# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d1339 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H50 Co N4 O3, C7 H7 O3 S, 2(C2 H6 O)' _chemical_formula_sum 'C55 H69 Co N4 O8 S' _chemical_formula_weight 1005.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.631(3) _cell_length_b 14.137(3) _cell_length_c 14.402(3) _cell_angle_alpha 98.858(5) _cell_angle_beta 95.100(5) _cell_angle_gamma 105.071(5) _cell_volume 2623.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used 5622 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.95 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6243 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 147(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Bruker Triumph' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45043 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11987 _reflns_number_gt 7600 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0560P)^2^+1.6178P] 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 11987 _refine_ls_number_parameters 651 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.67439(3) 0.32385(3) 0.43337(3) 0.02089(11) Uani 1 1 d . . . O1 O 0.69181(15) 0.46195(14) 0.44734(14) 0.0245(5) Uani 1 1 d . . . O2 O 0.76910(14) 0.33241(14) 0.34487(14) 0.0246(5) Uani 1 1 d . . . O3 O 0.57322(18) 0.22999(17) 0.68770(17) 0.0374(6) Uani 1 1 d . . . H3O H 0.573(3) 0.180(3) 0.729(3) 0.081(14) Uiso 1 1 d . . . N1 N 0.6741(2) 0.18263(19) 0.41840(19) 0.0237(6) Uani 1 1 d . . . H1B H 0.617(3) 0.136(3) 0.403(2) 0.040(10) Uiso 1 1 d . . . H1C H 0.710(3) 0.179(3) 0.371(3) 0.046(11) Uiso 1 1 d . . . N2 N 0.7902(2) 0.34537(19) 0.5332(2) 0.0251(6) Uani 1 1 d . . . H2B H 0.839(3) 0.392(3) 0.524(2) 0.034(10) Uiso 1 1 d . . . H2C H 0.777(2) 0.363(2) 0.590(2) 0.029(9) Uiso 1 1 d . . . N3 N 0.57678(18) 0.31626(17) 0.51929(16) 0.0218(5) Uani 1 1 d . . . N4 N 0.55881(17) 0.29408(16) 0.34179(17) 0.0208(5) Uani 1 1 d . . . C1 C 0.7332(2) 0.1655(2) 0.5027(2) 0.0303(7) Uani 1 1 d . . . H1A H 0.6905 0.1663 0.5557 0.036 Uiso 1 1 calc R . . C2 C 0.8272(2) 0.2548(2) 0.5298(2) 0.0305(7) Uani 1 1 d . . . H2A H 0.8696 0.2531 0.4767 0.037 Uiso 1 1 calc R . . C3 C 0.7616(2) 0.0685(2) 0.4902(2) 0.0272(7) Uani 1 1 d . . . C4 C 0.8183(3) 0.0427(2) 0.4206(2) 0.0405(9) Uani 1 1 d . . . H4A H 0.8378 0.0854 0.3766 0.049 Uiso 1 1 calc R . . C5 C 0.8469(3) -0.0448(3) 0.4143(3) 0.0554(11) Uani 1 1 d . . . H5A H 0.8851 -0.0626 0.3658 0.067 Uiso 1 1 calc R . . C6 C 0.8195(3) -0.1063(3) 0.4794(3) 0.0476(10) Uani 1 1 d . . . H6A H 0.8397 -0.1661 0.4762 0.057 Uiso 1 1 calc R . . C7 C 0.7635(3) -0.0808(3) 0.5480(3) 0.0421(9) Uani 1 1 d . . . H7A H 0.7446 -0.1231 0.5925 0.050 Uiso 1 1 calc R . . C8 C 0.7339(2) 0.0057(2) 0.5537(2) 0.0332(8) Uani 1 1 d . . . H8A H 0.6942 0.0222 0.6015 0.040 Uiso 1 1 calc R . . C9 C 0.8950(2) 0.2567(2) 0.6193(2) 0.0269(7) Uani 1 1 d . . . C10 C 0.9976(3) 0.2639(2) 0.6142(3) 0.0404(9) Uani 1 1 d . . . H10A H 1.0234 0.2662 0.5552 0.049 Uiso 1 1 calc R . . C11 C 1.0628(3) 0.2678(3) 0.6952(3) 0.0584(12) Uani 1 1 d . . . H11A H 1.1330 0.2719 0.6915 0.070 Uiso 1 1 calc R . . C12 C 1.0257(4) 0.2659(3) 0.7809(3) 0.0640(14) Uani 1 1 d . . . H12A H 1.0704 0.2697 0.8367 0.077 Uiso 1 1 calc R . . C13 C 0.9237(4) 0.2584(3) 0.7854(3) 0.0533(11) Uani 1 1 d . . . H13A H 0.8981 0.2565 0.8445 0.064 Uiso 1 1 calc R . . C14 C 0.8586(3) 0.2536(2) 0.7054(2) 0.0376(8) Uani 1 1 d . . . H14A H 0.7883 0.2482 0.7094 0.045 Uiso 1 1 calc R . . C15 C 0.7016(2) 0.5162(2) 0.5327(2) 0.0237(6) Uani 1 1 d . . . C16 C 0.7594(2) 0.6171(2) 0.5482(2) 0.0279(7) Uani 1 1 d . . . H16A H 0.7870 0.6446 0.4967 0.034 Uiso 1 1 calc R . . C17 C 0.7766(2) 0.6765(2) 0.6366(2) 0.0293(7) Uani 1 1 d . . . H17A H 0.8169 0.7439 0.6453 0.035 Uiso 1 1 calc R . . C18 C 0.7359(2) 0.6394(2) 0.7138(2) 0.0307(7) Uani 1 1 d . . . H18A H 0.7501 0.6803 0.7750 0.037 Uiso 1 1 calc R . . C19 C 0.6750(2) 0.5430(2) 0.6997(2) 0.0272(7) Uani 1 1 d . . . H19A H 0.6451 0.5184 0.7515 0.033 Uiso 1 1 calc R . . C20 C 0.6555(2) 0.4792(2) 0.6102(2) 0.0228(6) Uani 1 1 d . . . C21 C 0.5788(2) 0.3827(2) 0.5932(2) 0.0220(6) Uani 1 1 d . . . C22 C 0.5028(2) 0.3598(2) 0.6602(2) 0.0222(6) Uani 1 1 d . . . C23 C 0.5009(2) 0.2786(2) 0.7058(2) 0.0262(7) Uani 1 1 d . . . C24 C 0.4293(3) 0.2536(2) 0.7672(2) 0.0330(8) Uani 1 1 d . . . H24A H 0.4285 0.1996 0.7992 0.040 Uiso 1 1 calc R . . C25 C 0.3591(3) 0.3078(2) 0.7815(2) 0.0360(8) Uani 1 1 d . . . H25A H 0.3097 0.2900 0.8229 0.043 Uiso 1 1 calc R . . C26 C 0.3597(2) 0.3874(2) 0.7365(2) 0.0338(8) Uani 1 1 d . . . H26A H 0.3106 0.4236 0.7464 0.041 Uiso 1 1 calc R . . C27 C 0.4326(2) 0.4140(2) 0.6764(2) 0.0281(7) Uani 1 1 d . . . H27A H 0.4344 0.4696 0.6464 0.034 Uiso 1 1 calc R . . C28 C 0.4818(2) 0.2376(2) 0.4770(2) 0.0249(6) Uani 1 1 d . . . H28A H 0.4249 0.2415 0.5144 0.030 Uiso 1 1 calc R . . H28B H 0.4924 0.1706 0.4730 0.030 Uiso 1 1 calc R . . C29 C 0.4599(2) 0.2606(2) 0.3783(2) 