# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'C McKenzie' 'Andrew D Bond' 'Rune Kirk Egdal' 'Frank B. Johansson' 'Sune Veltze' _publ_contact_author_name 'Christine McKenzie' _publ_contact_author_email CHK@IFK.SDU.DK _publ_section_title ; Coordinative Flexibility in an Acyclic Bis(Sulfonamide) Ligand ; # Attachment 'submit.cif' ################################################################ ## Coordinative flexibility of a dinucleating acyclic ## ## bis(sulfonamide) ligand ## ## S. Veltze, A. D. Bond and C. J. McKenzie ## ################################################################ data_bpsmpH _database_code_depnum_ccdc_archive 'CCDC 737969' _chemical_name_systematic ; 2,6-bis(N,N-bis-(2-pyridylmethyl)-sulfonamido)-4-methylphenol ; _chemical_name_common bpsmpH _chemical_melting_point 414 _chemical_formula_moiety 'C31 H30 N6 O5 S2' _chemical_formula_sum 'C31 H30 N6 O5 S2' _chemical_formula_weight 630.73 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8121(2) _cell_length_b 9.9746(2) _cell_length_c 33.1686(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.344(1) _cell_angle_gamma 90.00 _cell_volume 2907.05(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8706 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; H atoms visible on both O1 and N5 in difference Fourier maps. Refined as a 50:50 mixture of the two cases, with the H atom constrained in an idealised position for N5 and the observed position for O1. [Free refinement of the H atom causes it to move half-way between the two atoms, leaving residual peaks on both] ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 32567 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 5903 _reflns_number_gt 4384 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0446P)^2^+0.9372P] 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 5903 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.302 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.048 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 S1 S 0.68586(5) 0.59940(5) 0.076657(14) 0.02291(12) Uani 1 1 d . . . S2 S 0.28195(5) 0.66370(4) 0.193130(13) 0.01861(12) Uani 1 1 d . . . O1 O 0.58921(13) 0.69462(13) 0.15446(4) 0.0240(3) Uani 1 1 d . . . H1 H 0.5805 0.7276 0.1781 0.036 Uiso 0.50 1 d PR . . O11 O 0.78299(14) 0.53464(13) 0.10723(4) 0.0302(3) Uani 1 1 d . . . O12 O 0.67668(15) 0.54459(14) 0.03655(4) 0.0314(3) Uani 1 1 d . . . O21 O 0.12117(14) 0.64360(13) 0.19525(4) 0.0264(3) Uani 1 1 d . . . O22 O 0.38307(14) 0.58598(12) 0.21964(4) 0.0241(3) Uani 1 1 d . . . N1 N 0.73647(18) 0.75815(16) 0.07454(5) 0.0269(4) Uani 1 1 d . . . N2 N 0.9913(2) 1.01609(19) 0.08824(6) 0.0424(5) Uani 1 1 d . . . N3 N 0.4452(2) 0.89598(18) 0.04747(5) 0.0389(5) Uani 1 1 d . . . N4 N 0.32843(17) 0.82124(14) 0.20171(4) 0.0194(3) Uani 1 1 d . . . N5 N 0.64106(17) 0.79653(16) 0.22237(5) 0.0240(4) Uani 1 1 d . . . H5 H 0.5945 0.7569 0.2012 0.029 Uiso 0.50 1 calc PR . . N6 N 0.2669(2) 1.15866(16) 0.18306(5) 0.0312(4) Uani 1 1 d . . . C1 C 0.4750(2) 0.64765(17) 0.13169(5) 0.0190(4) Uani 1 1 d . . . C2 C 0.4987(2) 0.60274(17) 0.09205(5) 0.0189(4) Uani 1 1 d . . . C3 C 0.3816(2) 0.55611(18) 0.06558(5) 0.0218(4) Uani 1 1 d . . . H3A H 0.4031 0.5292 0.0391 0.026 Uiso 1 1 calc R . . C4 C 0.2332(2) 0.54779(18) 0.07686(5) 0.0228(4) Uani 1 1 d . . . C5 C 0.2070(2) 0.58603(17) 0.11588(5) 0.0207(4) Uani 1 1 d . . . H5A H 0.1070 0.5786 0.1245 0.025 Uiso 1 1 calc R . . C6 C 0.3233(2) 0.63522(17) 0.14288(5) 0.0184(4) Uani 1 1 d . . . C7 C 0.1066(2) 0.4987(2) 0.04741(6) 0.0351(5) Uani 1 1 d . . . H7A H 0.1443 0.4256 0.0311 0.053 Uiso 1 1 calc R . . H7B H 0.0710 0.5725 0.0296 0.053 Uiso 1 1 calc R . . H7C H 0.0222 0.4660 0.0623 0.053 Uiso 1 1 calc R . . C8 C 0.8841(2) 0.7958(2) 0.09475(7) 0.0380(5) Uani 1 1 d . . . H8A H 0.9653 0.7761 0.0766 0.046 Uiso 1 1 calc R . . H8B H 0.9035 0.7408 0.1195 0.046 Uiso 1 1 calc R . . C9 C 0.8909(2) 0.9415(2) 0.10609(7) 0.0334(5) Uani 1 1 d . . . C10 C 0.8015(3) 0.9920(2) 0.13486(8) 0.0497(6) Uani 1 1 d . . . H10A H 0.7305 0.9359 0.1469 0.060 Uiso 1 1 calc R . . C11 C 0.8164(3) 1.1246(3) 0.14594(9) 0.0600(7) Uani 1 1 d . . . H11A H 0.7568 1.1613 0.1659 0.072 Uiso 1 1 calc R . . C12 C 0.9190(3) 1.2029(3) 0.12757(8) 0.0542(7) Uani 1 1 d . . . H12A H 0.9314 1.2950 0.1343 0.065 Uiso 1 1 calc R . . C13 C 1.0028(3) 1.1448(3) 0.09937(8) 0.0513(7) Uani 1 1 d . . . H13A H 1.0740 1.1994 0.0868 0.062 Uiso 1 1 calc R . . C14 C 0.6988(2) 0.8256(2) 0.03515(6) 0.0366(5) Uani 1 1 d . . . H14A H 0.7514 0.7784 0.0140 0.044 Uiso 1 1 calc R . . H14B H 0.7380 0.9186 0.0368 0.044 Uiso 1 1 calc R . . C15 C 0.5315(2) 0.8295(2) 0.02281(6) 0.0316(5) Uani 1 1 d . . . C16 C 0.4725(3) 0.7686(2) -0.01234(6) 0.0409(6) Uani 1 1 d . . . H16A H 0.5376 0.7228 -0.0293 0.049 Uiso 1 1 calc R . . C17 C 0.3178(3) 0.7751(2) -0.02266(7) 0.0500(7) Uani 1 1 d . . . H17A H 0.2748 0.7343 -0.0468 0.060 Uiso 1 1 calc R . . C18 C 0.2269(3) 0.8424(2) 0.00290(8) 0.0498(6) Uani 1 1 d . . . H18A H 0.1199 0.8482 -0.0031 0.060 Uiso 1 1 calc R . . C19 C 0.2950(3) 0.9007(2) 0.03722(7) 0.0462(6) Uani 1 1 d . . . H19A H 0.2322 0.9470 0.0547 0.055 Uiso 1 1 calc R . . C20 C 0.3889(2) 0.85424(19) 0.24337(5) 0.0223(4) Uani 1 1 d . . . H20A H 0.3512 0.7868 0.2621 0.027 Uiso 1 1 calc R . . H20B H 0.3483 0.9426 0.2508 0.027 Uiso 1 1 calc R . . C21 C 0.5597(2) 0.85852(17) 0.24910(5) 0.0210(4) Uani 1 1 d . . . C22 C 0.6325(2) 0.9218(2) 0.28245(6) 0.0293(5) Uani 1 1 d . . . H22A H 0.5747 0.9661 0.3015 0.035 Uiso 1 1 calc R . . C23 C 0.7891(2) 0.9199(2) 0.28780(6) 0.0360(5) Uani 1 1 d . . . H23A H 0.8401 0.9635 0.3104 0.043 Uiso 1 1 calc R . . C24 C 0.8711(2) 0.8541(2) 0.25997(6) 0.0358(5) Uani 1 1 d . . . H24A H 0.9790 0.8505 0.2633 0.043 Uiso 1 1 calc R . . C25 C 0.7936(2) 0.7942(2) 0.22754(6) 0.0312(5) Uani 1 1 d . . . H25A H 0.8494 0.7497 0.2081 0.037 Uiso 1 1 calc R . . C26 C 0.2184(2) 0.92005(18) 0.18307(6) 0.0253(4) Uani 1 1 d . . . H26A H 0.1495 0.9500 0.2035 0.030 Uiso 1 1 calc R . . H26B H 0.1557 0.8765 0.1608 0.030 Uiso 1 1 calc R . . C27 C 0.2976(2) 1.03993(18) 0.16688(5) 0.0232(4) Uani 1 1 d . . . C28 C 0.3879(2) 1.0264(2) 0.13517(6) 0.0348(5) Uani 1 1 d . . . H28A H 0.4090 0.9400 0.1249 0.042 Uiso 1 1 calc R . . C29 C 0.4478(3) 1.1391(2) 0.11834(7) 0.0434(6) Uani 1 1 d . . . H29A H 0.5094 1.1321 0.0961 0.052 Uiso 1 1 calc R . . C30 C 0.4159(3) 1.2627(2) 0.13463(7) 0.0419(6) Uani 1 1 d . . . H30A H 0.4544 1.3429 0.1238 0.050 Uiso 1 1 calc R . . C31 C 0.3279(3) 1.2667(2) 0.16661(6) 0.0383(5) Uani 1 1 d . . . H31A H 0.3084 1.3518 0.1780 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0235(3) 0.0212(3) 0.0250(2) -0.00238(19) 0.0080(2) 0.0003(2) S2 0.0206(2) 0.0162(2) 0.0195(2) 0.00056(18) 0.00467(18) -0.00079(18) O1 0.0193(7) 0.0323(8) 0.0203(6) -0.0065(6) 0.0012(5) -0.0026(6) O11 0.0251(7) 0.0294(8) 0.0366(8) 0.0040(6) 0.0056(6) 0.0070(6) O12 0.0352(8) 0.0327(8) 0.0279(7) -0.0089(6) 0.0125(6) -0.0009(6) O21 0.0218(7) 0.0271(7) 0.0313(7) -0.0018(6) 0.0091(6) -0.0054(6) O22 0.0318(8) 0.0199(7) 0.0208(6) 0.0033(5) 0.0030(6) 0.0037(6) N1 0.0266(9) 0.0242(9) 0.0303(9) 0.0007(7) 0.0040(7) -0.0029(7) N2 0.0408(11) 0.0356(11) 0.0507(12) 0.0007(9) 0.0012(9) -0.0083(9) N3 0.0464(12) 0.0351(11) 0.0354(10) 0.0024(8) 0.0046(9) 0.0031(9) N4 0.0215(8) 0.0147(8) 0.0218(8) 0.0004(6) 0.0007(6) 0.0013(6) N5 0.0216(9) 0.0265(9) 0.0236(8) -0.0043(7) 0.0005(7) -0.0028(7) N6 0.0444(11) 0.0208(9) 0.0283(9) -0.0002(7) 0.0012(8) 0.0032(8) C1 0.0213(10) 0.0155(9) 0.0203(9) 0.0024(7) 0.0017(8) 0.0004(8) C2 0.0209(10) 0.0158(9) 0.0206(9) 0.0019(7) 0.0045(7) -0.0002(8) C3 0.0285(11) 0.0176(9) 0.0194(9) -0.0007(7) 0.0025(8) 0.0009(8) C4 0.0238(10) 0.0209(10) 0.0232(10) 0.0000(8) -0.0015(8) 0.0002(8) C5 0.0203(10) 0.0174(9) 0.0242(9) 0.0032(7) 0.0014(8) 0.0015(8) C6 0.0215(10) 0.0150(9) 0.0187(9) 0.0009(7) 0.0021(7) 0.0015(7) C7 0.0300(12) 0.0466(14) 0.0280(11) -0.0091(10) -0.0020(9) -0.0042(10) C8 0.0278(12) 0.0329(12) 0.0530(14) -0.0007(10) 0.0009(10) 0.0004(10) C9 0.0255(11) 0.0276(11) 0.0456(13) 0.0010(10) -0.0074(10) 0.0006(9) C10 0.0474(15) 0.0399(14) 0.0631(16) -0.0076(12) 0.0135(13) -0.0046(12) C11 0.0558(17) 0.0531(17) 0.0711(19) -0.0218(14) 0.0053(14) 0.0010(14) C12 0.0542(17) 0.0320(14) 0.0729(19) -0.0131(13) -0.0177(14) 0.0008(12) C13 0.0521(16) 0.0376(15) 0.0629(17) 0.0025(12) -0.0044(13) -0.0124(12) C14 0.0460(14) 0.0336(13) 0.0312(11) 0.0065(9) 0.0097(10) -0.0051(10) C15 0.0440(13) 0.0248(11) 0.0263(10) 0.0070(9) 0.0044(9) -0.0013(10) C16 0.0601(16) 0.0330(13) 0.0292(12) 0.0029(9) 0.0004(11) 0.0065(11) C17 0.0678(19) 0.0362(14) 0.0429(14) 0.0061(11) -0.0164(13) -0.0014(13) C18 0.0478(15) 0.0439(15) 0.0558(16) 0.0181(13) -0.0088(13) 0.0000(12) C19 0.0489(16) 0.0425(14) 0.0477(14) 0.0089(11) 0.0071(12) 0.0085(12) C20 0.0247(10) 0.0223(10) 0.0201(9) -0.0047(8) 0.0039(8) 0.0006(8) C21 0.0257(10) 0.0149(9) 0.0222(9) 0.0016(7) 0.0011(8) -0.0007(8) C22 0.0351(12) 0.0264(11) 0.0261(10) -0.0063(8) 0.0004(9) 0.0019(9) C23 0.0366(13) 0.0350(12) 0.0345(11) -0.0099(10) -0.0094(10) -0.0055(10) C24 0.0248(11) 0.0425(13) 0.0390(12) -0.0076(10) -0.0049(9) -0.0059(10) C25 0.0235(11) 0.0362(12) 0.0342(11) -0.0062(9) 0.0040(9) -0.0008(9) C26 0.0234(10) 0.0204(10) 0.0316(10) 0.0027(8) -0.0007(8) 0.0038(8) C27 0.0287(11) 0.0188(10) 0.0213(9) 0.0016(8) -0.0032(8) 0.0023(8) C28 0.0466(13) 0.0241(11) 0.0349(12) 0.0017(9) 0.0101(10) 0.0048(10) C29 0.0549(15) 0.0415(14) 0.0358(12) 0.0101(10) 0.0167(11) 0.0029(12) C30 0.0553(15) 0.0277(12) 0.0425(13) 0.0123(10) 0.0025(12) -0.0071(11) C31 0.0608(16) 0.0188(11) 0.0348(12) 0.0005(9) 0.0005(11) 0.0000(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O11 1.4307(14) . ? S1 O12 1.4349(13) . ? S1 N1 1.6481(16) . ? S1 C2 1.7632(18) . ? S2 O22 1.4317(13) . ? S2 O21 1.4379(13) . ? S2 N4 1.6433(15) . ? S2 C6 1.7561(17) . ? O1 C1 1.299(2) . ? O1 H1 0.861 . ? N1 C8 1.467(3) . ? N1 C14 1.485(2) . ? N2 C9 1.329(3) . ? N2 C13 1.338(3) . ? N3 C15 1.334(3) . ? N3 C19 1.343(3) . ? N4 C20 1.480(2) . ? N4 C26 1.484(2) . ? N5 C21 1.334(2) . ? N5 C25 1.343(2) . ? N5 H5 0.880 . ? N6 C27 1.336(2) . ? N6 C31 1.339(3) . ? C1 C6 1.419(2) . ? C1 C2 1.420(2) . ? C2 C3 1.384(3) . ? C3 C4 1.390(3) . ? C3 H3A 0.950 . ? C4 C5 1.385(2) . ? C4 C7 1.508(3) . ? C5 C6 1.398(2) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.501(3) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.378(3) . ? C10 C11 1.377(3) . ? C10 H10A 0.950 . ? C11 C12 1.372(4) . ? C11 H11A 0.950 . ? C12 C13 1.364(4) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.500(3) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.381(3) . ? C16 C17 1.382(3) . ? C16 H16A 0.950 . ? C17 C18 1.384(4) . ? C17 H17A 0.950 . ? C18 C19 1.375(3) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.503(3) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.388(3) . ? C22 C23 1.378(3) . ? C22 H22A 0.950 . ? C23 C24 1.381(3) . ? C23 H23A 0.950 . ? C24 C25 1.367(3) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.504(3) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.373(3) . ? C28 C29 1.377(3) . ? C28 H28A 0.950 . ? C29 C30 1.384(3) . ? C29 H29A 0.950 . ? C30 C31 1.361(3) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? 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 O11 S1 O12 118.28(8) . . ? O11 S1 N1 108.34(8) . . ? O12 S1 N1 108.84(8) . . ? O11 S1 C2 109.01(8) . . ? O12 S1 C2 106.70(8) . . ? N1 S1 C2 104.85(8) . . ? O22 S2 O21 117.66(8) . . ? O22 S2 N4 106.02(8) . . ? O21 S2 N4 111.01(8) . . ? O22 S2 C6 109.34(8) . . ? O21 S2 C6 107.46(8) . . ? N4 S2 C6 104.61(8) . . ? C1 O1 H1 123.3 . . ? C8 N1 C14 114.70(16) . . ? C8 N1 S1 117.39(13) . . ? C14 N1 S1 115.45(13) . . ? C9 N2 C13 117.0(2) . . ? C15 N3 C19 117.3(2) . . ? C20 N4 C26 114.77(14) . . ? C20 N4 S2 116.22(12) . . ? C26 N4 S2 114.60(12) . . ? C21 N5 C25 120.44(16) . . ? C21 N5 H5 119.8 . . ? C25 N5 H5 119.8 . . ? C27 N6 C31 116.75(18) . . ? O1 C1 C6 125.66(16) . . ? O1 C1 C2 119.35(16) . . ? C6 C1 C2 114.98(15) . . ? C3 C2 C1 122.59(16) . . ? C3 C2 S1 118.61(13) . . ? C1 C2 S1 118.74(13) . . ? C2 C3 C4 121.41(16) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 117.49(16) . . ? C5 C4 C7 121.83(17) . . ? C3 C4 C7 120.67(16) . . ? C4 C5 C6 121.96(17) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 121.49(16) . . ? C5 C6 S2 118.03(13) . . ? C1 C6 S2 120.09(13) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 112.31(17) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C10 122.6(2) . . ? N2 C9 C8 116.5(2) . . ? C10 C9 C8 120.9(2) . . ? C11 C10 C9 119.2(2) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 118.8(3) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C13 C12 C11 118.2(2) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? N2 C13 C12 124.3(2) . . ? N2 C13 H13A 117.9 . . ? C12 C13 H13A 117.9 . . ? N1 C14 C15 113.68(16) . . ? N1 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N1 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N3 C15 C16 122.7(2) . . ? N3 C15 C14 116.05(18) . . ? C16 C15 C14 121.2(2) . . ? C15 C16 C17 119.3(2) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C16 C17 C18 118.5(2) . . ? C16 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? C19 C18 C17 118.4(2) . . ? C19 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? N3 C19 C18 123.7(2) . . ? N3 C19 H19A 118.1 . . ? C18 C19 H19A 118.1 . . ? N4 C20 C21 114.24(14) . . ? N4 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? N4 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N5 C21 C22 120.06(17) . . ? N5 C21 C20 119.11(16) . . ? C22 C21 C20 120.79(17) . . ? C23 C22 C21 119.66(18) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 119.34(19) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 118.58(19) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? N5 C25 C24 121.91(19) . . ? N5 C25 H25A 119.0 . . ? C24 C25 H25A 119.0 . . ? N4 C26 C27 111.75(15) . . ? N4 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? N4 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? N6 C27 C28 122.78(18) . . ? N6 C27 C26 116.61(17) . . ? C28 C27 C26 120.47(17) . . ? C27 C28 C29 119.5(2) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C28 C29 C30 118.3(2) . . ? C28 C29 H29A 120.9 . . ? C30 C29 H29A 120.9 . . ? C31 C30 C29 118.3(2) . . ? C31 C30 H30A 120.8 . . ? C29 C30 H30A 120.8 . . ? N6 C31 C30 124.3(2) . . ? N6 C31 H31A 117.8 . . ? C30 C31 H31A 117.8 . . ? 