ? C2 C4 1.506(6) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.486(6) . ? C5 C7 1.507(6) . ? C5 H5 1.0000 . ? 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 C13 1.402(6) . ? C8 C9 1.419(5) . ? C9 C10 1.386(6) . ? C9 C14 1.500(6) . ? C10 C11 1.374(7) . ? C10 H10 0.9500 . ? C11 C12 1.388(6) . ? C11 H11 0.9500 . ? C12 C13 1.383(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C15 H15C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C17 C19 1.489(9) . ? C17 C18 1.502(7) . ? C17 H17 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 C21 1.493(6) . ? C20 C22 1.509(5) . ? C20 H20 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C28 1.396(5) . ? C23 C24 1.417(4) . ? C24 C25 1.397(5) . ? C24 C29 1.482(5) . ? C25 C26 1.378(6) . ? C25 H25 0.9500 . ? C26 C27 1.392(5) . ? C26 H26 0.9500 . ? C27 C28 1.377(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 H30C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 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 S2 Co1 S4 111.37(4) . . ? S2 Co1 S3 109.48(4) . . ? S4 Co1 S3 107.43(4) . . ? S2 Co1 S1 107.55(4) . . ? S4 Co1 S1 111.42(4) . . ? S3 Co1 S1 109.57(4) . . ? O1 P1 O2 102.56(12) . . ? O1 P1 N1 106.20(13) . . ? O2 P1 N1 106.06(14) . . ? O1 P1 S1 113.70(10) . . ? O2 P1 S1 109.80(10) . . ? N1 P1 S1 117.27(12) . . ? O5 P2 O6 103.22(13) . . ? O5 P2 N3 106.37(13) . . ? O6 P2 N3 105.74(13) . . ? O5 P2 S3 114.29(10) . . ? O6 P2 S3 108.62(9) . . ? N3 P2 S3 117.38(11) . . ? P1 S1 Co1 96.53(4) . . ? C1 S2 Co1 110.80(12) . . ? P2 S3 Co1 98.90(4) . . ? C16 S4 Co1 108.39(11) . . ? C1 N1 P1 127.8(2) . . ? C1 N2 C8 130.9(3) . . ? C1 N2 H2 116(3) . . ? C8 N2 H2 113(3) . . ? C16 N3 P2 125.9(2) . . ? C16 N4 C23 129.5(3) . . ? C16 N4 H4 115(2) . . ? C23 N4 H4 112(2) . . ? C2 O1 P1 123.3(2) . . ? C5 O2 P1 123.5(2) . . ? C14 O3 C15 114.5(4) . . ? C17 O5 P2 123.7(2) . . ? C20 O6 P2 121.4(2) . . ? C29 O7 C30 115.4(3) . . ? N1 C1 N2 121.2(3) . . ? N1 C1 S2 128.6(3) . . ? N2 C1 S2 110.2(3) . . ? O1 C2 C3 106.2(3) . . ? O1 C2 C4 108.8(3) . . ? C3 C2 C4 111.8(3) . . ? O1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? C4 C2 H2A 110.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C6 107.5(3) . . ? O2 C5 C7 106.6(3) . . ? C6 C5 C7 113.1(4) . . ? O2 C5 H5 109.8 . . ? C6 C5 H5 109.8 . . ? C7 C5 H5 109.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C13 123.2(3) . . ? N2 C8 C9 117.3(3) . . ? C13 C8 C9 119.5(3) . . ? C10 C9 C8 119.0(4) . . ? C10 C9 C14 119.9(4) . . ? C8 C9 C14 121.0(4) . . ? C11 C10 C9 121.3(4) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 119.3(4) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? O4 C14 O3 120.7(4) . . ? O4 C14 C9 126.3(4) . . ? O3 C14 C9 112.9(4) . . ? O3 C15 H15C 109.5 . . ? O3 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C16 N4 119.9(3) . . ? N3 C16 S4 127.9(2) . . ? N4 C16 S4 112.1(2) . . ? O5 C17 C19 108.2(5) . . ? O5 C17 C18 106.9(3) . . ? C19 C17 C18 113.2(5) . . ? O5 C17 H17 109.5 . . ? C19 C17 H17 109.5 . . ? C18 C17 H17 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C20 C21 107.2(3) . . ? O6 C20 C22 107.1(3) . . ? C21 C20 C22 114.3(4) . . ? O6 C20 H20 109.4 . . ? C21 C20 H20 109.4 . . ? C22 C20 H20 109.4 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C28 C23 N4 123.0(3) . . ? C28 C23 C24 118.8(3) . . ? N4 C23 C24 118.1(3) . . ? C25 C24 C23 118.7(3) . . ? C25 C24 C29 119.7(3) . . ? C23 C24 C29 121.5(3) . . ? C26 C25 C24 122.0(3) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C25 C26 C27 118.5(4) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 121.2(4) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 