0.0252(7) Uani 1 1 d . . . H29A H 0.4153 0.2003 0.3355 0.030 Uiso 1 1 calc R . . H29B H 0.4242 0.3135 0.3818 0.030 Uiso 1 1 calc R . . C30 C 0.5622(2) 0.3116(2) 0.2571(2) 0.0234(6) Uani 1 1 d . . . H30A H 0.4986 0.2986 0.2179 0.028 Uiso 1 1 calc R . . C31 C 0.6540(2) 0.3494(2) 0.2161(2) 0.0223(6) Uani 1 1 d . . . C32 C 0.6407(2) 0.3771(2) 0.1271(2) 0.0246(6) Uani 1 1 d . . . H32A H 0.5732 0.3706 0.0984 0.030 Uiso 1 1 calc R . . C33 C 0.7220(2) 0.4131(2) 0.0805(2) 0.0264(7) Uani 1 1 d . . . C34 C 0.8199(2) 0.4164(2) 0.1247(2) 0.0284(7) Uani 1 1 d . . . H34A H 0.8771 0.4390 0.0927 0.034 Uiso 1 1 calc R . . C35 C 0.8383(2) 0.3890(2) 0.2117(2) 0.0252(7) Uani 1 1 d . . . C36 C 0.7530(2) 0.3571(2) 0.2608(2) 0.0222(6) Uani 1 1 d . . . C37 C 0.7123(2) 0.4480(2) -0.0152(2) 0.0325(7) Uani 1 1 d . . . C38 C 0.6031(3) 0.4494(4) -0.0445(3) 0.0621(13) Uani 1 1 d . . . H38A H 0.6001 0.4783 -0.1019 0.093 Uiso 1 1 calc R . . H38B H 0.5807 0.4895 0.0067 0.093 Uiso 1 1 calc R . . H38C H 0.5580 0.3811 -0.0573 0.093 Uiso 1 1 calc R . . C39 C 0.7456(3) 0.3799(3) -0.0914(2) 0.0481(10) Uani 1 1 d . . . H39A H 0.7413 0.4041 -0.1515 0.072 Uiso 1 1 calc R . . H39B H 0.7004 0.3120 -0.0996 0.072 Uiso 1 1 calc R . . H39C H 0.8164 0.3799 -0.0722 0.072 Uiso 1 1 calc R . . C40 C 0.7817(3) 0.5544(3) -0.0051(3) 0.0477(10) Uani 1 1 d . . . H40A H 0.7744 0.5776 -0.0654 0.072 Uiso 1 1 calc R . . H40B H 0.8532 0.5551 0.0117 0.072 Uiso 1 1 calc R . . H40C H 0.7619 0.5984 0.0447 0.072 Uiso 1 1 calc R . . C41 C 0.9469(2) 0.3904(2) 0.2525(2) 0.0311(7) Uani 1 1 d . . . C42 C 0.9800(3) 0.4593(3) 0.3503(3) 0.0466(10) Uani 1 1 d . . . H42A H 0.9801 0.5273 0.3439 0.070 Uiso 1 1 calc R . . H42B H 1.0490 0.4587 0.3754 0.070 Uiso 1 1 calc R . . H42C H 0.9318 0.4356 0.3939 0.070 Uiso 1 1 calc R . . C43 C 0.9488(2) 0.2843(2) 0.2612(2) 0.0339(8) Uani 1 1 d . . . H43A H 0.9328 0.2421 0.1981 0.051 Uiso 1 1 calc R . . H43B H 0.8978 0.2575 0.3012 0.051 Uiso 1 1 calc R . . H43C H 1.0171 0.2854 0.2899 0.051 Uiso 1 1 calc R . . C44 C 1.0275(3) 0.4286(3) 0.1889(3) 0.0582(12) Uani 1 1 d . . . H44A H 1.0096 0.3859 0.1260 0.087 Uiso 1 1 calc R . . H44B H 1.0950 0.4270 0.2172 0.087 Uiso 1 1 calc R . . H44C H 1.0293 0.4971 0.1830 0.087 Uiso 1 1 calc R . . S1 S 0.44501(6) 0.00407(6) 0.23268(6) 0.02776(18) Uani 1 1 d . . . O4 O 0.48577(16) 0.03024(16) 0.33306(15) 0.0354(5) Uani 1 1 d . . . O5 O 0.36902(17) 0.05434(17) 0.20648(17) 0.0419(6) Uani 1 1 d . . . O6 O 0.40812(17) -0.10399(15) 0.20070(15) 0.0347(5) Uani 1 1 d . . . C45 C 0.5493(2) 0.0463(2) 0.1703(2) 0.0274(7) Uani 1 1 d . . . C46 C 0.6426(2) 0.0295(2) 0.1958(2) 0.0322(7) Uani 1 1 d . . . H46A H 0.6513 -0.0029 0.2478 0.039 Uiso 1 1 calc R . . C47 C 0.7233(3) 0.0600(2) 0.1455(2) 0.0383(8) Uani 1 1 d . . . H47A H 0.7875 0.0488 0.1638 0.046 Uiso 1 1 calc R . . C48 C 0.7120(3) 0.1071(2) 0.0679(2) 0.0385(8) Uani 1 1 d . . . C49 C 0.6181(3) 0.1237(2) 0.0440(2) 0.0386(8) Uani 1 1 d . . . H49A H 0.6089 0.1560 -0.0079 0.046 Uiso 1 1 calc R . . C50 C 0.5374(3) 0.0940(2) 0.0944(2) 0.0334(8) Uani 1 1 d . . . H50A H 0.4736 0.1062 0.0770 0.040 Uiso 1 1 calc R . . C51 C 0.7985(3) 0.1382(3) 0.0106(3) 0.0562(11) Uani 1 1 d . . . H51A H 0.7735 0.1136 -0.0570 0.084 Uiso 1 1 calc R . . H51B H 0.8542 0.1102 0.0293 0.084 Uiso 1 1 calc R . . H51C H 0.8239 0.2111 0.0224 0.084 Uiso 1 1 calc R . . O1S O 0.1820(2) 0.0925(2) 0.2057(2) 0.0718(9) Uani 1 1 d . . . H1S H 0.2378 0.0782 0.2019 0.108 Uiso 1 1 calc R . . C1S C 0.0049(4) 0.0260(4) 0.2126(5) 0.113(2) Uani 1 1 d D . . H1S1 H -0.0502 -0.0362 0.2052 0.169 Uiso 1 1 calc R . . H1S2 H -0.0082 0.0623 0.1623 0.169 Uiso 1 1 calc R . . H1S3 H 0.0072 0.0672 0.2745 0.169 Uiso 1 1 calc R . . C2S C 0.1017(3) 0.0034(4) 0.2066(4) 0.0750(14) Uani 1 1 d D . . H2SA H 0.1186 -0.0266 0.2615 0.090 Uiso 1 1 calc R . . H2SB H 0.0963 -0.0457 0.1480 0.090 Uiso 1 1 calc R . . O2S O 0.1456(3) 0.1923(3) 0.0566(4) 0.1269(16) Uani 1 1 d . . . H2S H 0.1581 0.1713 0.1066 0.190 Uiso 1 1 calc R . . C3S C 0.3227(4) 0.2130(4) 0.0272(5) 0.099(2) Uani 1 1 d . . . H3SA H 0.3647 0.1769 -0.0073 0.149 Uiso 1 1 calc R . . H3SB H 0.3331 0.2094 0.0946 0.149 Uiso 1 1 calc R . . H3SC H 0.3427 0.2829 0.0197 0.149 Uiso 1 1 calc R . . C4S C 0.2122(5) 0.1669(4) -0.0115(4) 0.0969(19) Uani 1 1 d . . . H4SA H 0.1966 0.1907 -0.0708 0.116 Uiso 1 1 calc R . . H4SB H 0.1985 0.0936 -0.0269 0.116 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 0.0194(2) 0.0218(2) 0.0213(2) 0.00363(15) -0.00059(16) 0.00667(15) O1 0.0259(11) 0.0248(11) 0.0234(11) 0.0064(9) 0.0017(9) 0.0074(8) O2 0.0196(11) 0.0304(11) 0.0248(11) 0.0060(9) 0.0007(9) 0.0092(8) O3 0.0479(15) 0.0392(14) 0.0395(14) 0.0207(11) 0.0176(11) 0.0256(11) N1 0.0225(14) 0.0228(14) 0.0246(15) 0.0020(11) -0.0014(12) 0.0072(11) N2 0.0240(15) 0.0222(14) 0.0290(16) 0.0043(12) -0.0006(12) 0.0081(11) N3 0.0236(13) 0.0213(12) 0.0202(13) 0.0041(10) 0.0003(10) 0.0062(10) N4 0.0174(12) 0.0209(12) 0.0248(14) 0.0045(10) 