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 O11 S1 N1 C8 14.58(17) . . . . ? O12 S1 N1 C8 -115.26(15) . . . . ? C2 S1 N1 C8 130.87(15) . . . . ? O11 S1 N1 C14 154.75(13) . . . . ? O12 S1 N1 C14 24.91(16) . . . . ? C2 S1 N1 C14 -88.96(15) . . . . ? O22 S2 N4 C20 -31.09(14) . . . . ? O21 S2 N4 C20 97.78(13) . . . . ? C6 S2 N4 C20 -146.61(12) . . . . ? O22 S2 N4 C26 -168.76(12) . . . . ? O21 S2 N4 C26 -39.89(14) . . . . ? C6 S2 N4 C26 75.72(14) . . . . ? O1 C1 C2 C3 -177.58(16) . . . . ? C6 C1 C2 C3 2.9(2) . . . . ? O1 C1 C2 S1 5.2(2) . . . . ? C6 C1 C2 S1 -174.32(12) . . . . ? O11 S1 C2 C3 -128.74(14) . . . . ? O12 S1 C2 C3 0.07(17) . . . . ? N1 S1 C2 C3 115.43(15) . . . . ? O11 S1 C2 C1 48.57(16) . . . . ? O12 S1 C2 C1 177.37(14) . . . . ? N1 S1 C2 C1 -67.26(15) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? S1 C2 C3 C4 175.69(14) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C2 C3 C4 C7 179.08(18) . . . . ? C3 C4 C5 C6 1.9(3) . . . . ? C7 C4 C5 C6 -178.13(17) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? C4 C5 C6 S2 -173.31(14) . . . . ? O1 C1 C6 C5 178.57(17) . . . . ? C2 C1 C6 C5 -1.9(2) . . . . ? O1 C1 C6 S2 -8.7(2) . . . . ? C2 C1 C6 S2 170.82(13) . . . . ? O22 S2 C6 C5 121.88(14) . . . . ? O21 S2 C6 C5 -6.88(16) . . . . ? N4 S2 C6 C5 -124.93(14) . . . . ? O22 S2 C6 C1 -51.10(16) . . . . ? O21 S2 C6 C1 -179.86(13) . . . . ? N4 S2 C6 C1 62.08(15) . . . . ? C14 N1 C8 C9 63.5(2) . . . . ? S1 N1 C8 C9 -156.04(15) . . . . ? C13 N2 C9 C10 -0.1(3) . . . . ? C13 N2 C9 C8 -177.3(2) . . . . ? N1 C8 C9 N2 -116.4(2) . . . . ? N1 C8 C9 C10 66.4(3) . . . . ? N2 C9 C10 C11 -0.4(4) . . . . ? C8 C9 C10 C11 176.8(2) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? C9 N2 C13 C12 0.1(4) . . . . ? C11 C12 C13 N2 0.2(4) . . . . ? C8 N1 C14 C15 -157.66(17) . . . . ? S1 N1 C14 C15 61.1(2) . . . . ? C19 N3 C15 C16 0.9(3) . . . . ? C19 N3 C15 C14 -179.82(19) . . . . ? N1 C14 C15 N3 61.7(2) . . . . ? N1 C14 C15 C16 -119.1(2) . . . . ? N3 C15 C16 C17 -0.5(3) . . . . ? C14 C15 C16 C17 -179.72(19) . . . . ? C15 C16 C17 C18 -0.3(3) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C15 N3 C19 C18 -0.6(3) . . . . ? C17 C18 C19 N3 -0.1(4) . . . . ? C26 N4 C20 C21 -125.27(16) . . . . ? S2 N4 C20 C21 97.14(16) . . . . ? C25 N5 C21 C22 0.3(3) . . . . ? C25 N5 C21 C20 -177.42(17) . . . . ? N4 C20 C21 N5 -19.8(2) . . . . ? N4 C20 C21 C22 162.54(16) . . . . ? N5 C21 C22 C23 -0.1(3) . . . . ? C20 C21 C22 C23 177.56(18) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? C21 N5 C25 C24 0.1(3) . . . . ? C23 C24 C25 N5 -0.7(3) . . . . ? C20 N4 C26 C27 80.25(19) . . . . ? S2 N4 C26 C27 -141.46(13) . . . . ? C31 N6 C27 C28 0.6(3) . . . . ? C31 N6 C27 C26 -174.99(17) . . . . ? N4 C26 C27 N6 -118.85(18) . . . . ? N4 C26 C27 C28 65.5(2) . . . . ? N6 C27 C28 C29 -1.5(3) . . . . ? C26 C27 C28 C29 173.92(19) . . . . ? C27 C28 C29 C30 0.9(3) . . . . ? C28 C29 C30 C31 0.4(3) . . . . ? C27 N6 C31 C30 0.9(3) . . . . ? C29 C30 C31 N6 -1.4(4) . . . . ? 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 O1 H1 N5 0.86 1.67 2.4819(19) 156.1 . N5 H5 O1 0.88 1.67 2.4819(19) 152.6 . #======================================================================= data_psmsp _database_code_depnum_ccdc_archive 'CCDC 737970' _chemical_name_systematic ; 2-hydroxy-3-(N,N-bis-(2-pyridylmethyl)-sulfonamido)- 5-methylbenzenesulfonic acid ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H19 N3 O6 S2, C H Cl3' _chemical_formula_sum 'C20 H20 Cl3 N3 O6 S2' _chemical_formula_weight 568.86 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' Cl Cl 0.1484 0.1585 '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 8.1135(9) _cell_length_b 11.9046(17) _cell_length_c 13.1532(19) _cell_angle_alpha 72.956(5) _cell_angle_beta 87.292(6) _cell_angle_gamma 89.602(4) _cell_volume 1213.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1523 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 23.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The molecular and intermolecular geometry requires the molecule to be a zwitterion: SO3^-^ and NH^+^. There is no place for an H atom in the vicinity of the SO3^-^ group and there must be an H atom mediating the interaction between the N atoms of the pyridyl rings. This H atom was NOT evident in difference Fourier maps: it is placed in the most chemically reasonable position. The H atom of theOH group was placed geometrically and allowed to rotate about the OH bond to the position of maximum electron density (AFIX 147). The highest residual peak is associated with the chloroform molecule. The crystals decompose on removal from mother liquor (presumably on account of loss of chloroform). The crystal was transferred directly from mother liquour to polyfluoroether oil, then transferred rapidly into the N2 stream after mounting. The crystal was then stable for the duration of the data collection. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 8967 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.12 _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.920 _reflns_number_total 4856 _reflns_number_gt 2748 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.1411P)^2^+3.1282P] 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 4856 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1594 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2857 _refine_ls_wR_factor_gt 0.2488 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.991 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.120 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 S1 S 0.1041(2) 0.58382(13) 0.79762(12) 0.0277(4) Uani 1 1 d . . . S2 S -0.2956(2) 0.72595(14) 0.45129(13) 0.0330(5) Uani 1 1 d . . . O1 O -0.0536(7) 0.7600(4) 0.6151(4) 0.0397(12) Uani 1 1 d . . . H1 H -0.0967 0.8054 0.5617 0.060 Uiso 1 1 calc R . . O11 O 0.0310(6) 0.6754(4) 0.8340(4) 0.0354(11) Uani 1 1 d . . . O12 O 0.1335(6) 0.4724(4) 0.8727(3) 0.0358(11) Uani 1 1 d . . . O21 O -0.4597(8) 0.7204(6) 0.4854(5) 0.081(2) Uani 1 1 d . . . O22 O -0.2677(8) 0.7005(5) 0.3524(4) 0.0563(16) Uani 1 1 d . . . O23 O -0.2161(8) 0.8375(4) 0.4461(5) 0.0608(18) Uani 1 1 d . . . N1 N 0.2856(7) 0.6304(4) 0.7427(4) 0.0292(12) Uani 1 1 d . . . N2 N 0.5575(7) 0.7685(5) 0.7613(6) 0.0439(16) Uani 1 1 d . . . N3 N 0.5814(7) 0.5381(5) 0.8476(4) 0.0301(12) Uani 1 1 d . . . H3B H 0.5724 0.6151 0.8279 0.036 Uiso 1 1 calc R . . C1 C -0.0887(8) 0.6476(5) 0.6205(5) 0.0282(14) Uani 1 1 d . . . C2 C -0.0208(8) 0.5551(5) 0.7004(5) 0.0270(14) Uani 1 1 d . . . C3 C -0.0505(8) 0.4392(6) 0.7061(5) 0.0303(14) Uani 1 1 d . . . H3A H -0.0014 0.3787 0.7600 0.036 Uiso 1 1 calc R . . C4 C -0.1494(9) 0.4092(6) 0.6358(5) 0.0340(15) Uani 1 1 d . . . C5 C -0.2210(8) 0.4994(6) 0.5588(5) 0.0311(15) Uani 1 1 d . . . H5A H -0.2919 0.4805 0.5106 0.037 Uiso 1 1 calc R . . C6 C -0.1916(8) 0.6170(5) 0.5504(5) 0.0290(14) Uani 1 1 d . . . C7 C -0.1841(10) 0.2829(6) 0.6430(6) 0.0411(18) Uani 1 1 d . . . H7A H -0.0850 0.2361 0.6644 0.062 Uiso 1 1 calc R . . H7B H -0.2152 0.2778 0.5734 0.062 Uiso 1 1 calc R . . H7C H -0.2746 0.2528 0.6958 0.062 Uiso 1 1 calc R . . C8 C 0.3014(9) 0.7526(5) 0.6747(6) 0.0372(16) Uani 1 1 d . . . H8A H 0.1982 0.7943 0.6836 0.045 Uiso 1 1 calc R . . H8B H 0.3117 0.7521 0.5995 0.045 Uiso 1 1 calc R . . C9 C 0.4428(9) 0.8209(6) 0.6951(6) 0.0370(16) Uani 1 1 d . . . C10 C 0.4535(9) 0.9395(6) 0.6412(8) 0.051(2) Uani 1 1 d . . . H10A H 0.3713 0.9761 0.5936 0.061 Uiso 1 1 calc R . . C11 C 0.5849(11) 1.0041(7) 0.6573(10) 0.076(3) Uani 1 1 d . . . H11A H 0.5938 1.0858 0.6218 0.092 Uiso 1 1 calc R . . C12 C 0.7005(13) 0.9492(7) 0.7241(12) 0.101(5) Uani 1 1 d . . . H12A H 0.7930 0.9919 0.7353 0.121 Uiso 1 1 calc R . . C13 C 0.6844(11) 0.8323(7) 0.7757(10) 0.071(3) Uani 1 1 d . . . H13A H 0.7661 0.7949 0.8234 0.086 Uiso 1 1 calc R . . C14 C 0.3891(8) 0.5412(5) 0.7121(5) 0.0305(14) Uani 1 1 d . . . H14A H 0.4614 0.5808 0.6492 0.037 Uiso 1 1 calc R . . H14B H 0.3169 0.4854 0.6919 0.037 Uiso 1 1 calc R . . C15 C 0.4935(8) 0.4746(5) 0.8004(5) 0.0284(14) Uani 1 1 d . . . C16 C 0.5059(9) 0.3535(6) 0.8323(6) 0.0390(17) Uani 1 1 d . . . H16A H 0.4437 0.3075 0.7995 0.047 Uiso 1 1 calc R . . C17 C 0.6100(9) 0.3000(6) 0.9125(6) 0.0429(18) Uani 1 1 d . . . H17A H 0.6183 0.2168 0.9352 0.051 Uiso 1 1 calc R . . C18 C 0.7016(9) 0.3660(6) 0.9598(6) 0.0412(18) Uani 1 1 d . . . H18A H 0.7744 0.3303 1.0144 0.049 Uiso 1 1 calc R . . C19 C 0.6830(8) 0.4860(6) 0.9245(5) 0.0347(16) Uani 1 1 d . . . H19A H 0.7446 0.5336 0.9559 0.042 Uiso 1 1 calc R . . C20 C 0.1917(13) 1.0648(7) 0.8372(8) 0.066(3) Uani 1 1 d . . . H20A H 0.2130 1.1139 0.7618 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.1127(3) 0.9289(2) 0.8352(2) 0.0630(7) Uani 1 1 d . . . Cl2 Cl 0.3815(6) 1.0389(3) 0.8980(4) 0.145(2) Uani 1 1 d . . . Cl3 Cl 0.0570(6) 1.1390(2) 0.8975(3) 0.1378(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0245(10) 0.0291(8) 0.0285(8) -0.0053(6) -0.0115(6) -0.0004(6) S2 0.0279(11) 0.0374(9) 0.0323(9) -0.0067(7) -0.0129(7) 0.0085(7) O1 0.050(3) 0.024(2) 0.045(3) -0.005(2) -0.026(2) 0.003(2) O11 0.037(3) 0.038(3) 0.035(3) -0.014(2) -0.013(2) 0.009(2) O12 0.041(3) 0.034(3) 0.029(2) -0.002(2) -0.014(2) 0.001(2) O21 0.044(4) 0.094(5) 0.073(4) 0.024(4) -0.010(3) 0.023(3) O22 0.086(5) 0.050(3) 0.032(3) -0.006(2) -0.020(3) 0.023(3) O23 0.085(5) 0.032(3) 0.065(4) -0.007(3) -0.048(3) 0.015(3) N1 0.028(3) 0.021(3) 0.037(3) -0.004(2) -0.012(2) 0.005(2) N2 0.030(4) 0.031(3) 0.072(5) -0.015(3) -0.018(3) 0.003(2) N3 0.027(3) 0.029(3) 0.033(3) -0.006(2) -0.010(2) 0.003(2) C1 0.022(4) 0.028(3) 0.035(3) -0.009(3) -0.010(3) 0.002(2) C2 0.023(4) 0.031(3) 0.028(3) -0.007(3) -0.010(3) 0.001(2) C3 0.023(4) 0.031(3) 0.033(3) -0.003(3) -0.004(3) 0.000(3) C4 0.034(4) 0.032(3) 0.037(4) -0.011(3) -0.004(3) -0.004(3) C5 0.025(4) 0.038(4) 0.034(3) -0.014(3) -0.012(3) 0.001(3) C6 0.027(4) 0.028(3) 0.032(3) -0.008(3) -0.012(3) 0.003(3) C7 0.045(5) 0.027(3) 0.053(5) -0.012(3) -0.014(4) -0.008(3) C8 0.038(5) 0.026(3) 0.042(4) -0.001(3) -0.011(3) 0.001(3) C9 0.031(4) 0.029(3) 0.050(4) -0.009(3) -0.004(3) 0.006(3) C10 0.024(4) 0.036(4) 0.086(6) -0.008(4) -0.007(4) 0.003(3) C11 0.039(6) 0.028(4) 0.148(10) -0.001(5) -0.023(6) -0.001(3) C12 0.056(7) 0.035(5) 0.218(15) -0.035(7) -0.068(8) 0.006(4) C13 0.040(6) 0.036(4) 0.141(10) -0.024(5) -0.043(6) 0.006(4) C14 0.026(4) 0.030(3) 0.032(3) -0.003(3) -0.011(3) 0.002(3) C15 0.024(4) 0.032(3) 0.027(3) -0.004(3) -0.004(3) 0.000(3) C16 0.043(5) 0.031(4) 0.040(4) -0.005(3) -0.011(3) 0.001(3) C17 0.039(5) 0.026(3) 0.056(5) 0.003(3) -0.015(4) 0.003(3) C18 0.044(5) 0.041(4) 0.033(4) 0.000(3) -0.018(3) 0.006(3) C19 0.026(4) 0.043(4) 0.034(4) -0.009(3) -0.010(3) 0.001(3) C20 0.097(8) 0.029(4) 0.064(6) 0.005(4) -0.021(5) 0.003(4) Cl1 0.0625(16) 0.0637(14) 0.0676(15) -0.0268(11) -0.0012(11) -0.0127(11) Cl2 0.167(4) 0.071(2) 0.180(4) 0.007(2) -0.124(3) -0.031(2) Cl3 0.271(5) 0.0502(15) 0.073(2) 0.0037(14) 0.042(3) 0.043(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O11 1.428(5) . ? S1 O12 1.429(4) . ? S1 N1 1.635(6) . ? S1 C2 1.779(6) . ? S2 O21 1.381(7) . ? S2 O22 1.428(5) . ? S2 O23 1.463(6) . ? S2 C6 1.786(6) . ? O1 C1 1.350(7) . ? O1 H1 0.840 . ? N1 C8 1.470(8) . ? N1 C14 1.484(8) . ? N2 C9 1.329(9) . ? N2 C13 1.336(10) . ? N3 C19 1.338(8) . ? N3 C15 1.339(8) . ? N3 H3B 0.880 . ? C1 C6 1.397(9) . ? C1 C2 1.410(8) . ? C2 C3 1.381(9) . ? C3 C4 1.377(9) . ? C3 H3A 0.950 . ? C4 C5 1.388(9) . ? C4 C7 1.505(9) . ? C5 C6 1.394(9) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.490(10) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.383(10) . ? C10 C11 1.379(12) . ? C10 H10A 0.950 . ? C11 C12 1.346(14) . ? C11 H11A 0.950 . ? C12 C13 1.362(13) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.497(9) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.383(9) . ? C16 C17 1.384(10) . ? C16 H16A 0.950 . ? C17 C18 1.376(10) . ? C17 H17A 0.950 . ? C18 C19 1.376(10) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 Cl3 1.709(10) . ? C20 Cl1 1.752(9) . ? C20 Cl2 1.753(10) . ? C20 H20A 1.000 . ? 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 O11 S1 O12 119.3(3) . . ? O11 S1 N1 107.6(3) . . ? O12 S1 N1 105.1(3) . . ? O11 S1 C2 109.2(3) . . ? O12 S1 C2 106.2(3) . . ? N1 S1 C2 109.2(3) . . ? O21 S2 O22 113.6(4) . . ? O21 S2 O23 113.2(4) . . ? O22 S2 O23 109.8(4) . . ? O21 S2 C6 106.5(3) . . ? O22 S2 C6 107.7(3) . . ? O23 S2 C6 105.4(3) . . ? C1 O1 H1 109.5 . . ? C8 N1 C14 117.3(5) . . ? C8 N1 S1 118.3(4) . . ? C14 N1 S1 115.2(4) . . ? C9 N2 C13 119.0(7) . . ? C19 N3 C15 120.8(6) . . ? C19 N3 H3B 119.6 . . ? C15 N3 H3B 119.6 . . ? O1 C1 C6 123.1(6) . . ? O1 C1 C2 119.6(6) . . ? C6 C1 C2 117.3(6) . . ? C3 C2 C1 121.0(6) . . ? C3 C2 S1 117.9(5) . . ? C1 C2 S1 121.1(5) . . ? C4 C3 C2 121.6(6) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 117.9(6) . . ? C3 C4 C7 121.7(6) . . ? C5 C4 C7 120.4(6) . . ? C4 C5 C6 121.6(6) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 120.5(6) . . ? C5 C6 S2 117.9(5) . . ? C1 C6 S2 121.6(5) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 115.9(5) . . ? N1 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? N1 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? N2 C9 C10 121.0(7) . . ? N2 C9 C8 120.8(6) . . ? C10 C9 C8 118.2(6) . . ? C11 C10 C9 119.3(8) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 118.9(8) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 119.8(8) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? N2 C13 C12 122.1(8) . . ? N2 C13 H13A 118.9 . . ? C12 C13 H13A 118.9 . . ? N1 C14 C15 112.2(5) . . ? N1 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N1 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N3 C15 C16 119.7(6) . . ? N3 C15 C14 116.8(5) . . ? C16 C15 C14 123.5(6) . . ? C15 C16 C17 119.2(6) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C19 C18 C17 117.0(6) . . ? C19 C18 H18A 121.5 . . ? C17 C18 H18A 121.5 . . ? N3 C19 C18 122.5(6) . . ? N3 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? Cl3 C20 Cl1 112.6(6) . . ? Cl3 C20 Cl2 112.7(6) . . ? Cl1 C20 Cl2 107.6(4) . . ? Cl3 C20 H20A 107.9 . . ? Cl1 C20 H20A 107.9 . . ? Cl2 C20 H20A 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 S1 N1 C8 -41.4(5) . . . . ? O12 S1 N1 C8 -169.6(5) . . . . ? C2 S1 N1 C8 76.9(5) . . . . ? O11 S1 N1 C14 172.6(4) . . . . ? O12 S1 N1 C14 44.5(5) . . . . ? C2 S1 N1 C14 -69.0(5) . . . . ? O1 C1 C2 C3 -178.1(6) . . . . ? C6 C1 C2 C3 2.3(10) . . . . ? O1 C1 C2 S1 2.5(9) . . . . ? C6 C1 C2 S1 -177.1(5) . . . . ? O11 S1 C2 C3 -136.5(5) . . . . ? O12 S1 C2 C3 -6.7(6) . . . . ? N1 S1 C2 C3 106.2(5) . . . . ? O11 S1 C2 C1 42.9(6) . . . . ? O12 S1 C2 C1 172.7(5) . . . . ? N1 S1 C2 C1 -74.4(6) . . . . ? C1 C2 C3 C4 -1.2(10) . . . . ? S1 C2 C3 C4 178.2(5) . . . . ? C2 C3 C4 C5 -0.8(11) . . . . ? C2 C3 C4 C7 -179.0(7) . . . . ? C3 C4 C5 C6 1.6(11) . . . . ? C7 C4 C5 C6 179.8(7) . . . . ? C4 C5 C6 C1 -0.4(11) . . . . ? C4 C5 C6 S2 -177.9(6) . . . . ? O1 C1 C6 C5 178.9(6) . . . . ? C2 C1 C6 C5 -1.5(10) . . . . ? O1 C1 C6 S2 -3.7(10) . . . . ? C2 C1 C6 S2 176.0(5) . . . . ? O21 S2 C6 C5 71.0(7) . . . . ? O22 S2 C6 C5 -51.3(6) . . . . ? O23 S2 C6 C5 -168.5(6) . . . . ? O21 S2 C6 C1 -106.5(7) . . . . ? O22 S2 C6 C1 131.2(6) . . . . ? O23 S2 C6 C1 14.0(7) . . . . ? C14 N1 C8 C9 -82.2(7) . . . . ? S1 N1 C8 C9 132.6(6) . . . . ? C13 N2 C9 C10 0.2(12) . . . . ? C13 N2 C9 C8 178.5(8) . . . . ? N1 C8 C9 N2 8.3(10) . . . . ? N1 C8 C9 C10 -173.4(7) . . . . ? N2 C9 C10 C11 -0.5(13) . . . . ? C8 C9 C10 C11 -178.8(8) . . . . ? C9 C10 C11 C12 0.9(16) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? C9 N2 C13 C12 -0.4(16) . . . . ? C11 C12 C13 N2 1(2) . . . . ? C8 N1 C14 C15 124.3(6) . . . . ? S1 N1 C14 C15 -89.4(6) . . . . ? C19 N3 C15 C16 0.8(10) . . . . ? C19 N3 C15 C14 -177.4(6) . . . . ? N1 C14 C15 N3 -49.6(8) . . . . ? N1 C14 C15 C16 132.2(7) . . . . ? N3 C15 C16 C17 -0.2(10) . . . . ? C14 C15 C16 C17 177.9(7) . . . . ? C15 C16 C17 C18 -0.6(12) . . . . ? C16 C17 C18 C19 0.7(12) . . . . ? C15 N3 C19 C18 -0.7(10) . . . . ? C17 C18 C19 N3 -0.1(11) . . . . ? #======================================================================= data_1 _database_code_depnum_ccdc_archive 'CCDC 737971' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 70 % : (C32 H34 N6 O7 S2 V 2+), (Cl O4 -)2, (C H4 O)2, H2 O 30 % : (C31 H32 N6 O7 S2 V 2+), (Cl O4 -)2, (C H4 O)2, 2(H2 O) ; _chemical_formula_sum 'C33.70 H44 Cl2 N6 O18.30 S2 V' _chemical_formula_weight 1011.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9275(11) _cell_length_b 25.6124(17) _cell_length_c 14.0430(10) _cell_angle_alpha 90.00 _cell_angle_beta 119.576(3) _cell_angle_gamma 90.00 _cell_volume 4356.