120.6(3) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? O8 C29 O7 122.9(3) . . ? O8 C29 C24 125.4(3) . . ? O7 C29 C24 111.7(3) . . ? O7 C30 H30C 109.5 . . ? O7 C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? O7 C30 H30B 109.5 . . ? H30C C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Co1 65.01(11) . . . . ? O2 P1 S1 Co1 179.24(9) . . . . ? N1 P1 S1 Co1 -59.67(12) . . . . ? S2 Co1 S1 P1 26.16(5) . . . . ? S4 Co1 S1 P1 -96.17(5) . . . . ? S3 Co1 S1 P1 145.09(4) . . . . ? S4 Co1 S2 C1 128.62(12) . . . . ? S3 Co1 S2 C1 -112.72(12) . . . . ? S1 Co1 S2 C1 6.26(13) . . . . ? O5 P2 S3 Co1 -73.27(11) . . . . ? O6 P2 S3 Co1 172.11(9) . . . . ? N3 P2 S3 Co1 52.31(13) . . . . ? S2 Co1 S3 P2 -131.08(5) . . . . ? S4 Co1 S3 P2 -10.00(6) . . . . ? S1 Co1 S3 P2 111.19(5) . . . . ? S2 Co1 S4 C16 94.27(13) . . . . ? S3 Co1 S4 C16 -25.62(13) . . . . ? S1 Co1 S4 C16 -145.63(12) . . . . ? O1 P1 N1 C1 -68.4(3) . . . . ? O2 P1 N1 C1 -177.0(3) . . . . ? S1 P1 N1 C1 60.0(3) . . . . ? O5 P2 N3 C16 65.4(3) . . . . ? O6 P2 N3 C16 174.7(3) . . . . ? S3 P2 N3 C16 -64.0(3) . . . . ? O2 P1 O1 C2 -71.1(3) . . . . ? N1 P1 O1 C2 177.8(3) . . . . ? S1 P1 O1 C2 47.4(3) . . . . ? O1 P1 O2 C5 174.8(3) . . . . ? N1 P1 O2 C5 -74.0(3) . . . . ? S1 P1 O2 C5 53.6(3) . . . . ? O6 P2 O5 C17 83.1(3) . . . . ? N3 P2 O5 C17 -165.9(3) . . . . ? S3 P2 O5 C17 -34.7(3) . . . . ? O5 P2 O6 C20 -175.6(2) . . . . ? N3 P2 O6 C20 72.8(2) . . . . ? S3 P2 O6 C20 -54.0(2) . . . . ? P1 N1 C1 N2 172.1(3) . . . . ? P1 N1 C1 S2 -5.6(5) . . . . ? C8 N2 C1 N1 -4.6(6) . . . . ? C8 N2 C1 S2 173.5(3) . . . . ? Co1 S2 C1 N1 -24.8(3) . . . . ? Co1 S2 C1 N2 157.2(2) . . . . ? P1 O1 C2 C3 -150.2(3) . . . . ? P1 O1 C2 C4 89.2(4) . . . . ? P1 O2 C5 C6 -109.6(3) . . . . ? P1 O2 C5 C7 128.8(3) . . . . ? C1 N2 C8 C13 12.3(6) . . . . ? C1 N2 C8 C9 -168.7(3) . . . . ? N2 C8 C9 C10 178.0(3) . . . . ? C13 C8 C9 C10 -3.0(5) . . . . ? N2 C8 C9 C14 -4.6(5) . . . . ? C13 C8 C9 C14 174.5(3) . . . . ? C8 C9 C10 C11 0.8(6) . . . . ? C14 C9 C10 C11 -176.7(4) . . . . ? C9 C10 C11 C12 2.3(6) . . . . ? C10 C11 C12 C13 -3.1(6) . . . . ? C11 C12 C13 C8 0.9(6) . . . . ? N2 C8 C13 C12 -178.8(3) . . . . ? C9 C8 C13 C12 2.2(5) . . . . ? C15 O3 C14 O4 -3.2(6) . . . . ? C15 O3 C14 C9 174.8(4) . . . . ? C10 C9 C14 O4 -179.6(4) . . . . ? C8 C9 C14 O4 2.9(7) . . . . ? C10 C9 C14 O3 2.5(5) . . . . ? C8 C9 C14 O3 -174.9(3) . . . . ? P2 N3 C16 N4 -170.0(2) . . . . ? P2 N3 C16 S4 7.9(5) . . . . ? C23 N4 C16 N3 20.2(5) . . . . ? C23 N4 C16 S4 -157.9(3) . . . . ? Co1 S4 C16 N3 35.7(3) . . . . ? Co1 S4 C16 N4 -146.4(2) . . . . ? P2 O5 C17 C19 -97.4(5) . . . . ? P2 O5 C17 C18 140.3(3) . . . . ? P2 O6 C20 C21 -128.0(3) . . . . ? P2 O6 C20 C22 108.9(3) . . . . ? C16 N4 C23 C28 -25.2(5) . . . . ? C16 N4 C23 C24 153.1(3) . . . . ? C28 C23 C24 C25 4.0(5) . . . . ? N4 C23 C24 C25 -174.3(3) . . . . ? C28 C23 C24 C29 -174.8(3) . . . . ? N4 C23 C24 C29 6.8(5) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? C29 C24 C25 C26 178.1(3) . . . . ? C24 C25 C26 C27 -3.2(6) . . . . ? C25 C26 C27 C28 3.8(6) . . . . ? C26 C27 C28 C23 -0.5(6) . . . . ? N4 C23 C28 C27 174.8(3) . . . . ? C24 C23 C28 C27 -3.4(5) . . . . ? C30 O7 C29 O8 -1.1(5) . . . . ? C30 O7 C29 C24 -179.5(3) . . . . ? C25 C24 C29 O8 -168.4(3) . . . . ? C23 C24 C29 O8 10.4(5) . . . . ? C25 C24 C29 O7 9.9(4) . . . . ? C23 C24 C29 O7 -171.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O4 0.866(10) 1.88(3) 2.636(4) 145(4) . N4 H4 O8 0.91(4) 1.89(4) 2.670(4) 142(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.588 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.092