0.0025(10) 0.0067(9) C1 0.0321(18) 0.0268(16) 0.0316(18) 0.0040(13) -0.0043(14) 0.0114(13) C2 0.0282(17) 0.0243(16) 0.0370(19) 0.0045(13) -0.0067(14) 0.0085(13) C3 0.0283(17) 0.0229(15) 0.0287(17) 0.0002(12) -0.0053(14) 0.0099(12) C4 0.058(2) 0.0321(19) 0.039(2) 0.0132(15) 0.0168(18) 0.0183(16) C5 0.068(3) 0.049(2) 0.062(3) 0.010(2) 0.028(2) 0.032(2) C6 0.054(2) 0.0304(19) 0.067(3) 0.0133(18) 0.009(2) 0.0235(17) C7 0.037(2) 0.0326(19) 0.057(2) 0.0212(17) 0.0042(18) 0.0017(15) C8 0.0270(18) 0.0332(18) 0.040(2) 0.0080(15) 0.0066(15) 0.0078(14) C9 0.0245(16) 0.0218(15) 0.0321(18) 0.0018(13) -0.0065(13) 0.0077(12) C10 0.0300(19) 0.039(2) 0.049(2) 0.0015(16) -0.0007(17) 0.0098(15) C11 0.031(2) 0.055(3) 0.082(3) -0.012(2) -0.021(2) 0.0216(18) C12 0.081(3) 0.051(3) 0.053(3) -0.017(2) -0.043(3) 0.038(2) C13 0.081(3) 0.050(2) 0.034(2) -0.0002(17) -0.005(2) 0.037(2) C14 0.040(2) 0.0372(19) 0.037(2) 0.0022(15) 0.0007(16) 0.0177(15) C15 0.0197(15) 0.0243(15) 0.0292(17) 0.0069(12) -0.0029(13) 0.0105(12) C16 0.0229(16) 0.0258(16) 0.0374(19) 0.0113(14) 0.0027(14) 0.0080(12) C17 0.0206(16) 0.0204(15) 0.044(2) 0.0037(14) -0.0044(14) 0.0057(12) C18 0.0281(17) 0.0268(17) 0.0334(19) -0.0013(13) -0.0100(14) 0.0099(13) C19 0.0296(17) 0.0270(16) 0.0262(17) 0.0048(13) -0.0004(13) 0.0114(13) C20 0.0228(15) 0.0203(14) 0.0252(16) 0.0050(12) -0.0017(12) 0.0074(11) C21 0.0234(15) 0.0213(15) 0.0236(16) 0.0075(12) 0.0009(12) 0.0094(11) C22 0.0244(16) 0.0223(15) 0.0190(15) 0.0014(11) 0.0006(12) 0.0070(11) C23 0.0291(17) 0.0250(16) 0.0257(17) 0.0040(12) 0.0029(13) 0.0102(12) C24 0.039(2) 0.0289(17) 0.0321(19) 0.0106(14) 0.0110(15) 0.0066(14) C25 0.0336(19) 0.0350(19) 0.037(2) 0.0024(15) 0.0132(15) 0.0043(14) C26 0.0270(18) 0.0331(18) 0.039(2) -0.0038(15) 0.0035(15) 0.0107(14) C27 0.0306(17) 0.0280(16) 0.0251(17) 0.0039(13) 0.0010(13) 0.0088(13) C28 0.0239(16) 0.0234(15) 0.0245(16) 0.0005(12) 0.0010(13) 0.0044(12) C29 0.0165(15) 0.0339(17) 0.0248(16) 0.0042(13) 0.0020(12) 0.0074(12) C30 0.0203(15) 0.0262(15) 0.0230(16) 0.0028(12) -0.0013(12) 0.0076(12) C31 0.0190(15) 0.0271(15) 0.0201(15) 0.0002(12) -0.0004(12) 0.0084(11) C32 0.0211(15) 0.0297(16) 0.0226(16) 0.0014(12) 0.0007(12) 0.0087(12) C33 0.0284(17) 0.0303(17) 0.0223(16) 0.0048(12) 0.0032(13) 0.0116(13) C34 0.0243(16) 0.0310(17) 0.0332(18) 0.0087(14) 0.0111(14) 0.0097(13) C35 0.0188(15) 0.0243(15) 0.0332(18) 0.0061(13) 0.0023(13) 0.0071(12) C36 0.0223(15) 0.0206(15) 0.0236(16) 0.0016(12) 0.0014(12) 0.0079(11) C37 0.0344(19) 0.0421(19) 0.0255(18) 0.0106(14) 0.0090(14) 0.0142(15) C38 0.041(2) 0.124(4) 0.035(2) 0.042(2) 0.0086(18) 0.031(2) C39 0.070(3) 0.049(2) 0.029(2) 0.0052(16) 0.0163(19) 0.0211(19) C40 0.066(3) 0.048(2) 0.036(2) 0.0178(17) 0.0092(19) 0.0215(19) C41 0.0176(16) 0.0324(17) 0.045(2) 0.0150(15) 0.0027(14) 0.0061(13) C42 0.0281(19) 0.034(2) 0.069(3) 0.0027(18) -0.0148(18) 0.0035(14) C43 0.0243(17) 0.0349(18) 0.045(2) 0.0114(15) 0.0030(15) 0.0117(13) C44 0.0217(19) 0.078(3) 0.088(3) 0.051(3) 0.017(2) 0.0143(18) S1 0.0265(4) 0.0268(4) 0.0282(4) 0.0042(3) 0.0006(3) 0.0059(3) O4 0.0333(13) 0.0401(13) 0.0260(12) -0.0002(10) 0.0032(10) 0.0020(10) O5 0.0310(13) 0.0448(14) 0.0557(16) 0.0151(12) 0.0046(12) 0.0178(11) O6 0.0422(14) 0.0268(12) 0.0300(13) 0.0080(9) -0.0042(10) 0.0022(10) C45 0.0311(18) 0.0219(15) 0.0268(17) -0.0014(12) 0.0031(14) 0.0067(12) C46 0.0351(19) 0.0299(17) 0.0321(19) 0.0054(14) 0.0037(15) 0.0103(14) C47 0.0327(19) 0.038(2) 0.042(2) -0.0007(16) 0.0049(16) 0.0106(15) C48 0.043(2) 0.0329(19) 0.032(2) -0.0047(15) 0.0097(16) 0.0016(15) C49 0.055(2) 0.0304(18) 0.0266(19) 0.0055(14) 0.0060(16) 0.0049(16) C50 0.0378(19) 0.0282(17) 0.0341(19) 0.0051(14) 0.0012(15) 0.0103(14) C51 0.060(3) 0.052(2) 0.049(3) 0.0016(19) 0.023(2) 0.0005(19) O1S 0.0535(19) 0.064(2) 0.104(3) 0.0214(18) 0.0159(18) 0.0206(15) C1S 0.069(4) 0.099(5) 0.183(7) 0.041(4) 0.040(4) 0.030(3) C2S 0.053(3) 0.066(3) 0.097(4) 0.000(3) 0.002(3) 0.011(2) O2S 0.106(3) 0.112(4) 0.162(5) 0.047(3) -0.014(3) 0.027(3) C3S 0.060(3) 0.095(4) 0.166(6) 0.061(4) 0.012(4) 0.041(3) C4S 0.146(6) 0.080(4) 0.074(4) 0.010(3) 0.033(4) 0.043(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 1.874(2) . ? Co1 O1 1.881(2) . ? Co1 O2 1.888(2) . ? Co1 N3 1.890(2) . ? Co1 N2 1.966(3) . ? Co1 N1 1.974(3) . ? O1 C15 1.321(3) . ? O2 C36 1.326(3) . ? O3 C23 1.362(4) . ? O3 H3O 0.99(5) . ? N1 C1 1.483(4) . ? N1 H1B 0.87(4) . ? N1 H1C 0.88(4) . ? N2 C2 1.490(4) . ? N2 H2B 0.85(3) . ? N2 H2C 0.87(3) . ? N3 C21 1.300(4) . ? N3 C28 1.478(3) . ? N4 C30 1.284(4) . ? N4 C29 1.480(3) . ? C1 C3 1.509(4) . ? C1 C2 1.519(4) . ? C1 H1A 1.0000 . ? C2 C9 1.510(4) . ? C2 H2A 1.0000 . ? C3 C8 1.380(4) . ? C3 C4 1.382(5) . ? C4 C5 1.383(5) . ? C4 H4A 0.9500 . ? C5 C6 1.385(5) . ? C5 H5A 0.9500 . ? C6 C7 1.363(5) . ? C6 H6A 0.9500 . ? C7 C8 1.377(5) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C14 1.378(5) . ? C9 C10 1.385(4) . ? C10 C11 1.387(5) . ? C10 H10A 