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9832 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.25 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2094 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Disorder between H2O and CH2OH bound to the V centre: In 70% of the molecules, CH3OH is bound to V. In 30% of the molecules, H2O is bound to V. Where H2O is bound to V, there is also a lattice water molecule bound to this H2O (making two lattice water molecules per complex). Where CH3OH is bound to V, this lattice water molecule is not there (so that there is only one lattice water molecule per complex). H atoms were placed so as to form a reasonable H-bond network then allowed to ride with constrained displacement parameters. All CH3 groups were allowed to rotate about their local 3-fold axes (AFIX 137). The perchlorate anions were restrained to have tetrahedral geometry, with all Cl---O and all O...O distances restrained to a common refined value and 1.633 times that value, respectively. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 86785 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 8891 _reflns_number_gt 6006 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0692P)^2^+3.3202P] 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 8891 _refine_ls_number_parameters 613 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.894 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.073 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 V1 V 0.90988(4) 0.097661(19) 0.31361(4) 0.02229(15) Uani 1 1 d . . . S1 S 0.73549(7) 0.08617(3) 0.51108(7) 0.0274(2) Uani 1 1 d . . . S2 S 0.87051(7) 0.23022(3) 0.31595(7) 0.0302(2) Uani 1 1 d . . . O1 O 0.80206(17) 0.12486(8) 0.34996(16) 0.0243(5) Uani 1 1 d . . . O2 O 0.91172(19) 0.03633(8) 0.32901(18) 0.0323(5) Uani 1 1 d . . . O11 O 0.7026(2) 0.08987(9) 0.59257(19) 0.0368(6) Uani 1 1 d . . . O12 O 0.80940(19) 0.04539(9) 0.5198(2) 0.0357(6) Uani 1 1 d . . . O21 O 0.7721(2) 0.22048(9) 0.21466(19) 0.0368(6) Uani 1 1 d . . . O22 O 0.9154(2) 0.28180(8) 0.3363(2) 0.0424(6) Uani 1 1 d . . . N1 N 0.6224(2) 0.07802(10) 0.3940(2) 0.0278(6) Uani 1 1 d . . . N2 N 0.4889(2) -0.01121(11) 0.3044(2) 0.0286(6) Uani 1 1 d . . . H2A H 0.4754 0.0126 0.3413 0.034 Uiso 1 1 calc R . . N3 N 0.4252(2) 0.06061(11) 0.4069(2) 0.0323(7) Uani 1 1 d . . . N4 N 0.9658(2) 0.18698(9) 0.3197(2) 0.0234(6) Uani 1 1 d . . . N5 N 1.0228(2) 0.10054(10) 0.2544(2) 0.0279(6) Uani 1 1 d . A . N6 N 1.0340(2) 0.11157(9) 0.4783(2) 0.0226(6) Uani 1 1 d . A . C1 C 0.8154(2) 0.15950(12) 0.4249(2) 0.0243(7) Uani 1 1 d . . . C2 C 0.7895(3) 0.14839(12) 0.5078(3) 0.0277(7) Uani 1 1 d . . . C3 C 0.8014(3) 0.18558(14) 0.5844(3) 0.0396(9) Uani 1 1 d . . . H3A H 0.7808 0.1770 0.6378 0.047 Uiso 1 1 calc R A . C4 C 0.8426(4) 0.23518(15) 0.5853(3) 0.0472(10) Uani 1 1 d . . . C5 C 0.8685(3) 0.24696(13) 0.5052(3) 0.0393(9) Uani 1 1 d . . . H5A H 0.8961 0.2806 0.5036 0.047 Uiso 1 1 calc R A . C6 C 0.8546(3) 0.21017(12) 0.4264(3) 0.0270(7) Uani 1 1 d . . . C7 C 0.8529(5) 0.27559(19) 0.6681(4) 0.0804(17) Uani 1 1 d . . . H7A H 0.8422 0.3105 0.6358 0.121 Uiso 1 1 calc R A . H7B H 0.9264 0.2734 0.7329 0.121 Uiso 1 1 calc R . . H7C H 0.7966 0.2692 0.6894 0.121 Uiso 1 1 calc R . . C8 C 0.6268(3) 0.04972(13) 0.3053(3) 0.0340(8) Uani 1 1 d . . . H8A H 0.7051 0.0433 0.3270 0.041 Uiso 1 1 calc R . . H8B H 0.5948 0.0721 0.2392 0.041 Uiso 1 1 calc R . . C9 C 0.5662(3) -0.00182(13) 0.2767(2) 0.0279(7) Uani 1 1 d . . . C10 C 0.5872(3) -0.03908(15) 0.2193(3) 0.0416(9) Uani 1 1 d . . . H10A H 0.6418 -0.0329 0.1988 0.050 Uiso 1 1 calc R . . C11 C 0.5292(4) -0.08554(16) 0.1912(3) 0.0492(10) Uani 1 1 d . . . H11A H 0.5437 -0.1115 0.1516 0.059 Uiso 1 1 calc R . . C12 C 0.4503(4) -0.09370(16) 0.2211(3) 0.0498(10) Uani 1 1 d . . . H12A H 0.4096 -0.1254 0.2024 0.060 Uiso 1 1 calc R . . C13 C 0.4309(3) -0.05604(14) 0.2775(3) 0.0383(9) Uani 1 1 d . . . H13A H 0.3762 -0.0613 0.2982 0.046 Uiso 1 1 calc R . . C14 C 0.5363(3) 0.11881(13) 0.3650(3) 0.0354(8) Uani 1 1 d . . . H14A H 0.4895 0.1202 0.2843 0.042 Uiso 1 1 calc R . . H14B H 0.5728 0.1532 0.3897 0.042 Uiso 1 1 calc R . . C15 C 0.4641(3) 0.10937(13) 0.4148(3) 0.0337(8) Uani 1 1 d . . . C16 C 0.4357(3) 0.14907(15) 0.4622(4) 0.0485(10) Uani 1 1 d . . . H16A H 0.4651 0.1831 0.4681 0.058 Uiso 1 1 calc R . . C17 C 0.3638(3) 0.13872(17) 0.5010(4) 0.0535(11) Uani 1 1 d . . . H17A H 0.3425 0.1658 0.5330 0.064 Uiso 1 1 calc R . . C18 C 0.3235(3) 0.08913(17) 0.4932(3) 0.0458(10) Uani 1 1 d . . . H18A H 0.2743 0.0811 0.5197 0.055 Uiso 1 1 calc R . . C19 C 0.3563(3) 0.05131(15) 0.4455(3) 0.0383(9) Uani 1 1 d . . . H19A H 0.3286 0.0169 0.4398 0.046 Uiso 1 1 calc R . . C20 C 0.9748(3) 0.19216(12) 0.2184(3) 0.0304(8) Uani 1 1 d . . . H20A H 1.0151 0.2245 0.2215 0.036 Uiso 1 1 calc R A . H20B H 0.9003 0.1938 0.1530 0.036 Uiso 1 1 calc R . . C21 C 1.0360(3) 0.14545(13) 0.2116(3) 0.0316(8) Uani 1 1 d . A . C22 C 1.1007(3) 0.14817(16) 0.1628(3) 0.0418(9) Uani 1 1 d . . . H22A H 1.1097 0.1803 0.1343 0.050 Uiso 1 1 calc R A . C23 C 1.1523(3) 0.10347(18) 0.1559(3) 0.0506(11) Uani 1 1 d . . . H23A H 1.1965 0.1045 0.1217 0.061 Uiso 1 1 calc R . . C24 C 1.1393(3) 0.05774(17) 0.1986(3) 0.0462(10) Uani 1 1 d . . . H24A H 1.1743 0.0267 0.1942 0.055 Uiso 1 1 calc R A . C25 C 1.0751(3) 0.05728(14) 0.2477(3) 0.0374(8) Uani 1 1 d . A . H25A H 1.0671 0.0255 0.2780 0.045 Uiso 1 1 calc R . . C26 C 1.0750(3) 0.19394(12) 0.4206(3) 0.0290(7) Uani 1 1 d . . . H26A H 1.0813 0.2303 0.4472 0.035 Uiso 1 1 calc R A . H26B H 1.1345 0.1881 0.4026 0.035 Uiso 1 1 calc R . . C27 C 1.0898(2) 0.15689(11) 0.5096(3) 0.0251(7) Uani 1 1 d . A . C28 C 1.1614(3) 0.16811(13) 0.6178(3) 0.0363(8) Uani 1 1 d . . . H28A H 1.1996 0.2005 0.6375 0.044 Uiso 1 1 calc R A . C29 C 1.1778(3) 0.13254(14) 0.6972(3) 0.0416(9) Uani 1 1 d . . . H29A H 1.2275 0.1398 0.7722 0.050 Uiso 1 1 calc R . . C30 C 1.1205(3) 0.08585(13) 0.6662(3) 0.0348(8) Uani 1 1 d . . . H30A H 1.1298 0.0605 0.7194 0.042 Uiso 1 1 calc R A . C31 C 1.0501(3) 0.07687(12) 0.5573(3) 0.0275(7) Uani 1 1 d . A . H31A H 1.0109 0.0448 0.5363 0.033 Uiso 1 1 calc R . . C100 C 0.6779(5) 0.1129(3) 0.1002(5) 0.0552(16) Uani 0.70 1 d P A 1 H103 H 0.6534 0.1353 0.0357 0.083 Uiso 0.70 1 calc PR A 1 H102 H 0.6565 0.1288 0.1505 0.083 Uiso 0.70 1 calc PR A 1 H101 H 0.6433 0.0785 0.0774 0.083 Uiso 0.70 1 calc PR A 1 O100 O 0.79736(18) 0.10730(9) 0.15512(17) 0.0331(5) Uani 0.70 1 d P A 1 H100 H 0.8021 0.0875 0.1090 0.040 Uiso 0.70 1 d PR A 1 O1W O 0.79736(18) 0.10730(9) 0.15512(17) 0.0331(5) Uani 0.30 1 d P A 2 H1W H 0.8021 0.0875 0.1090 0.050 Uiso 0.30 1 d PR A 2 H2W H 0.7332 0.1198 0.1327 0.050 Uiso 0.30 1 d PR A 2 O2W O 0.5945(10) 0.1469(4) 0.0860(9) 0.073(3) Uiso 0.30 1 d P B 2 H3W H 0.6270 0.1581 0.0523 0.109 Uiso 0.30 1 d PR B 2 H4W H 0.5270 0.1379 0.0551 0.109 Uiso 0.30 1 d PR B 2 Cl1 Cl 0.77949(8) 0.20977(3) 0.88687(7) 0.0381(2) Uani 1 1 d D . . O1A O 0.7387(3) 0.25912(11) 0.8381(3) 0.0664(9) Uani 1 1 d D . . O1B O 0.7589(3) 0.17326(12) 0.8028(3) 0.0823(11) Uani 1 1 d D . . O1C O 0.7277(3) 0.19287(13) 0.9461(3) 0.0776(10) Uani 1 1 d D . . O1D O 0.8954(3) 0.21372(17) 0.9580(3) 0.0976(13) Uani 1 1 d D . . Cl2 Cl 0.66161(8) -0.07344(4) -0.01506(8) 0.0485(3) Uani 1 1 d D . . O2A O 0.6413(10) -0.0757(4) -0.1224(6) 0.075(4) Uani 0.50 1 d PD C 1 O2B O 0.6271(9) -0.1174(3) 0.0174(7) 0.103(3) Uani 0.50 1 d PD C 1 O2C O 0.7695(6) -0.0610(5) 0.0582(7) 0.137(5) Uani 0.50 1 d PD C 1 O2D O 0.5899(11) -0.0319(4) -0.0140(8) 0.146(6) Uani 0.50 1 d PD C 1 O2E O 0.7349(9) -0.1181(3) 0.0185(7) 0.115(3) Uani 0.50 1 d PD C 2 O2F O 0.5585(5) -0.0860(6) -0.0340(7) 0.201(9) Uani 0.50 1 d PD C 2 O2G O 0.6612(10) -0.0507(4) -0.1064(7) 0.081(4) Uani 0.50 1 d PD C 2 O2H O 0.7148(9) -0.0383(4) 0.0732(7) 0.095(3) Uani 0.50 1 d PD C 2 O3W O 0.8328(3) 0.04577(12) 0.0312(2) 0.0620(8) Uani 1 1 d . . . H5W H 0.8146 0.0151 0.0393 0.093 Uiso 1 1 d R . . H6W H 0.8408 0.0548 -0.0228 0.093 Uiso 1 1 d R . . O1S O 0.8590(3) 0.07342(11) 0.8587(2) 0.0616(8) Uani 1 1 d . . . H1S H 0.8291 0.1034 0.8419 0.092 Uiso 1 1 d R . . C1S C 0.9612(4) 0.0773(2) 0.8621(4) 0.0707(14) Uani 1 1 d . . . H1S1 H 1.0007 0.1082 0.9043 0.106 Uiso 1 1 calc R . . H1S2 H 0.9491 0.0803 0.7873 0.106 Uiso 1 1 calc R . . H1S3 H 1.0053 0.0460 0.8969 0.106 Uiso 1 1 calc R . . O2S O 0.0665(5) 0.2418(2) 0.9262(5) 0.161(2) Uani 1 1 d . . . H2S H 0.0130 0.2332 0.9359 0.241 Uiso 1 1 d R . . C2S C 0.0974(8) 0.2107(4) 0.8581(9) 0.169(4) Uani 1 1 d . . . H2S1 H 0.1390 0.2325 0.8337 0.254 Uiso 1 1 calc R . . H2S2 H 0.0306 0.1976 0.7942 0.254 Uiso 1 1 calc R . . H2S3 H 0.1434 0.1812 0.9008 0.254 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 V1 0.0263(3) 0.0175(3) 0.0237(3) -0.0010(2) 0.0127(2) -0.0015(2) S1 0.0295(4) 0.0282(4) 0.0282(4) 0.0047(3) 0.0170(4) -0.0038(3) S2 0.0436(5) 0.0173(4) 0.0423(5) 0.0083(4) 0.0308(4) 0.0068(3) O1 0.0298(12) 0.0217(11) 0.0251(12) -0.0006(9) 0.0163(10) -0.0025(9) O2 0.0406(14) 0.0182(11) 0.0346(13) -0.0044(9) 0.0158(11) -0.0025(10) O11 0.0437(15) 0.0439(15) 0.0312(13) 0.0029(11) 0.0249(12) -0.0103(11) O12 0.0331(13) 0.0304(13) 0.0453(15) 0.0103(11) 0.0207(12) 0.0015(10) O21 0.0399(14) 0.0345(13) 0.0402(14) 0.0151(11) 0.0230(12) 0.0138(11) O22 0.0654(17) 0.0178(12) 0.0651(18) 0.0066(11) 0.0483(15) 0.0025(11) N1 0.0279(15) 0.0280(15) 0.0304(15) 0.0007(12) 0.0167(13) -0.0032(11) N2 0.0281(15) 0.0329(16) 0.0227(14) 0.0012(12) 0.0109(12) -0.0006(12) N3 0.0288(15) 0.0341(16) 0.0352(16) 0.0100(13) 0.0168(13) 0.0028(12) N4 0.0296(14) 0.0195(13) 0.0268(14) 0.0039(11) 0.0184(12) 0.0032(11) N5 0.0295(15) 0.0267(15) 0.0298(15) -0.0058(12) 0.0164(13) -0.0002(11) N6 0.0251(14) 0.0167(13) 0.0268(14) -0.0010(11) 0.0134(12) -0.0002(10) C1 0.0252(17) 0.0248(17) 0.0239(17) 0.0051(13) 0.0128(14) 0.0043(13) C2 0.0319(18) 0.0270(17) 0.0295(18) 0.0026(14) 0.0192(15) -0.0031(14) C3 0.055(2) 0.039(2) 0.038(2) -0.0032(17) 0.0325(19) -0.0075(18) C4 0.070(3) 0.037(2) 0.054(2) -0.0150(18) 0.046(2) -0.0128(19) C5 0.055(2) 0.0243(18) 0.054(2) -0.0060(16) 0.039(2) -0.0060(16) C6 0.0373(19) 0.0194(16) 0.0362(19) 0.0040(14) 0.0271(16) 0.0039(14) C7 0.140(5) 0.055(3) 0.086(4) -0.033(3) 0.086(4) -0.037(3) C8 0.038(2) 0.038(2) 0.0324(19) -0.0008(15) 0.0221(17) -0.0085(16) C9 0.0277(17) 0.0340(18) 0.0212(17) 0.0014(14) 0.0114(14) -0.0022(14) C10 0.043(2) 0.049(2) 0.039(2) -0.0038(18) 0.0255(19) -0.0051(18) C11 0.061(3) 0.047(2) 0.048(2) -0.0158(19) 0.034(2) -0.010(2) C12 0.057(3) 0.044(2) 0.048(2) -0.0129(19) 0.025(2) -0.020(2) C13 0.035(2) 0.043(2) 0.036(2) -0.0007(17) 0.0173(17) -0.0116(16) C14 0.0346(19) 0.0305(19) 0.043(2) 0.0096(16) 0.0203(17) 0.0032(15) C15 0.0270(18) 0.033(2) 0.039(2) 0.0115(15) 0.0139(16) 0.0075(15) C16 0.047(2) 0.035(2) 0.069(3) 0.0054(19) 0.033(2) 0.0081(18) C17 0.051(3) 0.055(3) 0.063(3) 0.000(2) 0.034(2) 0.017(2) C18 0.035(2) 0.060(3) 0.046(2) 0.017(2) 0.0235(19) 0.0148(19) C19 0.0306(19) 0.045(2) 0.039(2) 0.0129(17) 0.0174(17) 0.0038(16) C20 0.041(2) 0.0270(18) 0.0340(19) 0.0042(14) 0.0273(17) -0.0008(15) C21 0.0317(18) 0.038(2) 0.0300(18) -0.0049(15) 0.0191(16) -0.0023(15) C22 0.044(2) 0.052(2) 0.043(2) -0.0035(18) 0.0316(19) -0.0041(18) C23 0.045(2) 0.072(3) 0.051(3) -0.016(2) 0.036(2) -0.003(2) C24 0.038(2) 0.056(3) 0.046(2) -0.018(2) 0.0206(19) 0.0073(19) C25 0.036(2) 0.035(2) 0.038(2) -0.0107(16) 0.0157(17) 0.0019(16) C26 0.0331(18) 0.0218(17) 0.0360(19) -0.0015(14) 0.0201(16) -0.0057(14) C27 0.0239(16) 0.0189(16) 0.0332(18) -0.0012(13) 0.0147(15) -0.0006(13) C28 0.039(2) 0.0237(18) 0.038(2) -0.0080(15) 0.0129(17) -0.0108(15) C29 0.047(2) 0.036(2) 0.0256(18) -0.0040(16) 0.0060(17) -0.0037(17) C30 0.042(2) 0.0260(18) 0.0300(19) 0.0038(14) 0.0124(17) 0.0018(15) C31 0.0316(18) 0.0196(16) 0.0291(18) 0.0016(13) 0.0134(15) 0.0007(13) C100 0.055(4) 0.064(4) 0.045(4) 0.004(3) 0.024(3) -0.006(3) O100 0.0297(13) 0.0435(14) 0.0245(12) -0.0009(10) 0.0120(10) -0.0002(10) O1W 0.0297(13) 0.0435(14) 0.0245(12) -0.0009(10) 0.0120(10) -0.0002(10) Cl1 0.0493(5) 0.0343(5) 0.0391(5) 0.0004(4) 0.0284(4) 0.0043(4) O1A 0.086(2) 0.0521(19) 0.084(2) 0.0183(16) 0.060(2) 0.0276(16) O1B 0.151(3) 0.0484(19) 0.072(2) -0.0049(16) 0.075(2) 0.011(2) O1C 0.103(3) 0.087(3) 0.071(2) 0.0046(18) 0.064(2) -0.015(2) O1D 0.055(2) 0.129(3) 0.086(3) 0.023(2) 0.018(2) 0.000(2) Cl2 0.0505(6) 0.0653(7) 0.0366(5) 0.0011(5) 0.0267(5) -0.0040(5) O2A 0.076(6) 0.114(9) 0.036(4) 0.016(5) 0.030(4) 0.044(6) O2B 0.134(8) 0.058(5) 0.113(7) 0.012(5) 0.058(7) -0.041(5) O2C 0.071(7) 0.173(13) 0.075(7) 0.029(7) -0.035(5) -0.034(7) O2D 0.251(16) 0.136(9) 0.113(8) 0.041(7) 0.137(11) 0.115(10) O2E 0.198(11) 0.077(6) 0.121(7) 0.053(5) 0.116(8) 0.052(7) O2F 0.037(5) 0.47(3) 0.090(8) 0.087(13) 0.023(5) -0.038(10) O2G 0.095(8) 0.111(9) 0.065(6) 0.055(6) 0.061(6) 0.062(7) O2H 0.110(8) 0.112(8) 0.076(6) -0.030(6) 0.055(7) -0.022(6) O3W 0.084(2) 0.0584(19) 0.0511(18) -0.0142(14) 0.0392(17) -0.0137(16) O1S 0.076(2) 0.0497(18) 0.065(2) 0.0085(15) 0.0391(18) 0.0150(16) C1S 0.063(3) 0.068(3) 0.071(3) -0.011(3) 0.026(3) 0.002(3) O2S 0.141(5) 0.150(5) 0.196(6) -0.049(4) 0.086(5) -0.015(4) C2S 0.134(7) 0.176(9) 0.225(11) -0.081(8) 0.109(8) -0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O2 1.584(2) . ? V1 O1 1.939(2) . ? V1 O100 2.007(2) . ? V1 N5 2.112(3) . ? V1 N6 2.125(3) . ? V1 N4 2.404(2) . ? S1 O12 1.429(2) . ? S1 O11 1.431(2) . ? S1 N1 1.635(3) . ? S1 C2 1.772(3) . ? S2 O21 1.428(3) . ? S2 O22 1.429(2) . ? S2 N4 1.709(3) . ? S2 C6 1.748(3) . ? O1 C1 1.318(4) . ? N1 C8 1.468(4) . ? N1 C14 1.487(4) . ? N2 C9 1.335(4) . ? N2 C13 1.346(4) . ? N2 H2A 0.880 . ? N3 C19 1.336(4) . ? N3 C15 1.343(4) . ? N4 C26 1.492(4) . ? N4 C20 1.496(4) . ? N5 C21 1.351(4) . ? N5 C25 1.355(4) . ? N6 C27 1.345(4) . ? N6 C31 1.351(4) . ? C1 C6 1.404(4) . ? C1 C2 1.407(4) . ? C2 C3 1.385(5) . ? C3 C4 1.392(5) . ? C3 H3A 0.950 . ? C4 C5 1.373(5) . ? C4 C7 1.510(5) . ? C5 C6 1.393(5) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.510(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.370(5) . ? C10 C11 1.382(5) . ? C10 H10A 0.950 . ? C11 C12 1.372(6) . ? C11 H11A 0.950 . ? C12 C13 1.357(5) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.503(5) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.375(5) . ? C16 C17 1.382(6) . ? C16 H16A 0.950 . ? C17 C18 1.371(6) . ? C17 H17A 0.950 . ? C18 C19 1.378(5) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.499(5) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.377(5) . ? C22 C23 1.380(5) . ? C22 H22A 0.950 . ? C23 C24 1.367(6) . ? C23 H23A 0.950 . ? C24 C25 1.372(5) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.500(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.374(5) . ? C28 C29 1.369(5) . ? C28 H28A 0.950 . ? C29 C30 1.383(5) . ? C29 H29A 0.950 . ? C30 C31 1.368(5) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C100 O100 1.455(6) . ? C100 H103 0.980 . ? C100 H102 0.980 . ? C100 H101 0.980 . ? O100 H100 0.850 . ? O1W H1W 0.850 . ? O1W H2W 0.850 . ? O2W H3W 0.850 . ? O2W H4W 0.850 . ? O3W H5W 0.850 . ? O3W H6W 0.850 . ? Cl1 O1A 1.416(3) . ? Cl1 O1B 1.420(3) . ? Cl1 O1C 1.411(3) . ? Cl1 O1D 1.422(3) . ? Cl2 O2A 1.391(6) . ? Cl2 O2B 1.388(5) . ? Cl2 O2C 1.376(6) . ? Cl2 O2D 1.464(6) . ? Cl2 O2E 1.448(6) . ? Cl2 O2F 1.363(6) . ? Cl2 O2G 1.407(6) . ? Cl2 O2H 1.410(6) . ? O1S C1S 1.405(6) . ? O1S H1S 0.850 . ? C1S H1S1 0.980 . ? C1S H1S2 0.980 . ? C1S H1S3 0.980 . ? O2S C2S 1.463(9) . ? O2S H2S 0.850 . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? 