0.9500 . ? C11 C12 1.377(6) . ? C11 H11A 0.9500 . ? C12 C13 1.374(6) . ? C12 H12A 0.9500 . ? C13 C14 1.372(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.411(4) . ? C15 C20 1.431(4) . ? C16 C17 1.377(4) . ? C16 H16A 0.9500 . ? C17 C18 1.399(4) . ? C17 H17A 0.9500 . ? C18 C19 1.373(4) . ? C18 H18A 0.9500 . ? C19 C20 1.415(4) . ? C19 H19A 0.9500 . ? C20 C21 1.457(4) . ? C21 C22 1.487(4) . ? C22 C27 1.385(4) . ? C22 C23 1.404(4) . ? C23 C24 1.388(4) . ? C24 C25 1.382(5) . ? C24 H24A 0.9500 . ? C25 C26 1.381(5) . ? C25 H25A 0.9500 . ? C26 C27 1.392(4) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.527(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.442(4) . ? C30 H30A 0.9500 . ? C31 C32 1.406(4) . ? C31 C36 1.413(4) . ? C32 C33 1.372(4) . ? C32 H32A 0.9500 . ? C33 C34 1.413(4) . ? C33 C37 1.541(4) . ? C34 C35 1.387(4) . ? C34 H34A 0.9500 . ? C35 C36 1.423(4) . ? C35 C41 1.537(4) . ? C37 C38 1.515(5) . ? C37 C39 1.526(5) . ? C37 C40 1.531(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.531(4) . ? C41 C44 1.536(5) . ? C41 C42 1.541(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? S1 O5 1.455(2) . ? S1 O4 1.456(2) . ? S1 O6 1.463(2) . ? S1 C45 1.771(3) . ? C45 C46 1.381(4) . ? C45 C50 1.389(4) . ? C46 C47 1.383(5) . ? C46 H46A 0.9500 . ? C47 C48 1.404(5) . ? C47 H47A 0.9500 . ? C48 C49 1.383(5) . ? C48 C51 1.510(5) . ? C49 C50 1.381(5) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O1S C2S 1.441(5) . ? O1S H1S 0.8400 . ? C1S C2S 1.443(4) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? O2S C4S 1.461(7) . ? O2S H2S 0.8400 . ? C3S C4S 1.494(7) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 O1 92.76(9) . . ? N4 Co1 O2 94.83(10) . . ? O1 Co1 O2 89.89(9) . . ? N4 Co1 N3 83.59(10) . . ? O1 Co1 N3 89.44(9) . . ? O2 Co1 N3 178.26(10) . . ? N4 Co1 N2 175.40(11) . . ? O1 Co1 N2 90.96(10) . . ? O2 Co1 N2 87.86(11) . . ? N3 Co1 N2 93.76(12) . . ? N4 Co1 N1 92.13(10) . . ? O1 Co1 N1 173.10(11) . . ? O2 Co1 N1 84.84(11) . . ? N3 Co1 N1 95.95(11) . . ? N2 Co1 N1 84.39(11) . . ? C15 O1 Co1 119.95(17) . . ? C36 O2 Co1 123.96(18) . . ? C23 O3 H3O 111(3) . . ? C1 N1 Co1 110.32(18) . . ? C1 N1 H1B 110(2) . . ? Co1 N1 H1B 120(2) . . ? C1 N1 H1C 108(2) . . ? Co1 N1 H1C 100(2) . . ? H1B N1 H1C 109(3) . . ? C2 N2 Co1 111.02(19) . . ? C2 N2 H2B 108(2) . . ? Co1 N2 H2B 109(2) . . ? C2 N2 H2C 109(2) . . ? Co1 N2 H2C 114(2) . . ? H2B N2 H2C 107(3) . . ? C21 N3 C28 121.7(2) . . ? C21 N3 Co1 126.7(2) . . ? C28 N3 Co1 109.66(18) . . ? C30 N4 C29 121.3(2) . . ? C30 N4 Co1 123.9(2) . . ? C29 N4 Co1 114.30(18) . . ? N1 C1 C3 115.3(3) . . ? N1 C1 C2 106.2(2) . . ? C3 C1 C2 111.8(3) . . ? N1 C1 H1A 107.8 . . ? C3 C1 H1A 107.8 . . ? C2 C1 H1A 107.8 . . ? N2 C2 C9 112.8(2) . . ? N2 C2 C1 106.8(2) . . ? C9 C2 C1 115.2(3) . . ? N2 C2 H2A 107.2 . . ? C9 C2 H2A 107.2 . . ? C1 C2 H2A 107.2 . . ? C8 C3 C4 119.0(3) . . ? C8 C3 C1 118.5(3) . . ? C4 C3 C1 122.5(3) . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 119.6(4) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C7 C6 C5 119.7(3) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C7 C8 C3 120.2(3) . . ? C7 C8 H8A 119.9 . . ? C3 C8 H8A 119.9 . . ? C14 C9 C10 119.4(3) . . ? C14 C9 C2 122.3(3) . . ? C10 C9 C2 118.3(3) . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C9 120.3(3) . . ? C13 C14 H14A 119.9 . . ? C9 C14 H14A 119.9 . . ? O1 C15 C16 118.2(3) . . ? O1 C15 C20 123.8(3) . . ? C16 C15 C20 117.9(3) . . ? C17 C16 C15 121.1(3) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C16 C17 C18 121.1(3) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 119.0(3) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C18 C19 C20 121.8(3) . . ? C18 C19 H19A 119.1 . . ? C20 C19 H19A 119.1 . . ? C19 C20 C15 118.9(3) . . ? C19 C20 C21 120.7(3) . . ? C15 C20 C21 119.8(3) . . ? N3 C21 C20 120.0(3) . . ? N3 C21 C22 119.8(2) . . ? C20 C21 C22 120.2(2) . . ? C27 C22 C23 119.6(3) . . ? C27 C22 C21 122.1(3) . . ? C23 C22 C21 118.2(3) . . ? O3 C23 C24 123.9(3) . . ? O3 C23 C22 116.3(3) . . ? C24 C23 C22 119.8(3) . . ? C25 C24 C23 119.7(3) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C25 C26 C27 119.5(3) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C22 C27 C26 120.3(3) . . ? C22 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? N3 C28 C29 103.4(2) . . ? N3 C28 H28A 111.1 . . ? C29 C28 H28A 111.1 . . ? N3 C28 H28B 111.1 . . ? C29 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? N4 C29 C28 108.3(2) . . ? N4 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? N4 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? N4 C30 C31 125.9(3) . . ? N4 C30 H30A 117.1 . . ? C31 C30 H30A 117.1 . . ? C32 C31 C36 120.6(3) . . ? C32 C31 C30 116.7(3) . . ? C36 C31 C30 122.7(3) . . ? C33 C32 C31 122.1(3) . . ? C33 C32 H32A 118.9 . . ? C31 C32 H32A 118.9 . . ? C32 C33 C34 116.2(3) . . ? C32 C33 C37 124.3(3) . . ? C34 C33 C37 119.4(3) . . ? C35 C34 C33 124.6(3) . . ? C35 C34 H34A 117.7 . . ? C33 C34 H34A 117.7 . . ? C34 C35 C36 117.9(3) . . ? C34 C35 C41 121.1(3) . . ? C36 C35 C41 121.0(3) . . ? O2 C36 C31 122.6(3) . . ? O2 C36 C35 118.9(3) . . ? C31 C36 C35 118.4(3) . . ? C38 C37 C39 110.0(3) . . ? C38 C37 C40 107.9(3) . . ? C39 C37 C40 108.9(3) . . ? C38 C37 C33 110.8(3) . . ? C39 C37 C33 110.1(3) . . ? C40 C37 C33 109.1(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 107.4(3) . . ? C43 C41 C35 109.3(2) . . ? C44 C41 C35 112.4(3) . . ? C43 C41 C42 110.0(3) . . ? C44 C41 C42 107.0(3) . . ? C35 C41 C42 110.7(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 S1 O4 113.54(14) . . ? O5 S1 O6 112.28(14) . . ? O4 S1 O6 111.69(13) . . ? O5 S1 C45 106.09(15) . . ? O4 S1 C45 106.45(14) . . ? O6 S1 C45 106.15(14) . . ? C46 C45 C50 119.7(3) . . ? C46 C45 S1 119.8(2) . . ? C50 C45 S1 120.5(2) . . ? C45 C46 C47 119.9(3) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C46 C47 C48 121.0(3) . . ? C46 C47 H47A 119.5 . . ? C48 C47 H47A 119.5 . . ? C49 C48 C47 118.1(3) . . ? C49 C48 C51 120.3(3) . . ? C47 C48 C51 121.7(4) . . ? C50 C49 C48 121.1(3) . . ? C50 C49 H49A 119.4 . . ? C48 C49 H49A 119.4 . . ? C49 C50 C45 120.2(3) . . ? C49 C50 H50A 119.9 . . ? C45 C50 H50A 119.9 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C2S O1S H1S 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O1S C2S C1S 110.5(4) . . ? O1S C2S H2SA 109.5 . . ? C1S C2S H2SA 109.5 . . ? O1S C2S H2SB 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 108.1 . . ? C4S O2S H2S 109.5 . . ? C4S C3S H3SA 109.5 . . ? C4S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C4S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O2S C4S C3S 111.2(5) . . ? O2S C4S H4SA 109.4 . . ? C3S C4S H4SA 109.4 . . ? O2S C4S H4SB 109.4 . . ? C3S C4S H4SB 109.4 . . ? H4SA C4S H4SB 108.0 . . ? 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 N4 Co1 O1 C15 128.8(2) . . . . ? O2 Co1 O1 C15 -136.4(2) . . . . ? N3 Co1 O1 C15 45.3(2) . . . . ? N2 Co1 O1 C15 -48.5(2) . . . . ? N4 Co1 O2 C36 27.1(2) . . . . ? O1 Co1 O2 C36 -65.6(2) . . . . ? N2 Co1 O2 C36 -156.6(2) . . . . ? N1 Co1 O2 C36 118.9(2) . . . . ? N4 Co1 N1 C1 -160.1(2) . . . . ? O2 Co1 N1 C1 105.3(2) . . . . ? N3 Co1 N1 C1 -76.3(2) . . . . ? N2 Co1 N1 C1 16.9(2) . . . . ? O1 Co1 N2 C2 -163.3(2) . . . . ? O2 Co1 N2 C2 -73.5(2) . . . . ? N3 Co1 N2 C2 107.2(2) . . . . ? N1 Co1 N2 C2 11.6(2) . . . . ? N4 Co1 N3 C21 -128.3(2) . . . . ? O1 Co1 N3 C21 -35.5(2) . . . . ? N2 Co1 N3 C21 55.4(2) . . . . ? N1 Co1 N3 C21 140.2(2) . . . . ? N4 Co1 N3 C28 35.65(18) . . . . ? O1 Co1 N3 C28 128.49(18) . . . . ? N2 Co1 N3 C28 -140.58(19) . . . . ? N1 Co1 N3 C28 -55.83(19) . . . . ? O1 Co1 N4 C30 70.7(2) . . . . ? O2 Co1 N4 C30 -19.4(2) . . . . ? N3 Co1 N4 C30 159.9(2) . . . . ? N1 Co1 N4 C30 -104.4(2) . . . . ? O1 Co1 N4 C29 -101.37(19) . . . . ? O2 Co1 N4 C29 168.51(19) . . . . ? N3 Co1 N4 C29 -12.24(19) . . . . ? N1 Co1 N4 C29 83.5(2) . . . . ? Co1 N1 C1 C3 -165.1(2) . . . . ? Co1 N1 C1 C2 -40.7(3) . . . . ? Co1 N2 C2 C9 -164.2(2) . . . . ? Co1 N2 C2 C1 -36.6(3) . . . . ? N1 C1 C2 N2 49.4(3) . . . . ? C3 C1 C2 N2 176.0(3) . . . . ? N1 C1 C2 C9 175.6(3) . . . . ? C3 C1 C2 C9 -57.9(4) . . . . ? N1 C1 C3 C8 -125.4(3) . . . . ? C2 C1 C3 C8 113.2(3) . . . . ? N1 C1 C3 C4 57.8(4) . . . . ? C2 C1 C3 C4 -63.6(4) . . . . ? C8 C3 C4 C5 0.1(5) . . . . ? C1 C3 C4 C5 176.9(3) . . . . ? C3 C4 C5 C6 -0.9(6) . . . . ? C4 C5 C6 C7 0.9(6) . . . . ? C5 C6 C7 C8 -0.1(6) . . . . ? C6 C7 C8 C3 -0.7(5) . . . . ? C4 C3 C8 C7 0.7(5) . . . . ? C1 C3 C8 C7 -176.2(3) . . . . ? N2 C2 C9 C14 65.9(4) . . . . ? C1 C2 C9 C14 -57.1(4) . . . . ? N2 C2 C9 C10 -112.7(3) . . . . ? C1 C2 C9 C10 124.3(3) . . . . ? C14 C9 C10 C11 0.1(5) . . . . ? C2 C9 C10 C11 178.8(3) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C13 1.1(6) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C12 C13 C14 C9 -0.2(5) . . . . ? C10 C9 C14 C13 0.4(5) . . . . ? C2 C9 C14 C13 -178.1(3) . . . . ? Co1 O1 C15 C16 151.0(2) . . . . ? Co1 O1 C15 C20 -30.2(3) . . . . ? O1 C15 C16 C17 -176.9(3) . . . . ? C20 C15 C16 C17 4.2(4) . . . . ? C15 C16 C17 C18 -1.2(4) . . . . ? C16 C17 C18 C19 -2.1(4) . . . . ? C17 C18 C19 C20 2.3(4) . . . . ? C18 C19 C20 C15 0.7(4) . . . . ? C18 C19 C20 C21 -170.7(3) . . . . ? O1 C15 C20 C19 177.3(3) . . . . ? C16 C15 C20 C19 -3.9(4) . . . . ? O1 C15 C20 C21 -11.3(4) . . . . ? C16 C15 C20 C21 167.6(3) . . . . ? C28 N3 C21 C20 -154.8(3) . . . . ? Co1 N3 C21 C20 7.4(4) . . . . ? C28 N3 C21 C22 25.2(4) . . . . ? Co1 N3 C21 C22 -172.55(19) . . . . ? C19 C20 C21 N3 -165.0(3) . . . . ? C15 C20 C21 N3 23.7(4) . . . . ? C19 C20 C21 C22 14.9(4) . . . . ? C15 C20 C21 C22 -156.4(3) . . . . ? N3 C21 C22 C27 -118.2(3) . . . . ? C20 C21 C22 C27 61.9(4) . . . . ? N3 C21 C22 C23 59.9(4) . . . . ? C20 C21 C22 C23 -120.0(3) . . . . ? C27 C22 C23 O3 -178.9(3) . . . . ? C21 C22 C23 O3 3.0(4) . . . . ? C27 C22 C23 C24 -0.4(4) . . . . ? C21 C22 C23 C24 -178.5(3) . . . . ? O3 C23 C24 C25 179.6(3) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? C23 C24 C25 C26 -0.7(5) . . . . ? C24 C25 C26 C27 -0.6(5) . . . . ? C23 C22 C27 C26 -1.0(4) . . . . ? C21 C22 C27 C26 177.1(3) . . . . ? C25 C26 C27 C22 1.5(5) . . . . ? C21 N3 C28 C29 116.0(3) . . . . ? Co1 N3 C28 C29 -48.9(2) . . . . ? C30 N4 C29 C28 175.0(3) . . . . ? Co1 N4 C29 C28 -12.6(3) . . . . ? N3 C28 C29 N4 38.0(3) . . . . ? C29 N4 C30 C31 176.5(3) . . . . ? Co1 N4 C30 C31 4.9(4) . . . . ? N4 C30 C31 C32 -171.0(3) . . . . ? N4 C30 C31 C36 10.2(5) . . . . ? C36 C31 C32 C33 -0.6(4) . . . . ? C30 C31 C32 C33 -179.4(3) . . . . ? C31 C32 C33 C34 3.0(4) . . . . ? C31 C32 C33 C37 -177.7(3) . . . . ? C32 C33 C34 C35 -2.1(5) . . . . ? C37 C33 C34 C35 178.5(3) . . . . ? C33 C34 C35 C36 -1.3(5) . . . . ? C33 C34 C35 C41 177.2(3) . . . . ? Co1 O2 C36 C31 -20.3(4) . . . . ? Co1 O2 C36 C35 162.12(19) . . . . ? C32 C31 C36 O2 179.6(3) . . . . ? C30 C31 C36 O2 -1.7(4) . . . . ? C32 C31 C36 C35 -2.9(4) . . . . ? C30 C31 C36 C35 175.8(3) . . . . ? C34 C35 C36 O2 -178.7(3) . . . . ? C41 C35 C36 O2 2.9(4) . . . . ? C34 C35 C36 C31 3.7(4) . . . . ? C41 C35 C36 C31 -174.8(3) . . . . ? C32 C33 C37 C38 7.0(5) . . . . ? C34 C33 C37 C38 -173.6(3) . . . . ? C32 C33 C37 C39 -114.9(3) . . . . ? C34 C33 C37 C39 64.5(4) . . . . ? C32 C33 C37 C40 125.7(3) . . . . ? C34 C33 C37 C40 -55.0(4) . . . . ? C34 C35 C41 C43 -116.8(3) . . . . ? C36 C35 C41 C43 61.6(4) . . . . ? C34 C35 C41 C44 2.4(4) . . . . ? C36 C35 C41 C44 -179.3(3) . . . . ? C34 C35 C41 C42 122.0(3) . . . . ? C36 C35 C41 C42 -59.6(4) . . . . ? O5 S1 C45 C46 165.7(2) . . . . ? O4 S1 C45 C46 44.4(3) . . . . ? O6 S1 C45 C46 -74.7(3) . . . . ? O5 S1 C45 C50 -15.9(3) . . . . ? O4 S1 C45 C50 -137.2(3) . . . . ? O6 S1 C45 C50 103.7(3) . . . . ? C50 C45 C46 C47 -0.2(5) . . . . ? S1 C45 C46 C47 178.2(2) . . . . ? C45 C46 C47 C48 -0.6(5) . . . . ? C46 C47 C48 C49 0.9(5) . . . . ? C46 C47 C48 C51 -178.3(3) . . . . ? C47 C48 C49 C50 -0.6(5) . . . . ? C51 C48 C49 C50 178.7(3) . . . . ? C48 C49 C50 C45 -0.2(5) . . . . ? C46 C45 C50 C49 0.6(5) . . . . ? S1 C45 C50 C49 -177.8(2) . . . . ? 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 O3 H3O O6 0.99(5) 1.63(5) 2.620(3) 172(4) 2_656 N1 H1B O4 0.87(4) 2.07(4) 2.914(3) 165(3) . O1S H1S O5 0.84 1.90 2.738(4) 173.8 . O2S H2S O1S 0.84 2.00 2.821(6) 167.2 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.968 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.071 _iucr_refine_instructions_details ; TITL mo_d1339r_0m in P-1 CELL 0.71073 13.6309 14.1372 14.4020 98.858 95.100 105.071 ZERR 2.00 0.0031 0.0032 0.0033 0.005 0.005 0.005 LATT 1 SFAC C H N O S CO UNIT 110 138 8 16 2 2 TEMP -126.140 SIZE 0.120 0.220 0.220 ACTA L.S.4 FMAP 2 PLAN 20 EQIV $1 -x+1, -y, -z+1 HTAB O3 O6_$1 HTAB N1 O4 HTAB O1S O5 HTAB O2S O1S HTAB BOND $H DFIX 1.46 0.006 C1S C2S CONF WGHT 0.056000 1.617800 FVAR 0.13018 CO1 6 0.674387 0.323849 0.433371 11.00000 0.01944 0.02175 = 0.02126 0.00363 -0.00059 0.00667 O1 4 0.691813 0.461947 0.447339 11.00000 0.02593 0.02480 = 0.02345 0.00638 0.00171 0.00744 O2 4 0.769097 0.332406 0.344873 11.00000 0.01962 0.03042 = 0.02483 0.00603 0.00072 0.00916 O3 4 0.573217 0.229988 0.687701 11.00000 0.04794 0.03920 = 0.03954 0.02075 0.01757 0.02557 H3O 2 0.573464 0.180313 0.729365 11.00000 0.08074 N1 3 0.674092 0.182634 0.418397 11.00000 0.02251 0.02283 = 0.02457 0.00202 -0.00143 0.00717 H1B 2 0.616547 0.136241 0.403403 11.00000 0.04044 H1C 2 0.710427 0.179072 0.371178 11.00000 0.04647 N2 3 0.790237 0.345373 0.533183 11.00000 0.02398 0.02222 = 0.02902 0.00426 -0.00059 0.00807 H2B 2 0.839000 0.392443 0.524051 11.00000 0.03444 H2C 2 0.776589 0.362536 0.590119 11.00000 0.02914 N3 3 0.576782 0.316264 0.519291 11.00000 0.02362 0.02125 = 0.02019 0.00405 0.00034 0.00619 N4 3 0.558811 0.294085 0.341793 11.00000 0.01736 0.02092 = 0.02477 0.00447 0.00249 0.00667 C1 1 0.733150 0.165527 0.502737 11.00000 0.03210 0.02680 = 0.03161 0.00395 -0.00428 0.01139 AFIX 13 H1A 2 0.690514 0.166297 0.555732 11.00000 -1.20000 AFIX 0 C2 1 0.827224 0.254752 0.529780 11.00000 0.02822 0.02432 = 0.03705 0.00450 -0.00672 0.00852 AFIX 13 H2A 2 0.869641 0.253085 0.476673 11.00000 -1.20000 AFIX 0 C3 1 0.761553 0.068497 0.490210 11.00000 0.02829 0.02287 = 0.02869 0.00020 -0.00529 0.00993 C4 1 0.818274 0.042656 0.420586 11.00000 0.05757 0.03210 = 0.03917 0.01320 0.01681 0.01827 AFIX 43 H4A 2 0.837819 0.085403 0.376561 11.00000 -1.20000 AFIX 0 C5 1 0.846886 -0.044835 0.414347 11.00000 0.06768 0.04897 = 0.06240 0.00984 0.02810 0.03223 AFIX 43 H5A 2 0.885070 -0.062620 0.365755 11.00000 -1.20000 AFIX 0 C6 1 0.819497 -0.106335 0.479410 11.00000 0.05358 0.03036 = 0.06706 0.01334 0.00875 0.02347 AFIX 43 H6A 2 0.839666 -0.166093 0.476237 11.00000 -1.20000 AFIX 0 C7 1 0.763468 -0.080761 0.548035 11.00000 0.03651 0.03256 = 0.05654 0.02118 0.00423 0.00168 AFIX 43 H7A 2 0.744621 -0.123139 0.592505 11.00000 -1.20000 AFIX 0 C8 1 0.733850 0.005701 0.553709 11.00000 0.02702 0.03323 = 0.03991 0.00798 0.00658 0.00777 AFIX 43 H8A 2 0.694204 0.022188 0.601508 11.00000 -1.20000 AFIX 0 C9 1 0.894995 0.256674 0.619309 11.00000 0.02451 0.02179 = 0.03214 0.00177 -0.00654 0.00773 C10 1 0.997611 0.263906 0.614229 11.00000 0.03003 0.03933 = 0.04868 0.00149 -0.00070 0.00975 AFIX 43 H10A 2 1.023357 0.266172 0.555200 11.00000 -1.20000 AFIX 0 C11 1 1.062809 0.267841 0.695195 11.00000 0.03059 0.05478 = 0.08204 -0.01166 -0.02096 0.02163 AFIX 43 H11A 2 1.132980 0.271872 0.691520 11.00000 -1.20000 AFIX 0 C12 1 1.025690 0.265898 0.780906 11.00000 0.08109 0.05090 = 0.05294 -0.01672 -0.04334 0.03833 AFIX 43 H12A 2 1.070385 0.269731 0.836715 11.00000 -1.20000 AFIX 0 C13 1 0.923738 0.258392 0.785439 11.00000 0.08075 0.05041 = 0.03437 -0.00023 -0.00514 0.03681 AFIX 43 H13A 2 0.898075 0.256480 0.844533 11.00000 -1.20000 AFIX 0 C14 1 0.858645 0.253632 0.705425 11.00000 0.04017 0.03721 = 0.03686 0.00216 0.00067 0.01766 AFIX 43 H14A 2 0.788261 0.248220 0.709394 11.00000 -1.20000 AFIX 0 C15 1 0.701626 0.516222 0.532688 11.00000 0.01968 0.02434 = 0.02920 0.00694 -0.00293 0.01051 C16 1 0.759446 0.617137 0.548172 11.00000 0.02295 0.02577 = 0.03737 0.01129 0.00271 0.00804 AFIX 43 H16A 2 0.786979 0.644553 0.496717 11.00000 -1.20000 AFIX 0 C17 1 0.776640 0.676547 0.636580 11.00000 0.02057 0.02040 = 0.04438 0.00372 -0.00443 0.00566 AFIX 43 H17A 2 0.816890 0.743892 0.645307 11.00000 -1.20000 AFIX 0 C18 1 0.735854 0.639440 0.713779 11.00000 0.02808 0.02678 = 0.03345 -0.00127 -0.01005 0.00992 AFIX 43 H18A 2 0.750066 0.680333 0.774952 11.00000 -1.20000 AFIX 0 C19 1 0.674958 0.542979 0.699721 11.00000 0.02961 0.02695 = 0.02622 0.00477 -0.00039 0.01142 AFIX 43 H19A 2 0.645101 0.518405 0.751493 11.00000 -1.20000 AFIX 0 C20 1 0.655484 0.479191 0.610177 11.00000 0.02284 0.02033 = 0.02524 0.00499 -0.00172 0.00735 C21 1 0.578800 0.382730 0.593199 11.00000 0.02343 0.02133 = 0.02364 0.00751 0.00094 0.00940 C22 1 0.502755 0.359844 0.660196 11.00000 0.02443 0.02225 = 0.01896 0.00142 0.00062 0.00705 C23 1 0.500889 0.278617 0.705839 11.00000 0.02908 0.02504 = 0.02565 0.00400 0.00289 0.01020 C24 1 0.429287 0.253642 0.767177 11.00000 0.03936 0.02886 = 0.03207 0.01064 0.01097 0.00664 AFIX 43 H24A 2 0.428533 0.199559 0.799185 11.00000 -1.20000 AFIX 0 C25 1 0.359095 0.307791 0.781486 11.00000 0.03362 0.03498 = 0.03654 0.00241 0.01323 0.00428 AFIX 43 H25A 2 0.309710 0.289988 0.822938 11.00000 -1.20000 AFIX 0 C26 1 0.359659 0.387355 0.736455 11.00000 0.02704 0.03307 = 0.03892 -0.00381 0.00354 0.01068 AFIX 43 H26A 2 0.310621 0.423611 0.746366 11.00000 -1.20000 AFIX 0 C27 1 0.432649 0.414013 0.676426 11.00000 0.03065 0.02798 = 0.02508 0.00390 0.00102 0.00879 AFIX 43 H27A 2 0.434400 0.469646 0.646427 11.00000 -1.20000 AFIX 0 C28 1 0.481799 0.237647 0.477019 11.00000 0.02389 0.02336 = 0.02449 0.00048 0.00101 0.00442 AFIX 23 H28A 2 0.424946 0.241522 0.514373 11.00000 -1.20000 H28B 2 0.492423 0.170554 0.473045 11.00000 -1.20000 AFIX 0 C29 1 0.459878 0.260629 0.378348 11.00000 0.01647 0.03389 = 0.02484 0.00419 0.00203 0.00737 AFIX 23 H29A 2 0.415309 0.200272 0.335458 11.00000 -1.20000 H29B 2 0.424198 0.313520 0.381782 11.00000 -1.20000 AFIX 0 C30 1 0.562224 0.311633 0.257086 11.00000 0.02029 0.02617 = 0.02296 0.00276 -0.00132 0.00755 AFIX 43 H30A 2 0.498579 0.298571 0.217920 11.00000 -1.20000 AFIX 0 C31 1 0.654001 0.349389 0.216083 11.00000 0.01896 0.02715 = 0.02007 0.00016 -0.00043 0.00836 C32 1 0.640673 0.377052 0.127107 11.00000 0.02108 0.02968 = 0.02255 0.00142 0.00066 0.00867 AFIX 43 H32A 2 0.573206 0.370594 0.098356 11.00000 -1.20000 AFIX 0 C33 1 0.721985 0.413066 0.080499 11.00000 0.02839 0.03033 = 0.02227 0.00475 0.00315 0.01161 C34 1 0.819910 0.416382 0.124739 11.00000 0.02430 0.03103 = 0.03315 0.00866 0.01114 0.00968 AFIX 43 H34A 2 0.877125 0.438959 0.092725 11.00000 -1.20000 AFIX 0 C35 1 0.838313 0.388966 0.211661 11.00000 0.01878 0.02431 = 0.03319 0.00608 0.00226 0.00706 C36 1 0.753048 0.357052 0.260769 11.00000 0.02233 0.02064 = 0.02355 0.00160 0.00139 0.00788 C37 1 0.712251 0.448031 -0.015207 11.00000 0.03442 0.04213 = 0.02551 0.01065 0.00904 0.01416 C38 1 0.603119 0.449352 -0.044522 11.00000 0.04132 0.12415 = 0.03518 0.04157 0.00865 0.03141 AFIX 137 H38A 2 0.600087 0.478337 -0.101935 11.00000 -1.50000 H38B 2 0.580727 0.489491 0.006692 11.00000 -1.50000 H38C 2 0.557972 0.381081 -0.057280 11.00000 -1.50000 AFIX 0 C39 1 0.745561 0.379898 -0.091443 11.00000 0.07029 0.04855 = 0.02927 0.00525 0.01632 0.02105 AFIX 137 H39A 2 0.741337 0.404052 -0.151501 11.00000 -1.50000 H39B 2 0.700375 0.311958 -0.099613 11.00000 -1.50000 H39C 2 0.816358 0.379939 -0.072162 11.00000 -1.50000 AFIX 0 C40 1 0.781680 0.554368 -0.005133 11.00000 0.06644 0.04753 = 0.03621 0.01775 0.00918 0.02145 AFIX 137 H40A 2 0.774387 0.577639 -0.065374 11.00000 -1.50000 H40B 2 0.853172 0.555100 0.011673 11.00000 -1.50000 H40C 