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 O2 V1 O1 106.43(10) . . ? O2 V1 O100 102.97(11) . . ? O1 V1 O100 88.02(9) . . ? O2 V1 N5 97.09(11) . . ? O1 V1 N5 156.23(10) . . ? O100 V1 N5 83.36(10) . . ? O2 V1 N6 93.90(10) . . ? O1 V1 N6 88.45(9) . . ? O100 V1 N6 163.07(10) . . ? N5 V1 N6 93.39(10) . . ? O2 V1 N4 162.85(11) . . ? O1 V1 N4 85.86(8) . . ? O100 V1 N4 89.10(9) . . ? N5 V1 N4 71.94(9) . . ? N6 V1 N4 74.13(9) . . ? O12 S1 O11 118.82(14) . . ? O12 S1 N1 106.76(14) . . ? O11 S1 N1 106.43(14) . . ? O12 S1 C2 111.25(14) . . ? O11 S1 C2 105.60(14) . . ? N1 S1 C2 107.41(14) . . ? O21 S2 O22 118.08(15) . . ? O21 S2 N4 105.43(13) . . ? O22 S2 N4 109.66(14) . . ? O21 S2 C6 110.67(15) . . ? O22 S2 C6 109.21(15) . . ? N4 S2 C6 102.62(13) . . ? C1 O1 V1 129.05(19) . . ? C8 N1 C14 118.7(3) . . ? C8 N1 S1 119.5(2) . . ? C14 N1 S1 115.6(2) . . ? C9 N2 C13 122.1(3) . . ? C9 N2 H2A 119.0 . . ? C13 N2 H2A 119.0 . . ? C19 N3 C15 118.2(3) . . ? C26 N4 C20 111.6(2) . . ? C26 N4 S2 111.4(2) . . ? C20 N4 S2 109.99(19) . . ? C26 N4 V1 107.93(17) . . ? C20 N4 V1 103.20(17) . . ? S2 N4 V1 112.52(12) . . ? C21 N5 C25 118.0(3) . . ? C21 N5 V1 119.7(2) . . ? C25 N5 V1 122.0(2) . . ? C27 N6 C31 117.6(3) . . ? C27 N6 V1 122.0(2) . . ? C31 N6 V1 120.0(2) . . ? O1 C1 C6 122.3(3) . . ? O1 C1 C2 122.1(3) . . ? C6 C1 C2 115.6(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 S1 119.2(2) . . ? C1 C2 S1 119.3(2) . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C7 121.1(3) . . ? C3 C4 C7 121.0(3) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 122.5(3) . . ? C5 C6 S2 118.6(2) . . ? C1 C6 S2 118.5(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 113.9(3) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C10 118.8(3) . . ? N2 C9 C8 120.3(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? N2 C13 C12 120.3(3) . . ? N2 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? N1 C14 C15 113.2(3) . . ? N1 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? N1 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? N3 C15 C16 121.8(3) . . ? N3 C15 C14 116.5(3) . . ? C16 C15 C14 121.6(3) . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 118.0(4) . . ? C17 C18 H18A 121.0 . . ? C19 C18 H18A 121.0 . . ? N3 C19 C18 123.3(4) . . ? N3 C19 H19A 118.3 . . ? C18 C19 H19A 118.3 . . ? N4 C20 C21 107.9(3) . . ? N4 C20 H20A 110.1 . . ? C21 C20 H20A 110.1 . . ? N4 C20 H20B 110.1 . . ? C21 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? N5 C21 C22 122.0(3) . . ? N5 C21 C20 116.4(3) . . ? C22 C21 C20 121.6(3) . . ? C21 C22 C23 119.0(4) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 119.2(3) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N5 C25 C24 122.3(4) . . ? N5 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? N4 C26 C27 111.9(2) . . ? N4 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? N4 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N6 C27 C28 122.0(3) . . ? N6 C27 C26 116.9(3) . . ? C28 C27 C26 121.0(3) . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 118.7(3) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? C31 C30 C29 118.8(3) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N6 C31 C30 123.0(3) . . ? N6 C31 H31A 118.5 . . ? C30 C31 H31A 118.5 . . ? C100 O100 V1 131.5(3) . . ? C100 O100 H100 98.8 . . ? V1 O100 H100 117.4 . . ? V1 O1W H1W 117.4 . . ? V1 O1W H2W 124.0 . . ? H1W O1W H2W 113.9 . . ? H3W O2W H4W 124.4 . . ? H5W O3W H6W 123.3 . . ? O1C Cl1 O1A 110.99(19) . . ? O1C Cl1 O1B 109.6(2) . . ? O1A Cl1 O1B 108.53(19) . . ? O1C Cl1 O1D 110.0(2) . . ? O1A Cl1 O1D 108.8(2) . . ? O1B Cl1 O1D 108.9(2) . . ? O2C Cl2 O2B 111.7(5) . . ? O2C Cl2 O2A 112.5(6) . . ? O2B Cl2 O2A 113.9(5) . . ? O2C Cl2 O2D 108.8(6) . . ? O2B Cl2 O2D 103.7(5) . . ? O2A Cl2 O2D 105.4(5) . . ? O2F Cl2 O2G 113.0(5) . . ? O2F Cl2 O2H 111.6(6) . . ? O2G Cl2 O2H 107.5(5) . . ? O2F Cl2 O2E 112.5(6) . . ? O2G Cl2 O2E 108.0(5) . . ? O2H Cl2 O2E 103.8(5) . . ? C1S O1S H1S 107.2 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 122.0 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 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 O2 V1 O1 C1 121.9(2) . . . . ? O100 V1 O1 C1 -135.1(2) . . . . ? N5 V1 O1 C1 -66.6(4) . . . . ? N6 V1 O1 C1 28.3(2) . . . . ? N4 V1 O1 C1 -45.9(2) . . . . ? O12 S1 N1 C8 -24.0(3) . . . . ? O11 S1 N1 C8 -151.9(2) . . . . ? C2 S1 N1 C8 95.4(3) . . . . ? O12 S1 N1 C14 -176.1(2) . . . . ? O11 S1 N1 C14 56.1(2) . . . . ? C2 S1 N1 C14 -56.6(2) . . . . ? O21 S2 N4 C26 178.14(19) . . . . ? O22 S2 N4 C26 50.0(2) . . . . ? C6 S2 N4 C26 -65.9(2) . . . . ? O21 S2 N4 C20 53.9(2) . . . . ? O22 S2 N4 C20 -74.2(2) . . . . ? C6 S2 N4 C20 169.8(2) . . . . ? O21 S2 N4 V1 -60.52(15) . . . . ? O22 S2 N4 V1 171.37(14) . . . . ? C6 S2 N4 V1 55.39(16) . . . . ? O2 V1 N4 C26 -28.9(4) . . . . ? O1 V1 N4 C26 107.71(19) . . . . ? O100 V1 N4 C26 -164.21(19) . . . . ? N5 V1 N4 C26 -80.90(19) . . . . ? N6 V1 N4 C26 18.15(18) . . . . ? O2 V1 N4 C20 89.3(4) . . . . ? O1 V1 N4 C20 -134.07(19) . . . . ? O100 V1 N4 C20 -45.99(19) . . . . ? N5 V1 N4 C20 37.32(18) . . . . ? N6 V1 N4 C20 136.4(2) . . . . ? O2 V1 N4 S2 -152.2(3) . . . . ? O1 V1 N4 S2 -15.56(13) . . . . ? O100 V1 N4 S2 72.52(14) . . . . ? N5 V1 N4 S2 155.83(16) . . . . ? N6 V1 N4 S2 -105.12(14) . . . . ? O2 V1 N5 C21 169.4(2) . . . . ? O1 V1 N5 C21 -2.4(4) . . . . ? O100 V1 N5 C21 67.0(2) . . . . ? N6 V1 N5 C21 -96.3(2) . . . . ? N4 V1 N5 C21 -24.2(2) . . . . ? O2 V1 N5 C25 -4.0(3) . . . . ? O1 V1 N5 C25 -175.8(2) . . . . ? O100 V1 N5 C25 -106.4(3) . . . . ? N6 V1 N5 C25 90.3(3) . . . . ? N4 V1 N5 C25 162.4(3) . . . . ? O2 V1 N6 C27 162.6(2) . . . . ? O1 V1 N6 C27 -91.1(2) . . . . ? O100 V1 N6 C27 -13.1(5) . . . . ? N5 V1 N6 C27 65.2(2) . . . . ? N4 V1 N6 C27 -4.9(2) . . . . ? O2 V1 N6 C31 -25.0(2) . . . . ? O1 V1 N6 C31 81.4(2) . . . . ? O100 V1 N6 C31 159.4(3) . . . . ? N5 V1 N6 C31 -122.3(2) . . . . ? N4 V1 N6 C31 167.5(2) . . . . ? V1 O1 C1 C6 58.1(4) . . . . ? V1 O1 C1 C2 -123.0(3) . . . . ? O1 C1 C2 C3 -178.4(3) . . . . ? C6 C1 C2 C3 0.5(5) . . . . ? O1 C1 C2 S1 -0.8(4) . . . . ? C6 C1 C2 S1 178.2(2) . . . . ? O12 S1 C2 C3 -124.0(3) . . . . ? O11 S1 C2 C3 6.2(3) . . . . ? N1 S1 C2 C3 119.5(3) . . . . ? O12 S1 C2 C1 58.3(3) . . . . ? O11 S1 C2 C1 -171.5(3) . . . . ? N1 S1 C2 C1 -58.2(3) . . . . ? C1 C2 C3 C4 -2.0(6) . . . . ? S1 C2 C3 C4 -179.6(3) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C2 C3 C4 C7 178.8(4) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C7 C4 C5 C6 -177.4(4) . . . . ? C4 C5 C6 C1 -0.8(6) . . . . ? C4 C5 C6 S2 171.2(3) . . . . ? O1 C1 C6 C5 179.7(3) . . . . ? C2 C1 C6 C5 0.8(5) . . . . ? O1 C1 C6 S2 7.7(4) . . . . ? C2 C1 C6 S2 -171.2(2) . . . . ? O21 S2 C6 C5 -121.5(3) . . . . ? O22 S2 C6 C5 10.1(3) . . . . ? N4 S2 C6 C5 126.4(3) . . . . ? O21 S2 C6 C1 50.8(3) . . . . ? O22 S2 C6 C1 -177.5(2) . . . . ? N4 S2 C6 C1 -61.2(3) . . . . ? C14 N1 C8 C9 -95.6(3) . . . . ? S1 N1 C8 C9 113.2(3) . . . . ? C13 N2 C9 C10 -0.1(5) . . . . ? C13 N2 C9 C8 178.0(3) . . . . ? N1 C8 C9 N2 20.2(4) . . . . ? N1 C8 C9 C10 -161.7(3) . . . . ? N2 C9 C10 C11 -0.2(5) . . . . ? C8 C9 C10 C11 -178.3(3) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C9 N2 C13 C12 0.4(5) . . . . ? C11 C12 C13 N2 -0.3(6) . . . . ? C8 N1 C14 C15 123.5(3) . . . . ? S1 N1 C14 C15 -84.2(3) . . . . ? C19 N3 C15 C16 0.7(5) . . . . ? C19 N3 C15 C14 -176.8(3) . . . . ? N1 C14 C15 N3 -46.3(4) . . . . ? N1 C14 C15 C16 136.2(4) . . . . ? N3 C15 C16 C17 -1.1(6) . . . . ? C14 C15 C16 C17 176.3(3) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C15 N3 C19 C18 -0.2(5) . . . . ? C17 C18 C19 N3 0.0(6) . . . . ? C26 N4 C20 C21 70.0(3) . . . . ? S2 N4 C20 C21 -165.9(2) . . . . ? V1 N4 C20 C21 -45.7(3) . . . . ? C25 N5 C21 C22 -0.2(5) . . . . ? V1 N5 C21 C22 -173.9(3) . . . . ? C25 N5 C21 C20 178.7(3) . . . . ? V1 N5 C21 C20 5.0(4) . . . . ? N4 C20 C21 N5 31.3(4) . . . . ? N4 C20 C21 C22 -149.8(3) . . . . ? N5 C21 C22 C23 1.0(5) . . . . ? C20 C21 C22 C23 -177.9(3) . . . . ? C21 C22 C23 C24 -0.8(6) . . . . ? C22 C23 C24 C25 -0.1(6) . . . . ? C21 N5 C25 C24 -0.6(5) . . . . ? V1 N5 C25 C24 172.9(3) . . . . ? C23 C24 C25 N5 0.8(6) . . . . ? C20 N4 C26 C27 -141.0(3) . . . . ? S2 N4 C26 C27 95.7(3) . . . . ? V1 N4 C26 C27 -28.3(3) . . . . ? C31 N6 C27 C28 0.2(4) . . . . ? V1 N6 C27 C28 172.8(2) . . . . ? C31 N6 C27 C26 177.3(3) . . . . ? V1 N6 C27 C26 -10.1(4) . . . . ? N4 C26 C27 N6 27.0(4) . . . . ? N4 C26 C27 C28 -155.9(3) . . . . ? N6 C27 C28 C29 0.2(5) . . . . ? C26 C27 C28 C29 -176.7(3) . . . . ? C27 C28 C29 C30 -0.5(6) . . . . ? C28 C29 C30 C31 0.3(5) . . . . ? C27 N6 C31 C30 -0.4(5) . . . . ? V1 N6 C31 C30 -173.2(3) . . . . ? C29 C30 C31 N6 0.1(5) . . . . ? O2 V1 O100 C100 86.8(4) . . . . ? O1 V1 O100 C100 -19.6(4) . . . . ? N5 V1 O100 C100 -177.4(4) . . . . ? N6 V1 O100 C100 -97.7(5) . . . . ? N4 V1 O100 C100 -105.5(4) . . . . ? 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 O1S H1S O1B 0.85 1.98 2.832(4) 179.8 . O2S H2S O1D 0.85 1.88 2.729(7) 179.5 1_455 O3W H5W O2C 0.85 2.10 2.955(11) 179.5 . O3W H6W O1S 0.85 1.87 2.715(4) 179.1 1_554 O2W H4W O2B 0.85 1.94 2.789(15) 179.2 3_655 O2W H3W O1C 0.85 2.66 3.505(12) 179.8 1_554 O1W H1W O3W 0.85 1.73 2.570(4) 171.0 . O1W H2W O2W 0.85 1.84 2.692(12) 179.2 . O100 H100 O3W 0.85 1.73 2.570(4) 171.0 . N2 H2A N3 0.88 1.87 2.740(4) 171.7 . #======================================================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 737972' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C31 H33 Mn N6 O7 S2 +), 2(Cl O4 -), 3(C2 H3 N), H2 O ; _chemical_formula_sum 'C68 H77 Cl2 Mn2 N15 O23 S4' _chemical_formula_weight 1781.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 13.1117(7) _cell_length_b 16.4295(7) _cell_length_c 19.0495(12) _cell_angle_alpha 77.147(2) _cell_angle_beta 86.282(2) _cell_angle_gamma 80.932(1) _cell_volume 3948.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7014 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.35 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 91586 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.42 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 16090 _reflns_number_gt 12128 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0595P)^2^+4.1498P] 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 contr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16090 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.397 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.071 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 Mn1 Mn 0.03861(3) 0.16591(2) 0.24919(2) 0.02050(10) Uani 1 1 d . . . S1 S -0.14150(6) 0.17523(4) 0.04922(4) 0.02847(16) Uani 1 1 d . . . S2 S -0.04950(5) -0.02804(4) 0.31320(4) 0.02325(15) Uani 1 1 d . . . O11 O -0.17935(19) 0.16006(14) -0.01497(11) 0.0416(6) Uani 1 1 d . . . O12 O -0.05616(16) 0.22097(13) 0.04359(11) 0.0365(5) Uani 1 1 d . . . O21 O -0.13558(15) 0.01781(13) 0.34443(10) 0.0298(4) Uani 1 1 d . . . O22 O -0.02443(17) -0.11638(12) 0.34302(11) 0.0346(5) Uani 1 1 d . . . O1 O -0.08610(14) 0.13753(11) 0.20414(10) 0.0240(4) Uani 1 1 d . . . O2 O 0.07951(15) 0.28101(12) 0.18664(11) 0.0325(5) Uani 1 1 d . . . H21 H 0.1396 0.2809 0.1685 0.049 Uiso 1 1 d R . . H22 H 0.0470 0.3300 0.1743 0.049 Uiso 1 1 d R . . O3 O -0.06898(14) 0.22010(12) 0.32267(10) 0.0269(4) Uani 1 1 d . . . H31 H -0.0526 0.2469 0.3520 0.040 Uiso 1 1 d R . . H32 H -0.1326 0.2173 0.3275 0.040 Uiso 1 1 d R . . N1 N -0.23633(18) 0.22613(15) 0.08768(14) 0.0307(6) Uani 1 1 d . . . N2 N -0.33552(18) 0.08920(15) 0.18021(13) 0.0291(5) Uani 1 1 d . . . N3 N -0.3489(2) 0.41962(15) 0.11631(13) 0.0314(6) Uani 1 1 d . . . N4 N 0.05345(16) 0.02019(13) 0.32141(11) 0.0205(5) Uani 1 1 d . . . N5 N 0.14369(17) 0.15334(14) 0.34120(12) 0.0235(5) Uani 1 1 d . . . N6 N 0.14887(17) 0.08311(14) 0.18783(12) 0.0235(5) Uani 1 1 d . . . C1 C -0.0856(2) 0.07052(16) 0.17863(14) 0.0224(6) Uani 1 1 d . . . C2 C -0.1098(2) 0.07507(17) 0.10630(15) 0.0248(6) Uani 1 1 d . . . C3 C -0.1124(2) 0.00374(18) 0.07962(15) 0.0277(6) Uani 1 1 d . . . H3A H -0.1301 0.0101 0.0309 0.033 Uiso 1 1 calc R . . C4 C -0.0897(2) -0.07748(18) 0.12243(16) 0.0295(6) Uani 1 1 d . . . C5 C -0.0644(2) -0.08423(17) 0.19275(15) 0.0265(6) Uani 1 1 d . . . H5A H -0.0478 -0.1386 0.2229 0.032 Uiso 1 1 calc R . . C6 C -0.0627(2) -0.01263(17) 0.22046(14) 0.0219(6) Uani 1 1 d . . . C7 C -0.0968(3) -0.1543(2) 0.09297(19) 0.0448(9) Uani 1 1 d . . . H7A H -0.0626 -0.2048 0.1253 0.067 Uiso 1 1 d R . . H7B H -0.0629 -0.1485 0.0451 0.067 Uiso 1 1 d R . . H7C H -0.1697 -0.1595 0.0894 0.067 Uiso 1 1 d R . . C8 C -0.3429(2) 0.2115(2) 0.08125(19) 0.0380(7) Uani 1 1 d . . . H8A H -0.3603 0.2267 0.0297 0.046 Uiso 1 1 calc R . . H8B H -0.3905 0.2494 0.1065 0.046 Uiso 1 1 calc R . . C9 C -0.3607(2) 0.12182(18) 0.11162(16) 0.0283(6) Uani 1 1 d . . . C10 C -0.4009(3) 0.0764(2) 0.07045(19) 0.0426(8) Uani 1 1 d . . . H10A H -0.4187 0.1010 0.0220 0.051 Uiso 1 1 calc R . . C11 C -0.4151(3) -0.0055(2) 0.1008(2) 0.0552(10) Uani 1 1 d . . . H11A H -0.4442 -0.0376 0.0736 0.066 Uiso 1 1 calc R . . C12 C -0.3871(3) -0.0403(2) 0.1699(2) 0.0500(9) Uani 1 1 d . . . H12A H -0.3945 -0.0972 0.1913 0.060 Uiso 1 1 calc R . . C13 C -0.3479(2) 0.0094(2) 0.20810(18) 0.0387(7) Uani 1 1 d . . . H13A H -0.3289 -0.0143 0.2565 0.046 Uiso 1 1 calc R . . C14 C -0.2213(2) 0.29447(18) 0.12157(15) 0.0287(6) Uani 1 1 d . . . H14A H -0.1464 0.2964 0.1233 0.034 Uiso 1 1 calc R . . H14B H -0.2495 0.2835 0.1717 0.034 Uiso 1 1 calc R . . C15 C -0.2741(2) 0.37875(18) 0.08071(15) 0.0278(6) Uani 1 1 d . . . C16 C -0.2466(3) 0.4120(2) 0.01082(18) 0.0438(8) Uani 1 1 d . . . H16A H -0.1931 0.3818 -0.0135 0.053 Uiso 1 1 calc R . . C17 C -0.2964(3) 0.4888(2) -0.02406(19) 0.0542(10) Uani 1 1 d . . . H17A H -0.2780 0.5122 -0.0726 0.065 Uiso 1 1 calc R . . C18 C -0.3731(3) 0.5314(2) 0.01238(19) 0.0458(9) Uani 1 1 d . . . H18A H -0.4091 0.5847 -0.0103 0.055 Uiso 1 1 calc R . . C19 C -0.3963(3) 0.4951(2) 0.08216(18) 0.0396(8) Uani 1 1 d . . . H19A H -0.4487 0.5247 0.1077 0.047 Uiso 1 1 calc R . . C20 C 0.0579(2) 0.03217(17) 0.39642(14) 0.0237(6) Uani 1 1 d . . . H20A H 0.0810 -0.0229 0.4288 0.028 Uiso 1 1 calc R . . H20B H -0.0120 0.0540 0.4131 0.028 Uiso 1 1 calc R . . C21 C 0.1310(2) 0.09297(17) 0.40030(14) 0.0238(6) Uani 1 1 d . . . C22 C 0.1780(2) 0.08934(18) 0.46412(15) 0.0279(6) Uani 1 1 d . . . H22A H 0.1690 0.0455 0.5049 0.033 Uiso 1 1 calc R . . C23 C 0.2381(2) 0.15004(19) 0.46792(17) 0.0317(7) Uani 1 1 d . . . H23A H 0.2704 0.1489 0.5114 0.038 Uiso 1 1 calc R . . C24 C 0.2505(2) 0.21260(19) 0.40722(17) 0.0324(7) Uani 1 1 d . . . H24A H 0.2910 0.2554 0.4084 0.039 Uiso 1 1 calc R . . C25 C 0.2031(2) 0.21162(18) 0.34539(16) 0.0275(6) Uani 1 1 d . . . H25A H 0.2127 0.2540 0.3036 0.033 Uiso 1 1 calc R . . C26 C 0.1523(2) -0.02580(18) 0.29863(15) 0.0261(6) Uani 1 1 d . . . H26A H 0.1474 -0.0869 0.3089 0.031 Uiso 1 1 calc R . . H26B H 0.2084 -0.0179 0.3276 0.031 Uiso 1 1 calc R . . C27 C 0.1800(2) 0.00253(17) 0.22010(14) 0.0240(6) Uani 1 1 d . . . C28 C 0.2414(3) -0.0533(2) 0.18477(17) 0.0387(8) Uani 1 1 d . . . H28A H 0.2620 -0.1102 0.2087 0.046 Uiso 1 1 calc R . . C29 C 0.2722(3) -0.0246(2) 0.11371(19) 0.0502(9) Uani 1 1 d . . . H29A H 0.3147 -0.0616 0.0883 0.060 Uiso 1 1 calc R . . C30 C 0.2407(3) 0.0577(2) 0.08057(17) 0.0422(8) Uani 1 1 d . . . H30A H 0.2618 0.0789 0.0322 0.051 Uiso 1 1 calc R . . C31 C 0.1781(2) 0.1090(2) 0.11863(15) 0.0311(7) Uani 1 1 d . . . H31A H 0.1544 0.1654 0.0949 0.037 Uiso 1 1 calc R . . Mn2 Mn 0.61063(3) 0.25449(2) 