2 0.761910 0.598416 0.044750 11.00000 -1.50000 AFIX 0 C41 1 0.946904 0.390377 0.252502 11.00000 0.01763 0.03238 = 0.04500 0.01497 0.00273 0.00612 C42 1 0.979957 0.459279 0.350347 11.00000 0.02807 0.03392 = 0.06860 0.00268 -0.01482 0.00355 AFIX 137 H42A 2 0.980145 0.527337 0.343933 11.00000 -1.50000 H42B 2 1.048985 0.458710 0.375447 11.00000 -1.50000 H42C 2 0.931766 0.435618 0.393898 11.00000 -1.50000 AFIX 0 C43 1 0.948833 0.284284 0.261219 11.00000 0.02429 0.03493 = 0.04544 0.01144 0.00303 0.01175 AFIX 137 H43A 2 0.932783 0.242067 0.198086 11.00000 -1.50000 H43B 2 0.897807 0.257496 0.301214 11.00000 -1.50000 H43C 2 1.017144 0.285377 0.289937 11.00000 -1.50000 AFIX 0 C44 1 1.027500 0.428559 0.188890 11.00000 0.02166 0.07834 = 0.08846 0.05125 0.01661 0.01427 AFIX 137 H44A 2 1.009566 0.385920 0.125953 11.00000 -1.50000 H44B 2 1.095038 0.427001 0.217156 11.00000 -1.50000 H44C 2 1.029304 0.497110 0.182984 11.00000 -1.50000 AFIX 0 S1 5 0.445005 0.004070 0.232682 11.00000 0.02654 0.02679 = 0.02818 0.00419 0.00056 0.00589 O4 4 0.485772 0.030237 0.333062 11.00000 0.03330 0.04006 = 0.02600 -0.00020 0.00319 0.00199 O5 4 0.369020 0.054342 0.206480 11.00000 0.03100 0.04477 = 0.05569 0.01514 0.00459 0.01776 O6 4 0.408117 -0.103989 0.200696 11.00000 0.04218 0.02683 = 0.02997 0.00796 -0.00418 0.00221 C45 1 0.549322 0.046270 0.170329 11.00000 0.03106 0.02185 = 0.02678 -0.00142 0.00306 0.00674 C46 1 0.642578 0.029517 0.195832 11.00000 0.03506 0.02989 = 0.03209 0.00544 0.00374 0.01027 AFIX 43 H46A 2 0.651253 -0.002864 0.247837 11.00000 -1.20000 AFIX 0 C47 1 0.723327 0.059962 0.145528 11.00000 0.03267 0.03815 = 0.04178 -0.00066 0.00494 0.01055 AFIX 43 H47A 2 0.787470 0.048770 0.163782 11.00000 -1.20000 AFIX 0 C48 1 0.711979 0.107143 0.067920 11.00000 0.04295 0.03293 = 0.03186 -0.00466 0.00971 0.00162 C49 1 0.618060 0.123667 0.044036 11.00000 0.05487 0.03042 = 0.02656 0.00545 0.00597 0.00487 AFIX 43 H49A 2 0.608909 0.156015 -0.007897 11.00000 -1.20000 AFIX 0 C50 1 0.537402 0.093959 0.094369 11.00000 0.03775 0.02821 = 0.03408 0.00507 0.00121 0.01034 AFIX 43 H50A 2 0.473550 0.106164 0.077010 11.00000 -1.20000 AFIX 0 C51 1 0.798470 0.138238 0.010603 11.00000 0.05959 0.05217 = 0.04868 0.00155 0.02256 0.00053 AFIX 137 H51A 2 0.773461 0.113616 -0.057007 11.00000 -1.50000 H51B 2 0.854211 0.110164 0.029262 11.00000 -1.50000 H51C 2 0.823874 0.211116 0.022353 11.00000 -1.50000 AFIX 0 O1S 4 0.182036 0.092483 0.205723 11.00000 0.05351 0.06371 = 0.10354 0.02142 0.01585 0.02056 AFIX 83 H1S 2 0.237788 0.078166 0.201877 11.00000 -1.50000 AFIX 0 C1S 1 0.004889 0.025973 0.212626 11.00000 0.06906 0.09930 = 0.18338 0.04145 0.03955 0.02980 AFIX 137 H1S1 2 -0.050157 -0.036177 0.205210 11.00000 -1.50000 H1S2 2 -0.008166 0.062265 0.162252 11.00000 -1.50000 H1S3 2 0.007240 0.067176 0.274528 11.00000 -1.50000 AFIX 0 C2S 1 0.101681 0.003384 0.206575 11.00000 0.05315 0.06550 = 0.09679 0.00036 0.00195 0.01080 AFIX 23 H2SA 2 0.096317 -0.045653 0.148002 11.00000 -1.20000 H2SB 2 0.118597 -0.026631 0.261472 11.00000 -1.20000 AFIX 0 O2S 4 0.145640 0.192284 0.056609 11.00000 0.10594 0.11174 = 0.16242 0.04680 -0.01352 0.02726 AFIX 83 H2S 2 0.158107 0.171318 0.106616 11.00000 -1.50000 AFIX 0 C3S 1 0.322713 0.213020 0.027194 11.00000 0.05963 0.09503 = 0.16647 0.06060 0.01249 0.04128 AFIX 137 H3SA 2 0.364748 0.176934 -0.007336 11.00000 -1.50000 H3SB 2 0.333130 0.209431 0.094631 11.00000 -1.50000 H3SC 2 0.342736 0.282911 0.019682 11.00000 -1.50000 AFIX 0 C4S 1 0.212193 0.166942 -0.011530 11.00000 0.14565 0.07979 = 0.07422 0.00996 0.03266 0.04336 AFIX 23 H4SA 2 0.196612 0.190669 -0.070832 11.00000 -1.20000 H4SB 2 0.198548 0.093611 -0.026927 11.00000 -1.20000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_d1339r_0m in P-1 REM R1 = 0.0570 for 7600 Fo > 4sig(Fo) and 0.1071 for all 11987 data REM 651 parameters refined using 1 restraints END WGHT 0.0572 1.4489 REM Highest difference peak 0.968, deepest hole -0.536, 1-sigma level 0.071 Q1 1 0.7839 0.1860 0.4642 11.00000 0.05 0.49 Q2 1 0.2004 0.1784 0.0033 11.00000 0.05 0.44 Q3 1 0.4486 0.4828 0.6267 11.00000 0.05 0.42 Q4 1 0.7815 0.2444 0.5743 11.00000 0.05 0.39 Q5 1 0.4187 -0.0424 0.2710 11.00000 0.05 0.39 Q6 1 0.6734 0.2944 0.4840 11.00000 0.05 0.39 Q7 1 0.1308 0.1000 -0.0081 11.00000 0.05 0.33 Q8 1 0.4042 -0.0566 0.2473 11.00000 0.05 0.31 Q9 1 0.0073 -0.0185 0.1493 11.00000 0.05 0.30 Q10 1 0.0788 0.0441 0.1476 11.00000 0.05 0.29 Q11 1 0.6876 0.4886 0.5740 11.00000 0.05 0.29 Q12 1 0.0879 0.0824 0.1127 11.00000 0.05 0.29 Q13 1 0.8184 0.4104 0.1753 11.00000 0.05 0.28 Q14 1 1.0376 0.3021 0.6586 11.00000 0.05 0.27 Q15 1 0.3532 0.0293 0.2612 11.00000 0.05 0.27 Q16 1 0.6405 0.3421 0.1716 11.00000 0.05 0.26 Q17 1 0.0043 0.0343 0.1211 11.00000 0.05 0.25 Q18 1 0.6240 0.4289 0.6059 11.00000 0.05 0.25 Q19 1 0.5168 0.0354 0.2077 11.00000 0.05 0.25 Q20 1 0.7214 0.5569 -0.1047 11.00000 0.05 0.24 ; _database_code_depnum_ccdc_archive 'CCDC 959826'