0.32780(2) 0.01957(10) Uani 1 1 d . . . S4 S 0.72142(5) 0.15304(4) 0.49049(3) 0.02223(15) Uani 1 1 d . . . S3 S 0.77426(5) 0.47519(4) 0.35675(4) 0.02493(15) Uani 1 1 d . . . O31 O 0.80864(18) 0.54247(13) 0.38149(11) 0.0369(5) Uani 1 1 d . . . O32 O 0.68133(15) 0.49384(13) 0.31704(11) 0.0324(5) Uani 1 1 d . . . O41 O 0.70806(16) 0.10618(12) 0.56270(10) 0.0307(5) Uani 1 1 d . . . O42 O 0.80539(14) 0.12129(12) 0.44757(10) 0.0282(4) Uani 1 1 d . . . O4 O 0.73170(13) 0.29975(11) 0.36352(9) 0.0209(4) Uani 1 1 d . . . O5 O 0.55655(15) 0.34153(13) 0.23471(10) 0.0334(5) Uani 1 1 d . . . H51 H 0.4924 0.3517 0.2293 0.050 Uiso 1 1 d R . . H52 H 0.5865 0.3661 0.1975 0.050 Uiso 1 1 d R . . O6 O 0.71859(14) 0.17182(12) 0.27680(10) 0.0283(4) Uani 1 1 d . . . H61 H 0.7017 0.1463 0.2467 0.042 Uiso 1 1 d R . . H62 H 0.7658 0.1408 0.3021 0.042 Uiso 1 1 d R . . N7 N 0.86574(18) 0.43645(15) 0.30795(12) 0.0269(5) Uani 1 1 d . . . N8 N 0.97188(19) 0.44428(16) 0.14515(12) 0.0307(6) Uani 1 1 d . . . N9 N 0.98283(17) 0.30601(14) 0.41681(13) 0.0260(5) Uani 1 1 d . . . N10 N 0.61311(17) 0.15696(13) 0.44470(12) 0.0214(5) Uani 1 1 d . . . N11 N 0.50855(17) 0.15711(14) 0.32429(12) 0.0249(5) Uani 1 1 d . . . N12 N 0.50521(17) 0.32187(14) 0.40230(12) 0.0227(5) Uani 1 1 d . . . C32 C 0.73836(19) 0.31641(16) 0.42628(14) 0.0199(5) Uani 1 1 d . . . C33 C 0.7276(2) 0.25759(16) 0.49214(14) 0.0213(5) Uani 1 1 d . . . C34 C 0.7382(2) 0.27566(18) 0.55903(15) 0.0256(6) Uani 1 1 d . . . H34A H 0.7293 0.2340 0.6015 0.031 Uiso 1 1 calc R . . C35 C 0.7613(2) 0.35289(19) 0.56488(15) 0.0296(6) Uani 1 1 d . . . C36 C 0.7714(2) 0.41276(18) 0.50108(15) 0.0265(6) Uani 1 1 d . . . H36A H 0.7876 0.4664 0.5036 0.032 Uiso 1 1 calc R . . C37 C 0.7584(2) 0.39627(16) 0.43450(14) 0.0213(5) Uani 1 1 d . . . C38 C 0.7810(3) 0.3709(2) 0.63648(17) 0.0445(8) Uani 1 1 d . . . H38A H 0.7530 0.3297 0.6753 0.067 Uiso 1 1 d R . . H38B H 0.7473 0.4279 0.6389 0.067 Uiso 1 1 d R . . H38C H 0.8556 0.3668 0.6419 0.067 Uiso 1 1 d R . . C39 C 0.8444(2) 0.41412(18) 0.24070(14) 0.0263(6) Uani 1 1 d . . . H39A H 0.7689 0.4164 0.2372 0.032 Uiso 1 1 calc R . . H39B H 0.8777 0.3557 0.2408 0.032 Uiso 1 1 calc R . . C40 C 0.8843(2) 0.47359(18) 0.17634(14) 0.0264(6) Uani 1 1 d . . . C41 C 0.8328(3) 0.55472(19) 0.15317(17) 0.0360(7) Uani 1 1 d . . . H41A H 0.7697 0.5732 0.1762 0.043 Uiso 1 1 calc R . . C42 C 0.8745(3) 0.6081(2) 0.09621(19) 0.0463(9) Uani 1 1 d . . . H42A H 0.8404 0.6639 0.0790 0.056 Uiso 1 1 calc R . . C43 C 0.9662(3) 0.5792(2) 0.06467(18) 0.0486(9) Uani 1 1 d . . . H43A H 0.9974 0.6150 0.0259 0.058 Uiso 1 1 calc R . . C44 C 1.0120(3) 0.4976(2) 0.09024(17) 0.0446(8) Uani 1 1 d . . . H44A H 1.0752 0.4778 0.0679 0.053 Uiso 1 1 calc R . . C45 C 0.9748(2) 0.4357(2) 0.32472(16) 0.0320(7) Uani 1 1 d . . . H45A H 0.9872 0.4945 0.3203 0.038 Uiso 1 1 calc R . . H45B H 1.0205 0.4115 0.2888 0.038 Uiso 1 1 calc R . . C46 C 1.0030(2) 0.38559(18) 0.39915(15) 0.0249(6) Uani 1 1 d . . . C47 C 1.0467(2) 0.42067(19) 0.44718(17) 0.0349(7) Uani 1 1 d . . . H47A H 1.0621 0.4767 0.4332 0.042 Uiso 1 1 calc R . . C48 C 1.0678(3) 0.3739(2) 0.51555(18) 0.0429(8) Uani 1 1 d . . . H48A H 1.0989 0.3969 0.5490 0.051 Uiso 1 1 calc R . . C49 C 1.0432(2) 0.2933(2) 0.53469(17) 0.0369(7) Uani 1 1 d . . . H49A H 1.0549 0.2601 0.5819 0.044 Uiso 1 1 calc R . . C50 C 1.0012(2) 0.26220(18) 0.48370(16) 0.0298(6) Uani 1 1 d . . . H50A H 0.9845 0.2065 0.4968 0.036 Uiso 1 1 calc R . . C51 C 0.6105(2) 0.07435(17) 0.42568(15) 0.0274(6) Uani 1 1 d . . . H51A H 0.5934 0.0329 0.4694 0.033 Uiso 1 1 calc R . . H51B H 0.6796 0.0533 0.4072 0.033 Uiso 1 1 calc R . . C52 C 0.5316(2) 0.08196(17) 0.36930(15) 0.0254(6) Uani 1 1 d . . . C53 C 0.4913(2) 0.01155(19) 0.36229(17) 0.0347(7) Uani 1 1 d . . . H53A H 0.5087 -0.0408 0.3953 0.042 Uiso 1 1 calc R . . C54 C 0.4254(2) 0.0179(2) 0.30677(18) 0.0376(7) Uani 1 1 d . . . H54A H 0.3978 -0.0301 0.3006 0.045 Uiso 1 1 calc R . . C55 C 0.4006(2) 0.0949(2) 0.26075(17) 0.0342(7) Uani 1 1 d . . . H55A H 0.3549 0.1013 0.2225 0.041 Uiso 1 1 calc R . . C56 C 0.4433(2) 0.16263(19) 0.27121(16) 0.0304(6) Uani 1 1 d . . . H56A H 0.4259 0.2158 0.2394 0.037 Uiso 1 1 calc R . . C57 C 0.5180(2) 0.18532(18) 0.48507(15) 0.0272(6) Uani 1 1 d . . . H57A H 0.5286 0.1641 0.5373 0.033 Uiso 1 1 calc R . . H57B H 0.4599 0.1604 0.4720 0.033 Uiso 1 1 calc R . . C58 C 0.4898(2) 0.27968(18) 0.47005(15) 0.0246(6) Uani 1 1 d . . . C59 C 0.4476(2) 0.3201(2) 0.52374(17) 0.0380(7) Uani 1 1 d . . . H59A H 0.4381 0.2888 0.5714 0.046 Uiso 1 1 calc R . . C60 C 0.4196(3) 0.4063(2) 0.50725(19) 0.0495(9) Uani 1 1 d . . . H60A H 0.3895 0.4354 0.5432 0.059 Uiso 1 1 calc R . . C61 C 0.4360(3) 0.4498(2) 0.43792(19) 0.0427(8) Uani 1 1 d . . . H61A H 0.4178 0.5094 0.4253 0.051 Uiso 1 1 calc R . . C62 C 0.4790(2) 0.40568(18) 0.38713(16) 0.0282(6) Uani 1 1 d . . . H62A H 0.4906 0.4360 0.3394 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.59150(9) 0.75607(6) 0.06216(5) 0.0595(3) Uani 1 1 d D . . O1A O 0.5224(5) 0.8268(4) 0.0791(4) 0.0972(8) Uiso 0.50 1 d PD A 1 O1B O 0.5204(5) 0.6977(4) 0.0608(4) 0.0972(8) Uiso 0.50 1 d PD A 1 O1C O 0.6535(5) 0.7212(5) 0.1248(3) 0.0972(8) Uiso 0.50 1 d PD A 1 O1D O 0.6500(5) 0.7704(5) 0.0011(3) 0.0972(8) Uiso 0.50 1 d PD A 1 O1E O 0.4964(5) 0.8053(4) 0.0865(4) 0.0972(8) Uiso 0.50 1 d PD A 2 O1F O 0.5762(6) 0.7509(5) -0.0099(3) 0.0972(8) Uiso 0.50 1 d PD A 2 O1G O 0.6128(6) 0.6773(4) 0.1073(4) 0.0972(8) Uiso 0.50 1 d PD A 2 O1H O 0.6738(5) 0.8034(4) 0.0627(4) 0.0972(8) Uiso 0.50 1 d PD A 2 Cl2 Cl 0.28175(6) 0.44187(5) 0.24238(4) 0.03431(17) Uani 1 1 d D . . O2A O 0.2522(3) 0.4139(2) 0.31532(14) 0.0794(10) Uani 1 1 d D . . O2B O 0.3388(2) 0.50967(16) 0.23591(15) 0.0628(8) Uani 1 1 d D . . O2C O 0.19286(19) 0.46499(19) 0.19990(14) 0.0634(8) Uani 1 1 d D . . O2D O 0.3465(2) 0.37462(18) 0.21684(19) 0.0760(10) Uani 1 1 d D . . O1W O 0.2735(2) 0.28095(18) 0.12729(16) 0.0628(8) Uani 1 1 d . . . H1W H 0.2947 0.3088 0.1539 0.094 Uiso 1 1 d R . . H2W H 0.3160 0.2719 0.0940 0.094 Uiso 1 1 d R . . N1S N 0.6829(4) 0.8373(3) 0.3651(2) 0.0790(12) Uani 1 1 d . . . C1S C 0.7160(4) 0.7955(3) 0.3276(3) 0.0634(12) Uani 1 1 d . . . C2S C 0.7574(5) 0.7409(3) 0.2786(3) 0.0899(16) Uani 1 1 d . . . H2S1 H 0.8330 0.7362 0.2767 0.135 Uiso 1 1 d R . . H2S2 H 0.7310 0.7652 0.2303 0.135 Uiso 1 1 d R . . H2S3 H 0.7372 0.6848 0.2959 0.135 Uiso 1 1 d R . . N2S N 0.4321(4) 0.7944(3) 0.2936(2) 0.0840(12) Uani 1 1 d . . . C3S C 0.4576(3) 0.7320(3) 0.2779(2) 0.0577(10) Uani 1 1 d . . . C4S C 0.4882(4) 0.6512(3) 0.2590(3) 0.0831(15) Uani 1 1 d . . . H4S1 H 0.5435 0.6188 0.2904 0.125 Uiso 1 1 d R . . H4S2 H 0.5130 0.6592 0.2087 0.125 Uiso 1 1 d R . . H4S3 H 0.4287 0.6205 0.2656 0.125 Uiso 1 1 d R . . N3S N 0.0054(5) 0.6676(4) 0.2544(3) 0.118(2) Uani 1 1 d . . . C5S C 0.0697(5) 0.6752(3) 0.2131(3) 0.0783(15) Uani 1 1 d . . . C6S C 0.1550(6) 0.6838(4) 0.1620(3) 0.125(3) Uani 1 1 d . . . H6S1 H 0.2088 0.7071 0.1813 0.188 Uiso 1 1 d R . . H6S2 H 0.1306 0.7218 0.1171 0.188 Uiso 1 1 d R . . H6S3 H 0.1834 0.6283 0.1526 0.188 Uiso 1 1 d 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 Mn1 0.0209(2) 0.0201(2) 0.0211(2) -0.00559(16) -0.00113(16) -0.00291(16) S1 0.0339(4) 0.0265(4) 0.0236(4) -0.0024(3) -0.0031(3) -0.0037(3) S2 0.0272(4) 0.0218(3) 0.0219(3) -0.0052(3) -0.0013(3) -0.0064(3) O11 0.0599(15) 0.0379(12) 0.0257(11) -0.0027(9) -0.0128(10) -0.0040(11) O12 0.0346(12) 0.0347(12) 0.0381(12) -0.0035(10) 0.0076(9) -0.0087(9) O21 0.0252(10) 0.0381(12) 0.0292(11) -0.0132(9) 0.0034(8) -0.0073(9) O22 0.0500(13) 0.0236(10) 0.0299(11) -0.0001(9) -0.0062(10) -0.0109(9) O1 0.0242(10) 0.0213(9) 0.0279(10) -0.0078(8) -0.0067(8) -0.0015(8) O2 0.0291(11) 0.0246(10) 0.0402(12) -0.0009(9) 0.0052(9) -0.0039(8) O3 0.0217(10) 0.0334(11) 0.0316(11) -0.0185(9) 0.0007(8) -0.0064(8) N1 0.0264(13) 0.0237(12) 0.0415(15) -0.0062(11) -0.0051(11) -0.0013(10) N2 0.0276(13) 0.0320(13) 0.0286(13) -0.0102(11) 0.0007(10) -0.0029(10) N3 0.0371(14) 0.0289(13) 0.0265(13) -0.0045(10) 0.0023(11) -0.0036(11) N4 0.0208(11) 0.0232(11) 0.0176(11) -0.0054(9) -0.0010(9) -0.0019(9) N5 0.0198(11) 0.0251(12) 0.0268(12) -0.0088(10) -0.0009(9) -0.0023(9) N6 0.0215(11) 0.0284(12) 0.0214(12) -0.0076(10) -0.0012(9) -0.0029(9) C1 0.0199(13) 0.0225(13) 0.0264(14) -0.0081(11) -0.0015(11) -0.0033(11) C2 0.0233(14) 0.0247(14) 0.0256(14) -0.0049(11) -0.0021(11) -0.0013(11) C3 0.0294(15) 0.0330(16) 0.0219(14) -0.0108(12) -0.0024(12) -0.0002(12) C4 0.0304(16) 0.0269(15) 0.0336(16) -0.0147(13) -0.0049(13) 0.0015(12) C5 0.0272(15) 0.0212(14) 0.0313(15) -0.0083(12) -0.0042(12) 0.0004(11) C6 0.0214(13) 0.0237(14) 0.0219(14) -0.0076(11) -0.0033(11) -0.0019(11) C7 0.068(2) 0.0307(17) 0.0397(19) -0.0167(15) -0.0177(17) -0.0001(16) C8 0.0267(16) 0.0339(17) 0.051(2) -0.0036(15) -0.0098(14) -0.0018(13) C9 0.0244(15) 0.0290(15) 0.0326(16) -0.0104(12) -0.0025(12) -0.0017(12) C10 0.0424(19) 0.050(2) 0.0407(19) -0.0157(16) -0.0092(15) -0.0095(16) C11 0.054(2) 0.046(2) 0.077(3) -0.030(2) -0.013(2) -0.0136(18) C12 0.047(2) 0.0310(18) 0.073(3) -0.0087(18) -0.0013(19) -0.0127(16) C13 0.0352(17) 0.0390(18) 0.0387(18) -0.0028(14) 0.0070(14) -0.0070(14) C14 0.0333(16) 0.0281(15) 0.0246(15) -0.0060(12) -0.0014(12) -0.0036(12) C15 0.0319(16) 0.0251(14) 0.0272(15) -0.0057(12) -0.0006(12) -0.0071(12) C16 0.056(2) 0.0348(18) 0.0342(18) -0.0008(14) 0.0123(16) -0.0018(16) C17 0.078(3) 0.040(2) 0.0337(19) 0.0104(16) 0.0088(18) -0.0052(19) C18 0.059(2) 0.0245(16) 0.046(2) 0.0058(15) -0.0050(17) 0.0000(15) C19 0.0457(19) 0.0283(16) 0.0407(19) -0.0057(14) 0.0016(15) 0.0032(14) C20 0.0292(15) 0.0235(14) 0.0190(13) -0.0063(11) 0.0001(11) -0.0039(11) C21 0.0224(14) 0.0262(14) 0.0233(14) -0.0092(11) -0.0010(11) 0.0007(11) C22 0.0259(15) 0.0294(15) 0.0275(15) -0.0082(12) -0.0046(12) 0.0029(12) C23 0.0258(15) 0.0370(17) 0.0353(17) -0.0151(14) -0.0083(13) -0.0001(13) C24 0.0236(15) 0.0348(16) 0.0428(18) -0.0135(14) -0.0055(13) -0.0073(12) C25 0.0225(14) 0.0292(15) 0.0309(15) -0.0068(12) -0.0014(12) -0.0035(12) C26 0.0255(14) 0.0252(14) 0.0266(15) -0.0069(12) -0.0026(12) 0.0022(11) C27 0.0217(14) 0.0284(15) 0.0233(14) -0.0088(11) -0.0037(11) -0.0018(11) C28 0.0436(19) 0.0357(17) 0.0339(17) -0.0119(14) 0.0021(14) 0.0081(14) C29 0.054(2) 0.056(2) 0.0365(19) -0.0202(17) 0.0080(16) 0.0150(18) C30 0.045(2) 0.056(2) 0.0241(16) -0.0118(15) 0.0052(14) -0.0022(17) C31 0.0332(16) 0.0364(17) 0.0236(15) -0.0048(13) -0.0020(12) -0.0065(13) Mn2 0.0203(2) 0.0200(2) 0.0183(2) -0.00371(16) -0.00134(15) -0.00298(16) S4 0.0235(3) 0.0214(3) 0.0202(3) -0.0026(3) -0.0027(3) -0.0007(3) S3 0.0282(4) 0.0218(3) 0.0255(4) -0.0053(3) -0.0013(3) -0.0057(3) O31 0.0524(14) 0.0268(11) 0.0362(12) -0.0108(9) 0.0010(10) -0.0156(10) O32 0.0294(11) 0.0303(11) 0.0343(12) -0.0026(9) -0.0043(9) 0.0001(9) O41 0.0401(12) 0.0270(10) 0.0214(10) 0.0024(8) -0.0058(9) -0.0032(9) O42 0.0251(10) 0.0275(10) 0.0310(11) -0.0084(8) 0.0000(8) 0.0014(8) O4 0.0217(9) 0.0245(10) 0.0182(9) -0.0067(7) 0.0003(7) -0.0056(7) O5 0.0246(10) 0.0430(12) 0.0250(11) 0.0053(9) 0.0007(8) -0.0005(9) O6 0.0249(10) 0.0314(11) 0.0313(11) -0.0145(9) -0.0033(8) -0.0002(8) N7 0.0242(12) 0.0382(14) 0.0204(12) -0.0063(10) -0.0029(9) -0.0100(10) N8 0.0322(14) 0.0368(14) 0.0221(12) -0.0038(10) -0.0022(10) -0.0048(11) N9 0.0215(12) 0.0278(12) 0.0313(13) -0.0134(10) -0.0012(10) -0.0015(10) N10 0.0215(11) 0.0194(11) 0.0222(11) -0.0031(9) -0.0010(9) -0.0011(9) N11 0.0231(12) 0.0242(12) 0.0274(12) -0.0045(10) -0.0018(10) -0.0043(9) N12 0.0206(11) 0.0248(12) 0.0222(12) -0.0049(9) -0.0008(9) -0.0017(9) C32 0.0153(12) 0.0246(13) 0.0197(13) -0.0063(11) -0.0002(10) -0.0011(10) C33 0.0183(13) 0.0236(13) 0.0226(14) -0.0070(11) -0.0014(10) -0.0014(10) C34 0.0244(14) 0.0298(15) 0.0213(14) -0.0060(11) -0.0007(11) 0.0002(12) C35 0.0295(15) 0.0364(16) 0.0245(15) -0.0107(12) -0.0026(12) -0.0028(13) C36 0.0261(15) 0.0275(15) 0.0291(15) -0.0125(12) -0.0023(12) -0.0037(12) C37 0.0188(13) 0.0233(13) 0.0217(13) -0.0051(11) -0.0006(10) -0.0022(10) C38 0.066(2) 0.047(2) 0.0256(16) -0.0141(15) -0.0068(16) -0.0117(18) C39 0.0293(15) 0.0254(14) 0.0256(15) -0.0077(12) -0.0024(12) -0.0050(12) C40 0.0324(16) 0.0272(15) 0.0213(14) -0.0061(11) -0.0052(12) -0.0063(12) C41 0.0443(19) 0.0300(16) 0.0314(17) -0.0046(13) -0.0019(14) -0.0013(14) C42 0.062(2) 0.0308(17) 0.041(2) 0.0038(15) -0.0090(17) -0.0054(16) C43 0.056(2) 0.053(2) 0.0313(18) 0.0090(16) -0.0026(16) -0.0186(18) C44 0.0413(19) 0.058(2) 0.0296(17) 0.0000(16) 0.0024(14) -0.0094(17) C45 0.0241(15) 0.0451(18) 0.0274(15) -0.0042(13) -0.0010(12) -0.0113(13) C46 0.0192(13) 0.0313(15) 0.0262(14) -0.0092(12) 0.0000(11) -0.0056(11) C47 0.0398(18) 0.0299(16) 0.0388(18) -0.0082(13) -0.0103(14) -0.0114(13) C48 0.056(2) 0.0428(19) 0.0356(18) -0.0116(15) -0.0183(16) -0.0120(16) C49 0.0406(18) 0.0364(17) 0.0310(17) -0.0023(13) -0.0094(14) -0.0010(14) C50 0.0277(15) 0.0241(14) 0.0379(17) -0.0078(13) -0.0019(13) -0.0020(12) C51 0.0361(16) 0.0179(13) 0.0279(15) -0.0032(11) -0.0040(12) -0.0046(12) C52 0.0250(14) 0.0234(14) 0.0280(15) -0.0062(11) 0.0014(11) -0.0042(11) C53 0.0376(17) 0.0280(16) 0.0404(18) -0.0060(13) 0.0002(14) -0.0126(13) C54 0.0335(17) 0.0373(18) 0.048(2) -0.0140(15) 0.0007(14) -0.0165(14) C55 0.0256(15) 0.0419(18) 0.0400(18) -0.0149(14) -0.0039(13) -0.0099(13) C56 0.0254(15) 0.0328(16) 0.0333(16) -0.0073(13) -0.0021(12) -0.0044(12) C57 0.0256(15) 0.0294(15) 0.0246(15) -0.0019(12) 0.0037(11) -0.0052(12) C58 0.0161(13) 0.0317(15) 0.0250(14) -0.0060(12) 0.0004(11) -0.0005(11) C59 0.0391(18) 0.0447(19) 0.0259(16) -0.0071(14) 0.0077(13) 0.0030(15) C60 0.060(2) 0.047(2) 0.038(2) -0.0176(16) 0.0086(17) 0.0103(18) C61 0.051(2) 0.0291(17) 0.044(2) -0.0107(15) -0.0013(16) 0.0086(15) C62 0.0268(15) 0.0256(15) 0.0297(15) -0.0040(12) -0.0027(12) 0.0022(12) Cl1 0.0902(8) 0.0334(5) 0.0548(6) -0.0092(4) -0.0213(5) -0.0020(5) Cl2 0.0327(4) 0.0337(4) 0.0362(4) -0.0060(3) -0.0056(3) -0.0045(3) O2A 0.109(3) 0.093(2) 0.0384(16) 0.0045(15) -0.0006(16) -0.049(2) O2B 0.0724(19) 0.0468(15) 0.0729(19) -0.0077(14) 0.0000(15) -0.0279(14) O2C 0.0387(14) 0.090(2) 0.0579(17) -0.0167(15) -0.0180(12) 0.0086(14) O2D 0.0406(15) 0.0688(19) 0.133(3) -0.061(2) -0.0236(17) 0.0135(14) O1W 0.0483(15) 0.0743(19) 0.081(2) -0.0403(16) 0.0235(14) -0.0301(14) N1S 0.089(3) 0.088(3) 0.057(3) -0.005(2) -0.015(2) -0.013(3) C1S 0.063(3) 0.057(3) 0.060(3) 0.017(2) -0.014(2) -0.016(2) C2S 0.100(4) 0.066(3) 0.091(4) 0.004(3) 0.005(3) -0.006(3) N2S 0.105(3) 0.062(3) 0.081(3) -0.012(2) 0.010(2) -0.011(2) C3S 0.055(2) 0.054(3) 0.057(3) 0.002(2) 0.0013(19) -0.007(2) C4S 0.074(3) 0.060(3) 0.109(4) -0.013(3) 0.018(3) -0.009(2) N3S 0.094(4) 0.145(5) 0.098(4) 0.003(4) -0.032(3) 0.003(4) C5S 0.101(4) 0.078(3) 0.047(3) 0.001(2) -0.030(3) 0.006(3) C6S 0.180(7) 0.099(5) 0.065(4) 0.014(3) -0.007(4) 0.034(5) _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 Mn1 O1 2.0562(18) . ? Mn1 O2 2.1255(19) . ? Mn1 O3 2.1550(19) . ? Mn1 N5 2.253(2) . ? Mn1 N6 2.275(2) . ? Mn1 N4 2.467(2) . ? S1 O12 1.429(2) . ? S1 O11 1.434(2) . ? S1 N1 1.615(3) . ? S1 C2 1.763(3) . ? S2 O21 1.428(2) . ? S2 O22 1.430(2) . ? S2 N4 1.701(2) . ? S2 C6 1.744(3) . ? O1 C1 1.298(3) . ? O2 H21 0.840 . ? O2 H22 0.840 . ? O3 H31 0.840 . ? O3 H32 0.840 . ? N1 C14 1.458(4) . ? N1 C8 1.472(4) . ? N2 C13 1.331(4) . ? N2 C9 1.339(4) . ? N3 C15 1.335(4) . ? N3 C19 1.340(4) . ? N4 C26 1.484(3) . ? N4 C20 1.491(3) . ? N5 C25 1.345(4) . ? N5 C21 1.345(3) . ? N6 C27 1.341(4) . ? N6 C31 1.342(4) . ? C1 C2 1.417(4) . ? C1 C6 1.417(4) . ? C2 C3 1.383(4) . ? C3 C4 1.399(4) . ? C3 H3A 0.950 . ? C4 C5 1.377(4) . ? C4 C7 1.508(4) . ? C5 C6 1.396(4) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.507(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.374(4) . ? C10 C11 1.377(5) . ? C10 H10A 0.950 . ? C11 C12 1.364(6) . ? C11 H11A 0.950 . ? C12 C13 1.381(5) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.513(4) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.370(4) . ? C16 C17 1.373(5) . ? C16 H16A 0.950 . ? C17 C18 1.374(5) . ? C17 H17A 0.950 . ? C18 C19 1.367(5) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.505(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.383(4) . ? C22 C23 1.381(4) . ? C22 H22A 0.950 . ? C23 C24 1.385(4) . ? C23 H23A 0.950 . ? C24 C25 1.371(4) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.503(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.383(4) . ? C28 C29 1.387(5) . ? C28 H28A 0.950 . ? C29 C30 1.370(5) . ? C29 H29A 0.950 . ? C30 C31 1.373(4) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? Mn2 O4 2.0672(17) . ? Mn2 O5 2.0995(19) . ? Mn2 O6 2.1437(19) . ? Mn2 N11 2.256(2) . ? Mn2 N12 2.261(2) . ? Mn2 N10 2.436(2) . ? S4 O42 1.430(2) . ? S4 O41 1.4339(19) . ? S4 N10 1.700(2) . ? S4 C33 1.740(3) . ? S3 O32 1.432(2) . ? S3 O31 1.436(2) . ? S3 N7 1.608(2) . ? S3 C37 1.763(3) . ? O4 C32 1.295(3) . ? O5 H51 0.840 . ? O5 H52 0.840 . ? O6 H61 0.840 . ? O6 H62 0.840 . ? N7 C39 1.464(3) . ? N7 C45 1.482(4) . ? N8 C40 1.330(4) . ? N8 C44 1.343(4) . ? N9 C50 1.333(4) . ? N9 C46 1.340(4) . ? N10 C51 1.487(3) . ? N10 C57 1.488(3) . ? N11 C52 1.340(4) . ? N11 C56 1.345(4) . ? N12 C62 1.336(4) . ? N12 C58 1.342(3) . ? C32 C33 1.417(4) . ? C32 C37 1.422(4) . ? C33 C34 1.391(4) . ? C34 C35 1.380(4) . ? C34 H34A 0.950 . ? C35 C36 1.397(4) . ? C35 C38 1.505(4) . ? C36 C37 1.381(4) . ? C36 H36A 0.950 . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 C40 1.509(4) . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C40 C41 1.386(4) . ? C41 C42 1.377(5) . ? C41 H41A 0.950 . ? C42 C43 1.373(5) . ? C42 H42A 0.950 . ? C43 C44 1.376(5) . ? C43 H43A 0.950 . ? C44 H44A 0.950 . ? C45 C46 1.509(4) . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C46 C47 1.380(4) . ? C47 C48 1.378(4) . ? C47 H47A 0.950 . ? C48 C49 1.377(5) . ? C48 H48A 0.950 . ? C49 C50 1.373(4) . ? C49 H49A 0.950 . ? C50 H50A 0.950 . ? C51 C52 1.511(4) . ? C51 H51A 0.990 . ? C51 H51B 0.990 . ? C52 C53 1.380(4) . ? C53 C54 1.385(4) . ? C53 H53A 0.950 . ? C54 C55 1.374(5) . ? C54 H54A 0.950 . ? C55 C56 1.380(4) . ? C55 H55A 0.950 . ? C56 H56A 0.950 . ? C57 C58 1.503(4) . ? C57 H57A 0.990 . ? C57 H57B 0.990 . ? C58 C59 1.380(4) . ? C59 C60 1.376(5) . ? C59 H59A 0.950 . ? C60 C61 1.376(5) . ? C60 H60A 0.950 . ? C61 C62 1.375(4) . ? C61 H61A 0.950 . ? C62 H62A 0.950 . ? Cl1 O1D 1.348(5) . ? Cl1 O1G 1.384(5) . ? Cl1 O1F 1.423(5) . ? Cl1 O1H 1.428(5) . ? Cl1 O1A 1.440(6) . ? Cl1 O1B 1.444(5) . ? Cl1 O1C 1.445(5) . ? Cl1 O1E 1.483(6) . ? Cl2 O2A 1.412(3) . ? Cl2 O2C 1.416(2) . ? Cl2 O2B 1.416(2) . ? Cl2 O2D 1.438(3) . ? O1W H1W 0.840 . ? O1W H2W 0.840 . ? N1S C1S 1.120(6) . ? C1S C2S 1.457(8) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? N2S C3S 1.126(6) . ? C3S C4S 1.441(7) . ? C4S H4S1 0.980 . ? C4S H4S2 0.980 . ? C4S H4S3 0.980 . ? N3S C5S 1.118(7) . ? C5S C6S 1.437(9) . ? C6S H6S1 0.980 . ? C6S H6S2 0.980 . ? C6S H6S3 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 108.73(8) . . ? O1 Mn1 O3 87.68(7) . . ? O2 Mn1 O3 97.21(8) . . ? O1 Mn1 N5 152.63(8) . . ? O2 Mn1 N5 97.20(8) . . ? O3 Mn1 N5 80.36(8) . . ? O1 Mn1 N6 90.71(8) . . ? O2 Mn1 N6 94.41(8) . . ? O3 Mn1 N6 168.16(8) . . ? N5 Mn1 N6 96.00(8) . . ? O1 Mn1 N4 85.73(7) . . ? O2 Mn1 N4 161.11(8) . . ? O3 Mn1 N4 95.42(7) . . ? N5 Mn1 N4 71.15(8) . . ? N6 Mn1 N4 72.76(8) . . ? O12 S1 O11 119.14(14) . . ? O12 S1 N1 107.05(13) . . ? O11 S1 N1 107.50(14) . . ? O12 S1 C2 109.27(13) . . ? O11 S1 C2 105.93(13) . . ? N1 S1 C2 107.44(13) . . ? O21 S2 O22 117.88(13) . . ? O21 S2 N4 105.34(11) . . ? O22 S2 N4 108.77(12) . . ? O21 S2 C6 110.45(12) . . ? O22 S2 C6 109.12(13) . . ? N4 S2 C6 104.36(12) . . ? C1 O1 Mn1 124.60(16) . . ? Mn1 O2 H21 118.4 . . ? Mn1 O2 H22 133.5 . . ? H21 O2 H22 108.1 . . ? Mn1 O3 H31 124.2 . . ? Mn1 O3 H32 126.5 . . ? H31 O3 H32 109.2 . . ? C14 N1 C8 117.9(2) . . ? C14 N1 S1 121.6(2) . . ? C8 N1 S1 120.1(2) . . ? C13 N2 C9 118.2(3) . . ? C15 N3 C19 118.3(3) . . ? C26 N4 C20 111.2(2) . . ? C26 N4 S2 112.25(17) . . ? C20 N4 S2 110.58(16) . . ? C26 N4 Mn1 106.87(15) . . ? C20 N4 Mn1 102.76(15) . . ? S2 N4 Mn1 112.75(10) . . ? C25 N5 C21 118.3(2) . . ? C25 N5 Mn1 123.32(18) . . ? C21 N5 Mn1 117.14(17) . . ? C27 N6 C31 117.9(2) . . ? C27 N6 Mn1 118.78(18) . . ? C31 N6 Mn1 123.11(19) . . ? O1 C1 C2 122.2(2) . . ? O1 C1 C6 123.3(2) . . ? C2 C1 C6 114.6(2) . . ? C3 C2 C1 122.3(2) . . ? C3 C2 S1 118.9(2) . . ? C1 C2 S1 118.8(2) . . ? C2 C3 C4 121.8(3) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C7 121.6(3) . . ? C3 C4 C7 120.8(3) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 122.7(2) . . ? C5 C6 S2 117.1(2) . . ? C1 C6 S2 119.5(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 114.0(2) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C10 122.1(3) . . ? N2 C9 C8 116.7(3) . . ? C10 C9 C8 121.2(3) . . ? C9 C10 C11 118.8(3) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 118.1(3) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? N2 C13 C12 123.0(3) . . ? N2 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? N1 C14 C15 111.3(2) . . ? N1 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N1 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N3 C15 C16 121.4(3) . . ? N3 C15 C14 116.6(2) . . ? C16 C15 C14 122.0(3) . . ? C15 C16 C17 120.0(3) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 118.9(3) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C19 C18 C17 118.2(3) . . ? C19 C18 H18A 120.9 . . ? C17 C18 H18A 120.9 . . ? N3 C19 C18 123.3(3) . . ? N3 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? N4 C20 C21 111.1(2) . . ? N4 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? N4 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N5 C21 C22 121.8(3) . . ? N5 C21 C20 117.7(2) . . ? C22 C21 C20 120.5(2) . . ? C23 C22 C21 119.4(3) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 118.7(3) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? N5 C25 C24 123.0(3) . . ? N5 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? N4 C26 C27 113.5(2) . . ? N4 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? N4 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? N6 C27 C28 122.2(3) . . ? N6 C27 C26 118.3(2) . . ? C28 C27 C26 119.4(3) . . ? C27 C28 C29 118.8(3) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C30 C29 C28 119.2(3) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C29 C30 C31 118.8(3) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? N6 C31 C30 123.1(3) . . ? N6 C31 H31A 118.4 . . ? C30 C31 H31A 118.4 . . ? O4 Mn2 O5 107.22(8) . . ? O4 Mn2 O6 90.02(7) . . ? O5 Mn2 O6 98.22(8) . . ? O4 Mn2 N11 155.28(8) . . ? O5 Mn2 N11 96.99(8) . . ? O6 Mn2 N11 81.47(8) . . ? O4 Mn2 N12 87.59(8) . . ? O5 Mn2 N12 93.39(8) . . ? O6 Mn2 N12 168.34(8) . . ? N11 Mn2 N12 96.08(8) . . ? O4 Mn2 N10 86.19(7) . . ? O5 Mn2 N10 161.26(8) . . ? O6 Mn2 N10 94.72(7) . . ? N11 Mn2 N10 71.55(8) . . ? N12 Mn2 N10 73.74(8) . . ? O42 S4 O41 117.52(12) . . ? O42 S4 N10 105.60(11) . . ? O41 S4 N10 108.61(12) . . ? O42 S4 C33 110.21(12) . . ? O41 S4 C33 109.28(12) . . ? N10 S4 C33 104.81(12) . . ? O32 S3 O31 118.17(13) . . ? O32 S3 N7 108.08(12) . . ? O31 S3 N7 108.25(13) . . ? O32 S3 C37 108.81(12) . . ? O31 S3 C37 105.85(13) . . ? N7 S3 C37 107.20(13) . . ? C32 O4 Mn2 126.70(16) . . ? Mn2 O5 H51 117.4 . . ? Mn2 O5 H52 132.9 . . ? H51 O5 H52 109.3 . . ? Mn2 O6 H61 123.4 . . ? Mn2 O6 H62 117.2 . . ? H61 O6 H62 109.3 . . ? C39 N7 C45 118.5(2) . . ? C39 N7 S3 121.27(19) . . ? C45 N7 S3 119.57(19) . . ? C40 N8 C44 117.4(3) . . ? C50 N9 C46 118.2(2) . . ? C51 N10 C57 112.5(2) . . ? C51 N10 S4 110.25(17) . . ? C57 N10 S4 111.65(17) . . ? C51 N10 Mn2 103.08(15) . . ? C57 N10 Mn2 106.36(15) . . ? S4 N10 Mn2 112.69(10) . . ? C52 N11 C56 117.7(2) . . ? C52 N11 Mn2 116.23(18) . . ? C56 N11 Mn2 124.38(19) . . ? C62 N12 C58 118.3(2) . . ? C62 N12 Mn2 121.70(18) . . ? C58 N12 Mn2 118.01(18) . . ? O4 C32 C33 123.7(2) . . ? O4 C32 C37 122.1(2) . . ? C33 C32 C37 114.2(2) . . ? C34 C33 C32 123.0(2) . . ? C34 C33 S4 117.0(2) . . ? C32 C33 S4 119.2(2) . . ? C35 C34 C33 121.3(3) . . ? C35 C34 H34A 119.4 . . ? C33 C34 H34A 119.4 . . ? C34 C35 C36 117.3(3) . . ? C34 C35 C38 121.8(3) . . ? C36 C35 C38 120.8(3) . . ? C37 C36 C35 121.9(3) . . ? C37 C36 H36A 119.1 . . ? C35 C36 H36A 119.1 . . ? C36 C37 C32 122.3(2) . . ? C36 C37 S3 118.8(2) . . ? C32 C37 S3 118.87(19) . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 111.0(2) . . ? N7 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? N7 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? N8 C40 C41 122.8(3) . . ? N8 C40 C39 116.2(2) . . ? C41 C40 C39 120.9(3) . . ? C42 C41 C40 118.9(3) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C43 C42 C41 118.8(3) . . ? C43 C42 H42A 120.6 . . ? C41 C42 H42A 120.6 . . ? C42 C43 C44 118.8(3) . . ? C42 C43 H43A 120.6 . . ? C44 C43 H43A 120.6 . . ? N8 C44 C43 123.3(3) . . ? N8 C44 H44A 118.4 . . ? C43 C44 H44A 118.4 . . ? N7 C45 C46 113.3(2) . . ? N7 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? N7 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? N9 C46 C47 121.5(3) . . ? N9 C46 C45 117.1(2) . . ? C47 C46 C45 121.4(3) . . ? C48 C47 C46 119.6(3) . . ? C48 C47 H47A 120.2 . . ? C46 C47 H47A 120.2 . . ? C49 C48 C47 118.9(3) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C48 118.2(3) . . ? C50 C49 H49A 120.9 . . ? C48 C49 H49A 120.9 . . ? N9 C50 C49 123.5(3) . . ? N9 C50 H50A 118.3 . . ? C49 C50 H50A 118.3 . . ? N10 C51 C52 111.3(2) . . ? N10 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? N10 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? N11 C52 C53 122.2(3) . . ? N11 C52 C51 117.7(2) . . ? C53 C52 C51 120.0(3) . . ? C52 C53 C54 119.4(3) . . ? C52 C53 H53A 120.3 . . ? C54 C53 H53A 120.3 . . ? C55 C54 C53 118.8(3) . . ? C55 C54 H54A 120.6 . . ? C53 C54 H54A 120.6 . . ? C54 C55 C56 118.6(3) . . ? C54 C55 H55A 120.7 . . ? C56 C55 H55A 120.7 . . ? N11 C56 C55 123.2(3) . . ? N11 C56 H56A 118.4 . . ? C55 C56 H56A 118.4 . . ? N10 C57 C58 113.0(2) . . ? N10 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? N10 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? N12 C58 C59 122.1(3) . . ? N12 C58 C57 117.0(2) . . ? C59 C58 C57 120.8(3) . . ? C60 C59 C58 119.1(3) . . ? C60 C59 H59A 120.5 . . ? C58 C59 H59A 120.5 . . ? C61 C60 C59 118.9(3) . . ? C61 C60 H60A 120.5 . . ? C59 C60 H60A 120.5 . . ? C62 C61 C60 119.0(3) . . ? C62 C61 H61A 120.5 . . ? C60 C61 H61A 120.5 . . ? N12 C62 C61 122.6(3) . . ? N12 C62 H62A 118.7 . . ? C61 C62 H62A 118.7 . . ? O1G Cl1 O1F 112.2(4) . . ? O1G Cl1 O1H 110.0(4) . . ? O1F Cl1 O1H 109.3(4) . . ? O1D Cl1 O1A 117.3(4) . . ? O1D Cl1 O1B 112.5(4) . . ? O1A Cl1 O1B 101.3(4) . . ? O1D Cl1 O1C 112.0(4) . . ? O1A Cl1 O1C 105.9(4) . . ? O1B Cl1 O1C 106.8(4) . . ? O1G Cl1 O1E 111.4(4) . . ? O1F Cl1 O1E 106.9(4) . . ? O1H Cl1 O1E 106.8(4) . . ? O2A Cl2 O2C 109.61(19) . . ? O2A Cl2 O2B 109.50(18) . . ? O2C Cl2 O2B 111.98(18) . . ? O2A Cl2 O2D 110.0(2) . . ? O2C Cl2 O2D 107.48(17) . . ? O2B Cl2 O2D 108.22(18) . . ? H1W O1W H2W 113.0 . . ? N1S C1S C2S 179.1(6) . . ? C1S C2S H2S1 108.6 . . ? C1S C2S H2S2 109.9 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.9 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 178.5(5) . . ? C3S C4S H4S1 109.1 . . ? C3S C4S H4S2 109.9 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.3 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 178.0(6) . . ? C5S C6S H6S1 110.0 . . ? C5S C6S H6S2 109.2 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.2 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 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 O2 Mn1 O1 C1 118.3(2) . . . . ? O3 Mn1 O1 C1 -144.9(2) . . . . ? N5 Mn1 O1 C1 -81.2(3) . . . . ? N6 Mn1 O1 C1 23.4(2) . . . . ? N4 Mn1 O1 C1 -49.3(2) . . . . ? O12 S1 N1 C14 -11.4(3) . . . . ? O11 S1 N1 C14 -140.5(2) . . . . ? C2 S1 N1 C14 105.9(2) . . . . ? O12 S1 N1 C8 160.8(2) . . . . ? O11 S1 N1 C8 31.7(3) . . . . ? C2 S1 N1 C8 -81.9(2) . . . . ? O21 S2 N4 C26 173.66(17) . . . . ? O22 S2 N4 C26 46.4(2) . . . . ? C6 S2 N4 C26 -69.96(19) . . . . ? O21 S2 N4 C20 48.84(19) . . . . ? O22 S2 N4 C20 -78.42(19) . . . . ? C6 S2 N4 C20 165.22(17) . . . . ? O21 S2 N4 Mn1 -65.58(13) . . . . ? O22 S2 N4 Mn1 167.17(11) . . . . ? C6 S2 N4 Mn1 50.80(14) . . . . ? O1 Mn1 N4 C26 114.27(16) . . . . ? O2 Mn1 N4 C26 -26.6(3) . . . . ? O3 Mn1 N4 C26 -158.47(16) . . . . ? N5 Mn1 N4 C26 -80.60(16) . . . . ? N6 Mn1 N4 C26 22.20(16) . . . . ? O1 Mn1 N4 C20 -128.58(16) . . . . ? O2 Mn1 N4 C20 90.5(3) . . . . ? O3 Mn1 N4 C20 -41.32(16) . . . . ? N5 Mn1 N4 C20 36.55(15) . . . . ? N6 Mn1 N4 C20 139.35(16) . . . . ? O1 Mn1 N4 S2 -9.51(11) . . . . ? O2 Mn1 N4 S2 -150.4(2) . . . . ? O3 Mn1 N4 S2 77.74(11) . . . . ? N5 Mn1 N4 S2 155.62(13) . . . . ? N6 Mn1 N4 S2 -101.58(12) . . . . ? O1 Mn1 N5 C25 -158.4(2) . . . . ? O2 Mn1 N5 C25 3.1(2) . . . . ? O3 Mn1 N5 C25 -93.1(2) . . . . ? N6 Mn1 N5 C25 98.3(2) . . . . ? N4 Mn1 N5 C25 167.8(2) . . . . ? O1 Mn1 N5 C21 8.7(3) . . . . ? O2 Mn1 N5 C21 170.19(19) . . . . ? O3 Mn1 N5 C21 74.05(19) . . . . ? N6 Mn1 N5 C21 -94.6(2) . . . . ? N4 Mn1 N5 C21 -25.11(18) . . . . ? O1 Mn1 N6 C27 -93.57(19) . . . . ? O2 Mn1 N6 C27 157.59(19) . . . . ? O3 Mn1 N6 C27 -11.5(5) . . . . ? N5 Mn1 N6 C27 59.9(2) . . . . ? N4 Mn1 N6 C27 -8.26(18) . . . . ? O1 Mn1 N6 C31 81.0(2) . . . . ? O2 Mn1 N6 C31 -27.8(2) . . . . ? O3 Mn1 N6 C31 163.1(3) . . . . ? N5 Mn1 N6 C31 -125.6(2) . . . . ? N4 Mn1 N6 C31 166.3(2) . . . . ? Mn1 O1 C1 C2 -122.2(2) . . . . ? Mn1 O1 C1 C6 58.8(3) . . . . ? O1 C1 C2 C3 -178.0(3) . . . . ? C6 C1 C2 C3 1.2(4) . . . . ? O1 C1 C2 S1 0.0(4) . . . . ? C6 C1 C2 S1 179.09(19) . . . . ? O12 S1 C2 C3 -121.5(2) . . . . ? O11 S1 C2 C3 8.0(3) . . . . ? N1 S1 C2 C3 122.7(2) . . . . ? O12 S1 C2 C1 60.5(2) . . . . ? O11 S1 C2 C1 -170.0(2) . . . . ? N1 S1 C2 C1 -55.3(2) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? S1 C2 C3 C4 -178.9(2) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C2 C3 C4 C7 177.8(3) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C7 C4 C5 C6 -177.0(3) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C4 C5 C6 S2 170.3(2) . . . . ? O1 C1 C6 C5 178.7(3) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? O1 C1 C6 S2 8.1(4) . . . . ? C2 C1 C6 S2 -171.0(2) . . . . ? O21 S2 C6 C5 -121.0(2) . . . . ? O22 S2 C6 C5 10.1(3) . . . . ? N4 S2 C6 C5 126.2(2) . . . . ? O21 S2 C6 C1 50.1(2) . . . . ? O22 S2 C6 C1 -178.8(2) . . . . ? N4 S2 C6 C1 -62.6(2) . . . . ? C14 N1 C8 C9 -126.9(3) . . . . ? S1 N1 C8 C9 60.6(3) . . . . ? C13 N2 C9 C10 1.7(4) . . . . ? C13 N2 C9 C8 -178.4(3) . . . . ? N1 C8 C9 N2 54.9(4) . . . . ? N1 C8 C9 C10 -125.1(3) . . . . ? N2 C9 C10 C11 -0.4(5) . . . . ? C8 C9 C10 C11 179.6(3) . . . . ? C9 C10 C11 C12 -1.4(6) . . . . ? C10 C11 C12 C13 1.8(6) . . . . ? C9 N2 C13 C12 -1.2(5) . . . . ? C11 C12 C13 N2 -0.5(5) . . . . ? C8 N1 C14 C15 -60.3(3) . . . . ? S1 N1 C14 C15 112.2(2) . . . . ? C19 N3 C15 C16 -0.7(4) . . . . ? C19 N3 C15 C14 179.0(3) . . . . ? N1 C14 C15 N3 118.0(3) . . . . ? N1 C14 C15 C16 -62.2(4) . . . . ? N3 C15 C16 C17 0.0(5) . . . . ? C14 C15 C16 C17 -179.8(3) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C16 C17 C18 C19 0.1(6) . . . . ? C15 N3 C19 C18 1.2(5) . . . . ? C17 C18 C19 N3 -0.9(6) . . . . ? C26 N4 C20 C21 68.7(3) . . . . ? S2 N4 C20 C21 -165.89(18) . . . . ? Mn1 N4 C20 C21 -45.3(2) . . . . ? C25 N5 C21 C22 -0.6(4) . . . . ? Mn1 N5 C21 C22 -168.3(2) . . . . ? C25 N5 C21 C20 175.5(2) . . . . ? Mn1 N5 C21 C20 7.7(3) . . . . ? N4 C20 C21 N5 29.2(3) . . . . ? N4 C20 C21 C22 -154.7(2) . . . . ? N5 C21 C22 C23 1.1(4) . . . . ? C20 C21 C22 C23 -174.8(3) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? C22 C23 C24 C25 -0.5(4) . . . . ? C21 N5 C25 C24 -0.6(4) . . . . ? Mn1 N5 C25 C24 166.4(2) . . . . ? C23 C24 C25 N5 1.1(4) . . . . ? C20 N4 C26 C27 -145.3(2) . . . . ? S2 N4 C26 C27 90.2(2) . . . . ? Mn1 N4 C26 C27 -33.9(3) . . . . ? C31 N6 C27 C28 0.7(4) . . . . ? Mn1 N6 C27 C28 175.6(2) . . . . ? C31 N6 C27 C26 176.9(2) . . . . ? Mn1 N6 C27 C26 -8.2(3) . . . . ? N4 C26 C27 N6 30.5(3) . . . . ? N4 C26 C27 C28 -153.3(3) . . . . ? N6 C27 C28 C29 0.5(5) . . . . ? C26 C27 C28 C29 -175.6(3) . . . . ? C27 C28 C29 C30 -0.3(5) . . . . ? C28 C29 C30 C31 -1.0(6) . . . . ? C27 N6 C31 C30 -2.1(4) . . . . ? Mn1 N6 C31 C30 -176.8(2) . . . . ? C29 C30 C31 N6 2.3(5) . . . . ? O5 Mn2 O4 C32 122.3(2) . . . . ? O6 Mn2 O4 C32 -139.1(2) . . . . ? N11 Mn2 O4 C32 -69.8(3) . . . . ? N12 Mn2 O4 C32 29.5(2) . . . . ? N10 Mn2 O4 C32 -44.4(2) . . . . ? O32 S3 N7 C39 -8.9(2) . . . . ? O31 S3 N7 C39 -138.0(2) . . . . ? C37 S3 N7 C39 108.2(2) . . . . ? O32 S3 N7 C45 161.3(2) . . . . ? O31 S3 N7 C45 32.2(2) . . . . ? C37 S3 N7 C45 -81.5(2) . . . . ? O42 S4 N10 C51 51.5(2) . . . . ? O41 S4 N10 C51 -75.4(2) . . . . ? C33 S4 N10 C51 167.88(18) . . . . ? O42 S4 N10 C57 177.28(17) . . . . ? O41 S4 N10 C57 50.4(2) . . . . ? C33 S4 N10 C57 -66.31(19) . . . . ? O42 S4 N10 Mn2 -63.09(13) . . . . ? O41 S4 N10 Mn2 170.02(11) . . . . ? C33 S4 N10 Mn2 53.32(14) . . . . ? O4 Mn2 N10 C51 -132.16(16) . . . . ? O5 Mn2 N10 C51 91.2(3) . . . . ? O6 Mn2 N10 C51 -42.45(16) . . . . ? N11 Mn2 N10 C51 36.92(16) . . . . ? N12 Mn2 N10 C51 139.25(17) . . . . ? O4 Mn2 N10 C57 109.32(16) . . . . ? O5 Mn2 N10 C57 -27.3(3) . . . . ? O6 Mn2 N10 C57 -160.97(16) . . . . ? N11 Mn2 N10 C57 -81.60(17) . . . . ? N12 Mn2 N10 C57 20.73(16) . . . . ? O4 Mn2 N10 S4 -13.32(11) . . . . ? O5 Mn2 N10 S4 -150.0(2) . . . . ? O6 Mn2 N10 S4 76.39(12) . . . . ? N11 Mn2 N10 S4 155.75(13) . . . . ? N12 Mn2 N10 S4 -101.92(12) . . . . ? O4 Mn2 N11 C52 0.4(3) . . . . ? O5 Mn2 N11 C52 168.8(2) . . . . ? O6 Mn2 N11 C52 71.5(2) . . . . ? N12 Mn2 N11 C52 -97.0(2) . . . . ? N10 Mn2 N11 C52 -26.45(19) . . . . ? O4 Mn2 N11 C56 -164.5(2) . . . . ? O5 Mn2 N11 C56 3.8(2) . . . . ? O6 Mn2 N11 C56 -93.5(2) . . . . ? N12 Mn2 N11 C56 98.0(2) . . . . ? N10 Mn2 N11 C56 168.6(2) . . . . ? O4 Mn2 N12 C62 74.1(2) . . . . ? O5 Mn2 N12 C62 -33.0(2) . . . . ? O6 Mn2 N12 C62 152.5(3) . . . . ? N11 Mn2 N12 C62 -130.4(2) . . . . ? N10 Mn2 N12 C62 160.9(2) . . . . ? O4 Mn2 N12 C58 -89.48(19) . . . . ? O5 Mn2 N12 C58 163.40(19) . . . . ? O6 Mn2 N12 C58 -11.2(5) . . . . ? N11 Mn2 N12 C58 66.0(2) . . . . ? N10 Mn2 N12 C58 -2.75(18) . . . . ? Mn2 O4 C32 C33 54.5(3) . . . . ? Mn2 O4 C32 C37 -126.2(2) . . . . ? O4 C32 C33 C34 177.9(2) . . . . ? C37 C32 C33 C34 -1.4(4) . . . . ? O4 C32 C33 S4 8.5(3) . . . . ? C37 C32 C33 S4 -170.83(19) . . . . ? O42 S4 C33 C34 -119.2(2) . . . . ? O41 S4 C33 C34 11.4(2) . . . . ? N10 S4 C33 C34 127.7(2) . . . . ? O42 S4 C33 C32 50.9(2) . . . . ? O41 S4 C33 C32 -178.6(2) . . . . ? N10 S4 C33 C32 -62.3(2) . . . . ? C32 C33 C34 C35 -0.8(4) . . . . ? S4 C33 C34 C35 168.8(2) . . . . ? C33 C34 C35 C36 1.4(4) . . . . ? C33 C34 C35 C38 -175.2(3) . . . . ? C34 C35 C36 C37 0.3(4) . . . . ? C38 C35 C36 C37 176.9(3) . . . . ? C35 C36 C37 C32 -2.7(4) . . . . ? C35 C36 C37 S3 -179.2(2) . . . . ? O4 C32 C37 C36 -176.3(2) . . . . ? C33 C32 C37 C36 3.1(4) . . . . ? O4 C32 C37 S3 0.2(3) . . . . ? C33 C32 C37 S3 179.64(18) . . . . ? O32 S3 C37 C36 -122.8(2) . . . . ? O31 S3 C37 C36 5.2(3) . . . . ? N7 S3 C37 C36 120.6(2) . . . . ? O32 S3 C37 C32 60.6(2) . . . . ? O31 S3 C37 C32 -171.5(2) . . . . ? N7 S3 C37 C32 -56.1(2) . . . . ? C45 N7 C39 C40 -60.1(3) . . . . ? S3 N7 C39 C40 110.3(2) . . . . ? C44 N8 C40 C41 1.9(4) . . . . ? C44 N8 C40 C39 -176.4(3) . . . . ? N7 C39 C40 N8 102.9(3) . . . . ? N7 C39 C40 C41 -75.4(3) . . . . ? N8 C40 C41 C42 -1.1(5) . . . . ? C39 C40 C41 C42 177.1(3) . . . . ? C40 C41 C42 C43 -0.5(5) . . . . ? C41 C42 C43 C44 1.2(5) . . . . ? C40 N8 C44 C43 -1.1(5) . . . . ? C42 C43 C44 N8 -0.5(6) . . . . ? C39 N7 C45 C46 -129.1(3) . . . . ? S3 N7 C45 C46 60.4(3) . . . . ? C50 N9 C46 C47 3.3(4) . . . . ? C50 N9 C46 C45 -176.0(2) . . . . ? N7 C45 C46 N9 53.1(4) . . . . ? N7 C45 C46 C47 -126.2(3) . . . . ? N9 C46 C47 C48 -1.7(5) . . . . ? C45 C46 C47 C48 177.6(3) . . . . ? C46 C47 C48 C49 -1.0(5) . . . . ? C47 C48 C49 C50 1.9(5) . . . . ? C46 N9 C50 C49 -2.4(4) . . . . ? C48 C49 C50 N9 -0.2(5) . . . . ? C57 N10 C51 C52 69.4(3) . . . . ? S4 N10 C51 C52 -165.23(19) . . . . ? Mn2 N10 C51 C52 -44.7(2) . . . . ? C56 N11 C52 C53 0.4(4) . . . . ? Mn2 N11 C52 C53 -165.5(2) . . . . ? C56 N11 C52 C51 175.9(3) . . . . ? Mn2 N11 C52 C51 9.9(3) . . . . ? N10 C51 C52 N11 27.0(3) . . . . ? N10 C51 C52 C53 -157.5(3) . . . . ? N11 C52 C53 C54 0.5(5) . . . . ? C51 C52 C53 C54 -174.9(3) . . . . ? C52 C53 C54 C55 -1.0(5) . . . . ? C53 C54 C55 C56 0.8(5) . . . . ? C52 N11 C56 C55 -0.8(4) . . . . ? Mn2 N11 C56 C55 164.0(2) . . . . ? C54 C55 C56 N11 0.1(5) . . . . ? C51 N10 C57 C58 -148.1(2) . . . . ? S4 N10 C57 C58 87.4(2) . . . . ? Mn2 N10 C57 C58 -35.9(3) . . . . ? C62 N12 C58 C59 0.3(4) . . . . ? Mn2 N12 C58 C59 164.5(2) . . . . ? C62 N12 C58 C57 178.8(2) . . . . ? Mn2 N12 C58 C57 -17.0(3) . . . . ? N10 C57 C58 N12 37.6(3) . . . . ? N10 C57 C58 C59 -143.9(3) . . . . ? N12 C58 C59 C60 0.6(5) . . . . ? C57 C58 C59 C60 -177.9(3) . . . . ? C58 C59 C60 C61 -1.0(5) . . . . ? C59 C60 C61 C62 0.5(6) . . . . ? C58 N12 C62 C61 -0.8(4) . . . . ? Mn2 N12 C62 C61 -164.4(2) . . . . ? C60 C61 C62 N12 0.4(5) . . . . ? 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 O2 H21 O1W 0.84 1.88 2.715(3) 179.6 . O2 H22 N8 0.84 1.96 2.796(3) 179.8 1_455 O3 H31 N9 0.84 1.85 2.694(3) 179.7 1_455 O3 H32 O4 0.84 2.23 2.874(3) 133.7 1_455 O1W H1W O2D 0.84 2.00 2.835(4) 179.4 . O1W H2W O1F 0.84 2.12 2.964(7) 179.9 2_665 O5 H51 O2D 0.84 1.91 2.750(3) 179.8 . O5 H52 N3 0.84 1.83 2.668(3) 179.6 1_655 O6 H61 N2 0.84 1.86 2.705(3) 179.8 1_655 O6 H62 O21 0.84 2.23 3.010(3) 153.7 1_655 #======================================================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 737973' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C31 H34 Co N6 O7 S2 2+, 2(Cl O4 -), C2 H6 O, H2 O ; _chemical_formula_sum 'C33 H42 Cl2 Co N6 O17 S2' _chemical_formula_weight 988.68 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8054(10) _cell_length_b 21.2676(14) _cell_length_c 15.8384(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.797(3) _cell_angle_gamma 90.00 _cell_volume 4283.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7454 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.90 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The perchlorate anions were restrained to have tetrahedral geometry, with all Cl---O and all O...O distances restrained to a common refined value and 1.633 times that value, respectively. H atoms were placed so as to form a reasonable H-bond network then allowed to ride with constrained displacement parameters. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 67973 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 25.71 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 8080 _reflns_number_gt 5569 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.1699P)^2^+15.4082P] 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 8080 _refine_ls_number_parameters 552 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.2792 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.321 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.143 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 0.25428(6) 0.55132(4) 0.24227(5) 0.0342(3) Uani 1 1 d . . . S1 S 0.44367(11) 0.60070(6) 0.38521(8) 0.0266(3) Uani 1 1 d . . . S2 S 0.40922(14) 0.68312(7) 0.06076(9) 0.0394(4) Uani 1 1 d . . . O1 O 0.3308(3) 0.62984(17) 0.2136(2) 0.0294(9) Uani 1 1 d . . . O2 O 0.3654(3) 0.64652(18) 0.4001(2) 0.0329(9) Uani 1 1 d . . . O3 O 0.5240(3) 0.58825(19) 0.4536(2) 0.0352(9) Uani 1 1 d . . . O4 O 0.4807(4) 0.7058(2) 0.0047(3) 0.0527(13) Uani 1 1 d . . . O5 O 0.3285(4) 0.6402(2) 0.0280(3) 0.0502(12) Uani 1 1 d . . . O6 O 0.1363(4) 0.5545(2) 0.1393(3) 0.0565(14) Uani 1 1 d . . . H61 H 0.0941 0.5820 0.1158 0.085 Uiso 1 1 d R . . H62 H 0.1342 0.5313 0.0955 0.085 Uiso 1 1 d R . . O7 O 0.1603(3) 0.6141(2) 0.3046(3) 0.0477(12) Uani 1 1 d . . . H71 H 0.1145 0.6044 0.3370 0.072 Uiso 1 1 d R . . H72 H 0.1662 0.6534 0.2965 0.072 Uiso 1 1 d R . . N1 N 0.3510(4) 0.7446(2) 0.0974(3) 0.0344(11) Uani 1 1 d . . . N2 N 0.4906(4) 0.7873(2) 0.2457(3) 0.0403(12) Uani 1 1 d . . . H2A H 0.4270 0.7774 0.2571 0.048 Uiso 1 1 calc R . . N3 N 0.2846(4) 0.7661(2) 0.2581(3) 0.0330(11) Uani 1 1 d . . . N4 N 0.3752(4) 0.5337(2) 0.3568(3) 0.0259(10) Uani 1 1 d . . . N5 N 0.3616(5) 0.4929(2) 0.1884(3) 0.0406(13) Uani 1 1 d . . . N6 N 0.1870(4) 0.4786(2) 0.3098(4) 0.0447(14) Uani 1 1 d . . . C1 C 0.4329(5) 0.6323(2) 0.2191(3) 0.0288(12) Uani 1 1 d . . . C2 C 0.5014(4) 0.6171(2) 0.2937(3) 0.0280(12) Uani 1 1 d . . . C3 C 0.6094(5) 0.6194(3) 0.2983(4) 0.0351(13) Uani 1 1 d . . . H3A H 0.6508 0.6082 0.3498 0.042 Uiso 1 1 calc R . . C4 C 0.6591(5) 0.6379(3) 0.2287(4) 0.0416(15) Uani 1 1 d . . . C5 C 0.5949(5) 0.6547(3) 0.1554(4) 0.0404(15) Uani 1 1 d . . . H5A H 0.6264 0.6686 0.1073 0.048 Uiso 1 1 calc R . . C6 C 0.4860(5) 0.6520(3) 0.1503(4) 0.0350(14) Uani 1 1 d . . . C7 C 0.7776(6) 0.6421(4) 0.2351(6) 0.063(2) Uani 1 1 d . . . H7A H 0.7990 0.6474 0.1781 0.095 Uiso 1 1 calc R . . H7B H 0.8087 0.6035 0.2607 0.095 Uiso 1 1 calc R . . H7C H 0.8020 0.6782 0.2705 0.095 Uiso 1 1 calc R . . C8 C 0.5720(6) 0.7865(3) 0.3079(5) 0.0515(18) Uani 1 1 d . . . H8A H 0.5599 0.7753 0.3640 0.062 Uiso 1 1 calc R . . C9 C 0.6720(6) 0.8015(4) 0.2922(6) 0.061(2) Uani 1 1 d . . . H9A H 0.7285 0.8017 0.3368 0.074 Uiso 1 1 calc R . . C10 C 0.6886(7) 0.8161(4) 0.2110(7) 0.069(2) Uani 1 1 d . . . H10A H 0.7578 0.8255 0.1989 0.083 Uiso 1 1 calc R . . C11 C 0.6068(7) 0.8174(3) 0.1461(5) 0.0552(19) Uani 1 1 d . . . H11A H 0.6183 0.8277 0.0896 0.066 Uiso 1 1 calc R . . C12 C 0.5064(6) 0.8030(3) 0.1665(4) 0.0406(15) Uani 1 1 d . . . C13 C 0.4112(6) 0.8038(3) 0.1015(4) 0.0449(16) Uani 1 1 d . . . H13A H 0.3646 0.8386 0.1148 0.054 Uiso 1 1 calc R . . H13B H 0.4337 0.8123 0.0449 0.054 Uiso 1 1 calc R . . C14 C 0.2403(5) 0.7455(3) 0.1044(4) 0.0415(15) Uani 1 1 d . . . H14A H 0.2096 0.7052 0.0819 0.050 Uiso 1 1 calc R . . H14B H 0.2078 0.7795 0.0676 0.050 Uiso 1 1 calc R . . C15 C 0.2103(5) 0.7549(3) 0.1934(4) 0.0363(14) Uani 1 1 d . . . C16 C 0.1065(6) 0.7543(3) 0.2081(5) 0.0453(16) Uani 1 1 d . . . H16A H 0.0527 0.7463 0.1627 0.054 Uiso 1 1 calc R . . C17 C 0.0808(6) 0.7653(3) 0.2895(5) 0.0519(18) Uani 1 1 d . . . H17A H 0.0093 0.7644 0.2999 0.062 Uiso 1 1 calc R . . C18 C 0.1580(6) 0.7775(3) 0.3548(5) 0.0503(18) Uani 1 1 d . . . H18A H 0.1407 0.7861 0.4104 0.060 Uiso 1 1 calc R . . C19 C 0.2607(6) 0.7771(3) 0.3385(4) 0.0435(16) Uani 1 1 d . . . H19A H 0.3155 0.7844 0.3833 0.052 Uiso 1 1 calc R . . C20 C 0.3580(7) 0.4815(3) 0.1049(4) 0.060(2) Uani 1 1 d . . . H20A H 0.2981 0.4947 0.0681 0.072 Uiso 1 1 calc R . . C21 C 0.4381(9) 0.4512(4) 0.0707(5) 0.074(3) Uani 1 1 d . . . H21A H 0.4329 0.4433 0.0113 0.089 Uiso 1 1 calc R . . C22 C 0.5243(7) 0.4327(4) 0.1222(5) 0.059(2) Uani 1 1 d . . . H22A H 0.5803 0.4119 0.0994 0.071 Uiso 1 1 calc R . . C23 C 0.5299(6) 0.4443(3) 0.2073(5) 0.0441(16) Uani 1 1 d . . . H23A H 0.5903 0.4321 0.2444 0.053 Uiso 1 1 calc R . . C24 C 0.4456(5) 0.4744(3) 0.2394(4) 0.0334(13) Uani 1 1 d . . . C25 C 0.4467(5) 0.4822(3) 0.3340(4) 0.0296(12) Uani 1 1 d . . . H25A H 0.4250 0.4421 0.3586 0.036 Uiso 1 1 calc R . . H25B H 0.5193 0.4915 0.3596 0.036 Uiso 1 1 calc R . . C26 C 0.3141(5) 0.5139(3) 0.4262(4) 0.0352(14) Uani 1 1 d . . . H26A H 0.2842 0.5513 0.4517 0.042 Uiso 1 1 calc R . . H26B H 0.3609 0.4922 0.4712 0.042 Uiso 1 1 calc R . . C27 C 0.2272(5) 0.4706(3) 0.3913(4) 0.0359(14) Uani 1 1 d . . . C28 C 0.1888(6) 0.4255(3) 0.4434(6) 0.055(2) Uani 1 1 d . . . H28A H 0.2191 0.4197 0.5006 0.067 Uiso 1 1 calc R . . C29 C 0.1041(7) 0.3891(4) 0.4081(8) 0.074(3) Uani 1 1 d . . . H29A H 0.0753 0.3583 0.4420 0.089 Uiso 1 1 calc R . . C30 C 0.0627(6) 0.3969(4) 0.3271(9) 0.074(3) Uani 1 1 d . . . H30A H 0.0049 0.3719 0.3037 0.088 Uiso 1 1 calc R . . C31 C 0.1049(5) 0.4416(3) 0.2779(7) 0.063(2) Uani 1 1 d . . . H31A H 0.0759 0.4468 0.2202 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.20067(12) 0.55393(8) 0.63548(11) 0.0433(4) Uani 1 1 d D . . O1A O 0.2948(4) 0.5245(3) 0.6213(3) 0.0748(18) Uani 1 1 d D . . O1B O 0.2204(5) 0.5968(3) 0.7030(4) 0.0805(18) Uani 1 1 d D . . O1C O 0.1305(5) 0.5091(3) 0.6581(6) 0.117(3) Uani 1 1 d D . . O1D O 0.1600(6) 0.5881(4) 0.5639(4) 0.110(3) Uani 1 1 d D . . Cl2 Cl 0.07723(18) 0.18837(11) 0.49493(15) 0.0721(6) Uani 1 1 d D . . O2A O 0.0177(9) 0.2417(4) 0.5136(9) 0.257(10) Uani 1 1 d D . . O2B O 0.1097(11) 0.1576(5) 0.5686(7) 0.326(15) Uani 1 1 d D . . O2C O 0.0129(9) 0.1503(4) 0.4408(6) 0.190(6) Uani 1 1 d D . . O2D O 0.1593(9) 0.2129(6) 0.4579(9) 0.269(10) Uani 1 1 d D . . O1W O 0.0188(6) 0.5878(7) 0.4026(6) 0.160(5) Uani 1 1 d . . . H1W H -0.0258 0.5599 0.3846 0.239 Uiso 1 1 d R . . H2W H 0.0595 0.5884 0.4490 0.239 Uiso 1 1 d R . . O1S O 0.1296(9) 0.4817(5) -0.0060(6) 0.143(4) Uani 1 1 d D . . H1S H 0.1104 0.4436 -0.0027 0.215 Uiso 1 1 d R . . C1S C 0.1449(11) 0.4936(6) -0.0945(6) 0.111(4) Uani 1 1 d D . . H1SA H 0.0959 0.4687 -0.1343 0.133 Uiso 1 1 calc R . . H1SB H 0.2182 0.4852 -0.1053 0.133 Uiso 1 1 calc R . . C2S C 0.1196(12) 0.5622(6) -0.0996(8) 0.116(4) Uani 1 1 d D . . H2SA H 0.1266 0.5776 -0.1570 0.174 Uiso 1 1 calc R . . H2SB H 0.1684 0.5852 -0.0582 0.174 Uiso 1 1 calc R . . H2SC H 0.0474 0.5689 -0.0870 0.174 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 0.0362(5) 0.0209(4) 0.0437(5) -0.0022(3) -0.0025(4) 0.0018(3) S1 0.0382(8) 0.0179(7) 0.0238(7) 0.0000(5) 0.0048(5) -0.0008(5) S2 0.0696(11) 0.0281(8) 0.0227(7) -0.0002(6) 0.0142(7) 0.0110(7) O1 0.037(2) 0.022(2) 0.029(2) 0.0011(16) 0.0056(16) 0.0035(16) O2 0.051(2) 0.023(2) 0.026(2) -0.0047(16) 0.0103(17) 0.0040(17) O3 0.048(2) 0.029(2) 0.028(2) -0.0008(17) 0.0041(18) -0.0055(18) O4 0.085(4) 0.048(3) 0.030(2) 0.008(2) 0.030(2) 0.016(3) O5 0.083(3) 0.041(3) 0.026(2) -0.0093(19) 0.004(2) 0.005(2) O6 0.054(3) 0.046(3) 0.063(3) -0.007(2) -0.020(2) 0.002(2) O7 0.041(2) 0.030(2) 0.075(3) 0.004(2) 0.019(2) 0.0072(19) N1 0.052(3) 0.025(3) 0.027(2) -0.003(2) 0.007(2) 0.010(2) N2 0.050(3) 0.030(3) 0.041(3) -0.006(2) 0.008(2) 0.003(2) N3 0.051(3) 0.023(3) 0.025(2) -0.0013(19) 0.008(2) 0.009(2) N4 0.032(2) 0.017(2) 0.030(2) 0.0021(18) 0.0094(19) 0.0030(18) N5 0.063(3) 0.022(3) 0.034(3) -0.003(2) -0.003(2) 0.003(2) N6 0.032(3) 0.023(3) 0.078(4) -0.002(3) 0.002(3) 0.000(2) C1 0.047(4) 0.009(2) 0.032(3) -0.002(2) 0.013(2) 0.001(2) C2 0.037(3) 0.017(3) 0.031(3) 0.002(2) 0.008(2) -0.005(2) C3 0.039(3) 0.022(3) 0.045(3) 0.005(2) 0.006(3) 0.002(2) C4 0.043(4) 0.027(3) 0.057(4) 0.006(3) 0.022(3) 0.001(3) C5 0.053(4) 0.025(3) 0.049(4) 0.003(3) 0.030(3) 0.009(3) C6 0.060(4) 0.016(3) 0.032(3) -0.001(2) 0.016(3) 0.011(3) C7 0.044(4) 0.062(5) 0.087(6) 0.015(4) 0.028(4) 0.007(4) C8 0.063(5) 0.036(4) 0.053(4) -0.007(3) -0.002(4) 0.005(3) C9 0.056(5) 0.040(4) 0.085(6) -0.008(4) -0.003(4) -0.006(3) C10 0.066(5) 0.037(4) 0.105(8) -0.001(4) 0.020(5) -0.011(4) C11 0.074(5) 0.028(4) 0.068(5) 0.010(3) 0.024(4) -0.007(3) C12 0.067(4) 0.013(3) 0.042(4) 0.000(2) 0.010(3) 0.003(3) C13 0.074(5) 0.024(3) 0.039(4) 0.006(3) 0.014(3) 0.011(3) C14 0.055(4) 0.037(4) 0.031(3) -0.001(3) -0.001(3) 0.011(3) C15 0.057(4) 0.021(3) 0.031(3) 0.000(2) 0.006(3) 0.012(3) C16 0.050(4) 0.034(4) 0.051(4) -0.002(3) 0.006(3) 0.008(3) C17 0.055(4) 0.047(4) 0.057(5) 0.002(3) 0.022(4) 0.015(3) C18 0.071(5) 0.040(4) 0.043(4) -0.001(3) 0.024(4) 0.014(3) C19 0.064(4) 0.030(3) 0.037(3) -0.001(3) 0.007(3) 0.010(3) C20 0.101(6) 0.039(4) 0.036(4) -0.010(3) -0.012(4) 0.015(4) C21 0.135(9) 0.046(5) 0.042(4) -0.015(4) 0.012(5) 0.023(5) C22 0.092(6) 0.039(4) 0.051(4) -0.010(3) 0.030(4) 0.015(4) C23 0.052(4) 0.029(3) 0.053(4) -0.003(3) 0.017(3) 0.004(3) C24 0.050(4) 0.018(3) 0.034(3) -0.002(2) 0.011(3) -0.002(2) C25 0.038(3) 0.018(3) 0.034(3) 0.001(2) 0.008(2) 0.002(2) C26 0.044(3) 0.024(3) 0.041(3) 0.003(3) 0.018(3) 0.002(2) C27 0.029(3) 0.024(3) 0.058(4) -0.005(3) 0.020(3) 0.001(2) C28 0.057(4) 0.033(4) 0.085(6) 0.006(4) 0.044(4) -0.003(3) C29 0.060(5) 0.038(4) 0.136(9) -0.012(5) 0.060(6) -0.012(4) C30 0.036(4) 0.036(4) 0.152(10) -0.019(5) 0.025(5) -0.008(3) C31 0.033(4) 0.033(4) 0.119(7) -0.013(4) -0.007(4) -0.003(3) Cl1 0.0352(8) 0.0409(9) 0.0555(10) -0.0017(7) 0.0129(7) 0.0029(6) O1A 0.046(3) 0.117(5) 0.063(3) -0.019(3) 0.010(3) 0.028(3) O1B 0.077(4) 0.071(4) 0.096(5) -0.022(4) 0.023(3) 0.002(3) O1C 0.083(5) 0.052(4) 0.226(10) 0.003(5) 0.055(6) -0.019(3) O1D 0.097(5) 0.152(8) 0.081(5) 0.033(5) 0.011(4) 0.048(5) Cl2 0.0683(13) 0.0708(15) 0.0759(14) -0.0097(11) 0.0034(11) 0.0065(11) O2A 0.311(18) 0.106(9) 0.40(2) -0.104(12) 0.243(18) -0.040(10) O2B 0.32(2) 0.164(12) 0.41(3) 0.142(15) -0.29(2) -0.095(13) O2C 0.270(15) 0.112(8) 0.160(10) -0.012(7) -0.089(10) -0.061(9) O2D 0.206(14) 0.226(17) 0.41(3) -0.074(16) 0.168(16) -0.140(13) O1W 0.071(5) 0.300(15) 0.110(6) -0.070(8) 0.018(5) -0.021(7) O1S 0.161(9) 0.132(8) 0.134(8) -0.040(7) 0.008(7) -0.026(7) C1S 0.131(11) 0.122(11) 0.073(8) -0.020(7) -0.017(7) -0.023(9) C2S 0.146(12) 0.109(11) 0.087(8) -0.019(7) -0.003(8) -0.005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.015(4) . ? Co1 O6 2.089(5) . ? Co1 N5 2.107(5) . ? Co1 O7 2.118(4) . ? Co1 N6 2.121(6) . ? Co1 N4 2.273(5) . ? S1 O3 1.428(4) . ? S1 O2 1.437(4) . ? S1 N4 1.706(5) . ? S1 C2 1.738(5) . ? S2 O5 1.430(5) . ? S2 O4 1.432(5) . ? S2 N1 1.644(5) . ? S2 C6 1.758(6) . ? O1 C1 1.301(7) . ? O6 H61 0.850 . ? O6 H62 0.850 . ? O7 H71 0.850 . ? O7 H72 0.850 . ? N1 C14 1.435(9) . ? N1 C13 1.473(9) . ? N2 C12 1.336(8) . ? N2 C8 1.348(9) . ? N2 H2A 0.880 . ? N3 C15 1.334(8) . ? N3 C19 1.365(8) . ? N4 C26 1.484(7) . ? N4 C25 1.497(7) . ? N5 C24 1.326(8) . ? N5 C20 1.340(9) . ? N6 C27 1.343(9) . ? N6 C31 1.361(9) . ? C1 C6 1.414(8) . ? C1 C2 1.424(8) . ? C2 C3 1.377(8) . ? C3 C4 1.392(9) . ? C3 H3A 0.950 . ? C4 C5 1.387(10) . ? C4 C7 1.512(9) . ? C5 C6 1.388(9) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.370(11) . ? C8 H8A 0.950 . ? C9 C10 1.364(13) . ? C9 H9A 0.950 . ? C10 C11 1.378(12) . ? C10 H10A 0.950 . ? C11 C12 1.396(10) . ? C11 H11A 0.950 . ? C12 C13 1.500(10) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 C15 1.518(9) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.377(9) . ? C16 C17 1.388(10) . ? C16 H16A 0.950 . ? C17 C18 1.369(11) . ? C17 H17A 0.950 . ? C18 C19 1.370(10) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.376(13) . ? C20 H20A 0.950 . ? C21 C22 1.351(13) . ? C21 H21A 0.950 . ? C22 C23 1.364(10) . ? C22 H22A 0.950 . ? C23 C24 1.401(9) . ? C23 H23A 0.950 . ? C24 C25 1.506(8) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.499(9) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.392(9) . ? C28 C29 1.394(13) . ? C28 H28A 0.950 . ? C29 C30 1.339(14) . ? C29 H29A 0.950 . ? C30 C31 1.380(13) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? Cl1 O1C 1.386(5) . ? Cl1 O1D 1.394(5) . ? Cl1 O1A 1.399(5) . ? Cl1 O1B 1.406(5) . ? Cl2 O2B 1.360(7) . ? Cl2 O2D 1.367(7) . ? Cl2 O2C 1.380(6) . ? Cl2 O2A 1.418(7) . ? O1W H1W 0.850 . ? O1W H2W 0.850 . ? O1S C1S 1.460(9) . ? O1S H1S 0.850 . ? C1S C2S 1.495(9) . ? C1S H1SA 0.990 . ? C1S H1SB 0.990 . ? C2S H2SA 0.980 . ? C2S H2SB 0.980 . ? C2S H2SC 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O6 97.06(18) . . ? O1 Co1 N5 92.27(18) . . ? O6 Co1 N5 98.6(2) . . ? O1 Co1 O7 84.30(17) . . ? O6 Co1 O7 86.8(2) . . ? N5 Co1 O7 173.9(2) . . ? O1 Co1 N6 162.8(2) . . ? O6 Co1 N6 96.8(2) . . ? N5 Co1 N6 95.6(2) . . ? O7 Co1 N6 86.4(2) . . ? O1 Co1 N4 90.75(15) . . ? O6 Co1 N4 171.94(18) . . ? N5 Co1 N4 79.04(18) . . ? O7 Co1 N4 95.95(17) . . ? N6 Co1 N4 75.89(19) . . ? O3 S1 O2 117.1(2) . . ? O3 S1 N4 110.3(2) . . ? O2 S1 N4 105.3(2) . . ? O3 S1 C2 109.3(3) . . ? O2 S1 C2 112.0(3) . . ? N4 S1 C2 101.7(2) . . ? O5 S2 O4 118.6(3) . . ? O5 S2 N1 107.3(3) . . ? O4 S2 N1 107.5(3) . . ? O5 S2 C6 111.3(3) . . ? O4 S2 C6 106.8(3) . . ? N1 S2 C6 104.4(3) . . ? C1 O1 Co1 122.0(3) . . ? Co1 O6 H61 136.7 . . ? Co1 O6 H62 124.7 . . ? H61 O6 H62 94.9 . . ? Co1 O7 H71 126.9 . . ? Co1 O7 H72 119.0 . . ? H71 O7 H72 114.1 . . ? C14 N1 C13 120.1(5) . . ? C14 N1 S2 122.0(4) . . ? C13 N1 S2 116.0(4) . . ? C12 N2 C8 120.0(6) . . ? C12 N2 H2A 120.0 . . ? C8 N2 H2A 120.0 . . ? C15 N3 C19 121.9(6) . . ? C26 N4 C25 111.2(4) . . ? C26 N4 S1 109.9(4) . . ? C25 N4 S1 111.4(3) . . ? C26 N4 Co1 105.6(3) . . ? C25 N4 Co1 107.9(3) . . ? S1 N4 Co1 110.7(2) . . ? C24 N5 C20 118.5(6) . . ? C24 N5 Co1 116.7(4) . . ? C20 N5 Co1 124.0(5) . . ? C27 N6 C31 118.4(7) . . ? C27 N6 Co1 116.4(4) . . ? C31 N6 Co1 125.1(6) . . ? O1 C1 C6 122.1(5) . . ? O1 C1 C2 124.2(5) . . ? C6 C1 C2 113.6(5) . . ? C3 C2 C1 123.5(5) . . ? C3 C2 S1 119.2(4) . . ? C1 C2 S1 117.2(4) . . ? C2 C3 C4 121.3(6) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 117.0(6) . . ? C5 C4 C7 122.0(6) . . ? C3 C4 C7 120.9(6) . . ? C4 C5 C6 121.9(6) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 122.6(6) . . ? C5 C6 S2 119.5(5) . . ? C1 C6 S2 117.3(5) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 121.5(8) . . ? N2 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C10 C9 C8 118.6(8) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 121.2(8) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C10 C11 C12 117.6(7) . . ? C10 C11 H11A 121.2 . . ? C12 C11 H11A 121.2 . . ? N2 C12 C11 121.2(7) . . ? N2 C12 C13 116.5(6) . . ? C11 C12 C13 122.3(6) . . ? N1 C13 C12 113.5(5) . . ? N1 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? N1 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? N1 C14 C15 115.7(5) . . ? N1 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? N1 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? N3 C15 C16 119.1(6) . . ? N3 C15 C14 120.1(6) . . ? C16 C15 C14 120.7(6) . . ? C15 C16 C17 119.7(7) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 120.3(7) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C19 118.6(6) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N3 C19 C18 120.3(6) . . ? N3 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? N5 C20 C21 122.3(7) . . ? N5 C20 H20A 118.9 . . ? C21 C20 H20A 118.9 . . ? C22 C21 C20 119.4(7) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 119.3(7) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C22 C23 C24 119.2(7) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? N5 C24 C23 121.3(6) . . ? N5 C24 C25 118.9(5) . . ? C23 C24 C25 119.6(6) . . ? N4 C25 C24 112.7(5) . . ? N4 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? N4 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? N4 C26 C27 109.6(5) . . ? N4 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? N4 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? N6 C27 C28 122.3(6) . . ? N6 C27 C26 117.4(5) . . ? C28 C27 C26 120.3(6) . . ? C27 C28 C29 117.2(9) . . ? C27 C28 H28A 121.4 . . ? C29 C28 H28A 121.4 . . ? C30 C29 C28 121.1(8) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 119.3(8) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? N6 C31 C30 121.7(9) . . ? N6 C31 H31A 119.2 . . ? C30 C31 H31A 119.2 . . ? O1C Cl1 O1D 112.2(5) . . ? O1C Cl1 O1A 109.3(4) . . ? O1D Cl1 O1A 110.4(4) . . ? O1C Cl1 O1B 108.2(4) . . ? O1D Cl1 O1B 107.2(4) . . ? O1A Cl1 O1B 109.3(3) . . ? O2B Cl2 O2D 112.3(7) . . ? O2B Cl2 O2C 110.5(6) . . ? O2D Cl2 O2C 113.0(7) . . ? O2B Cl2 O2A 108.9(7) . . ? O2D Cl2 O2A 104.1(6) . . ? O2C Cl2 O2A 107.6(6) . . ? H1W O1W H2W 128.3 . . ? C1S O1S H1S 107.2 . . ? O1S C1S C2S 99.7(10) . . ? O1S C1S H1SA 111.8 . . ? C2S C1S H1SA 111.8 . . ? O1S C1S H1SB 111.8 . . ? C2S C1S H1SB 111.8 . . ? H1SA C1S H1SB 109.5 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 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 O6 Co1 O1 C1 -136.9(4) . . . . ? N5 Co1 O1 C1 -37.9(4) . . . . ? O7 Co1 O1 C1 137.1(4) . . . . ? N6 Co1 O1 C1 79.5(7) . . . . ? N4 Co1 O1 C1 41.2(4) . . . . ? O5 S2 N1 C14 8.7(5) . . . . ? O4 S2 N1 C14 137.3(5) . . . . ? C6 S2 N1 C14 -109.5(5) . . . . ? O5 S2 N1 C13 -155.8(4) . . . . ? O4 S2 N1 C13 -27.3(5) . . . . ? C6 S2 N1 C13 85.9(5) . . . . ? O3 S1 N4 C26 67.5(4) . . . . ? O2 S1 N4 C26 -59.6(4) . . . . ? C2 S1 N4 C26 -176.6(4) . . . . ? O3 S1 N4 C25 -56.2(4) . . . . ? O2 S1 N4 C25 176.6(3) . . . . ? C2 S1 N4 C25 59.6(4) . . . . ? O3 S1 N4 Co1 -176.3(2) . . . . ? O2 S1 N4 Co1 56.6(3) . . . . ? C2 S1 N4 Co1 -60.4(3) . . . . ? O1 Co1 N4 C26 137.6(3) . . . . ? N5 Co1 N4 C26 -130.2(4) . . . . ? O7 Co1 N4 C26 53.3(3) . . . . ? N6 Co1 N4 C26 -31.5(3) . . . . ? O1 Co1 N4 C25 -103.4(3) . . . . ? N5 Co1 N4 C25 -11.2(3) . . . . ? O7 Co1 N4 C25 172.3(3) . . . . ? N6 Co1 N4 C25 87.5(3) . . . . ? O1 Co1 N4 S1 18.7(2) . . . . ? N5 Co1 N4 S1 110.9(3) . . . . ? O7 Co1 N4 S1 -65.6(2) . . . . ? N6 Co1 N4 S1 -150.4(3) . . . . ? O1 Co1 N5 C24 89.0(4) . . . . ? O6 Co1 N5 C24 -173.5(4) . . . . ? N6 Co1 N5 C24 -75.8(5) . . . . ? N4 Co1 N5 C24 -1.3(4) . . . . ? O1 Co1 N5 C20 -80.7(6) . . . . ? O6 Co1 N5 C20 16.8(6) . . . . ? N6 Co1 N5 C20 114.5(6) . . . . ? N4 Co1 N5 C20 -171.1(6) . . . . ? O1 Co1 N6 C27 -22.0(9) . . . . ? O6 Co1 N6 C27 -165.7(4) . . . . ? N5 Co1 N6 C27 95.0(4) . . . . ? O7 Co1 N6 C27 -79.3(4) . . . . ? N4 Co1 N6 C27 17.8(4) . . . . ? O1 Co1 N6 C31 155.6(6) . . . . ? O6 Co1 N6 C31 11.9(6) . . . . ? N5 Co1 N6 C31 -87.5(6) . . . . ? O7 Co1 N6 C31 98.2(6) . . . . ? N4 Co1 N6 C31 -164.7(6) . . . . ? Co1 O1 C1 C6 126.6(4) . . . . ? Co1 O1 C1 C2 -54.7(6) . . . . ? O1 C1 C2 C3 179.4(5) . . . . ? C6 C1 C2 C3 -1.7(8) . . . . ? O1 C1 C2 S1 -5.7(7) . . . . ? C6 C1 C2 S1 173.2(4) . . . . ? O3 S1 C2 C3 -3.3(5) . . . . ? O2 S1 C2 C3 128.1(5) . . . . ? N4 S1 C2 C3 -119.9(5) . . . . ? O3 S1 C2 C1 -178.4(4) . . . . ? O2 S1 C2 C1 -47.0(5) . . . . ? N4 S1 C2 C1 65.0(4) . . . . ? C1 C2 C3 C4 0.7(9) . . . . ? S1 C2 C3 C4 -174.1(5) . . . . ? C2 C3 C4 C5 1.0(9) . . . . ? C2 C3 C4 C7 178.2(6) . . . . ? C3 C4 C5 C6 -1.6(9) . . . . ? C7 C4 C5 C6 -178.7(6) . . . . ? C4 C5 C6 C1 0.4(9) . . . . ? C4 C5 C6 S2 172.1(5) . . . . ? O1 C1 C6 C5 -179.9(5) . . . . ? C2 C1 C6 C5 1.2(8) . . . . ? O1 C1 C6 S2 8.2(7) . . . . ? C2 C1 C6 S2 -170.6(4) . . . . ? O5 S2 C6 C5 132.4(5) . . . . ? O4 S2 C6 C5 1.6(6) . . . . ? N1 S2 C6 C5 -112.1(5) . . . . ? O5 S2 C6 C1 -55.5(5) . . . . ? O4 S2 C6 C1 173.7(4) . . . . ? N1 S2 C6 C1 60.0(5) . . . . ? C12 N2 C8 C9 -0.1(10) . . . . ? N2 C8 C9 C10 -1.5(11) . . . . ? C8 C9 C10 C11 1.6(12) . . . . ? C9 C10 C11 C12 -0.3(11) . . . . ? C8 N2 C12 C11 1.5(9) . . . . ? C8 N2 C12 C13 -178.9(5) . . . . ? C10 C11 C12 N2 -1.3(10) . . . . ? C10 C11 C12 C13 179.1(6) . . . . ? C14 N1 C13 C12 127.0(6) . . . . ? S2 N1 C13 C12 -68.1(6) . . . . ? N2 C12 C13 N1 -53.6(7) . . . . ? C11 C12 C13 N1 126.0(6) . . . . ? C13 N1 C14 C15 -76.4(7) . . . . ? S2 N1 C14 C15 119.6(5) . . . . ? C19 N3 C15 C16 0.0(8) . . . . ? C19 N3 C15 C14 177.7(5) . . . . ? N1 C14 C15 N3 4.7(8) . . . . ? N1 C14 C15 C16 -177.7(6) . . . . ? N3 C15 C16 C17 0.0(9) . . . . ? C14 C15 C16 C17 -177.6(6) . . . . ? C15 C16 C17 C18 0.7(10) . . . . ? C16 C17 C18 C19 -1.5(10) . . . . ? C15 N3 C19 C18 -0.8(9) . . . . ? C17 C18 C19 N3 1.5(10) . . . . ? C24 N5 C20 C21 0.2(11) . . . . ? Co1 N5 C20 C21 169.7(7) . . . . ? N5 C20 C21 C22 -0.7(14) . . . . ? C20 C21 C22 C23 0.2(13) . . . . ? C21 C22 C23 C24 0.8(11) . . . . ? C20 N5 C24 C23 0.9(9) . . . . ? Co1 N5 C24 C23 -169.4(5) . . . . ? C20 N5 C24 C25 -175.1(6) . . . . ? Co1 N5 C24 C25 14.6(7) . . . . ? C22 C23 C24 N5 -1.4(10) . . . . ? C22 C23 C24 C25 174.5(6) . . . . ? C26 N4 C25 C24 136.4(5) . . . . ? S1 N4 C25 C24 -100.6(5) . . . . ? Co1 N4 C25 C24 21.1(5) . . . . ? N5 C24 C25 N4 -24.9(7) . . . . ? C23 C24 C25 N4 159.1(5) . . . . ? C25 N4 C26 C27 -76.1(6) . . . . ? S1 N4 C26 C27 160.0(4) . . . . ? Co1 N4 C26 C27 40.6(5) . . . . ? C31 N6 C27 C28 0.9(9) . . . . ? Co1 N6 C27 C28 178.6(5) . . . . ? C31 N6 C27 C26 -177.2(6) . . . . ? Co1 N6 C27 C26 0.5(7) . . . . ? N4 C26 C27 N6 -29.8(7) . . . . ? N4 C26 C27 C28 152.1(5) . . . . ? N6 C27 C28 C29 -1.5(10) . . . . ? C26 C27 C28 C29 176.6(6) . . . . ? C27 C28 C29 C30 0.9(11) . . . . ? C28 C29 C30 C31 0.1(12) . . . . ? C27 N6 C31 C30 0.2(10) . . . . ? Co1 N6 C31 C30 -177.3(5) . . . . ? C29 C30 C31 N6 -0.7(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 O6 H62 O1S 0.85 1.92 2.767(11) 177.8 . O6 H61 O2C 0.85 2.12 2.971(8) 178.9 2 O7 H71 O1W 0.85 1.73 2.583(10) 177.6 . O1S H1S O2B 0.85 2.43 3.210(18) 152.7 4_565 O1S H1S O2C 0.85 2.47 3.244(15) 152.6 4_565 N2 H2A N3 0.88 1.84 2.705(8) 166.9 . #======================================================================= data_4 _database_code_depnum_ccdc_archive 'CCDC 737974' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H29 Cl Cu N6 O5 S2, 4(H2 O)' _chemical_formula_sum 'C31 H37 Cl Cu N6 O9 S2' _chemical_formula_weight 800.78 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 12.3780(9) _cell_length_b 12.6820(9) _cell_length_c 12.7179(7) _cell_angle_alpha 114.347(2) _cell_angle_beta 104.098(2) _cell_angle_gamma 92.327(2) _cell_volume 1741.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4109 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.90 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 830 _exptl_absorpt_coefficient_mu 0.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; H atoms on water molecules are placed so as to form a reasonable H-bond network. There must be disorder in this network: it is not possible to place the H atoms in an ordered arrangement. Problems arise particularly for for O1 and its equivalent across the centre of inversion. There are therefore two alternative positions for atoms H1W/H1W' and H3W/H3W', each with 50% site occupancy. This is consistent with the observed 2-fold disorder of the pyridine ring containing N3. Thus, the H-bond network in this region is either: #-------------------------------------------------------------- O1W---H1W'...O2W---H3W'...N3A (i.e. H3W is not present) #-------------------------------------------------------------- OR #-------------------------------------------------------------- C16---H16...O2W---H3W...O1W (i.e. H1W' is not present) #-------------------------------------------------------------- ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 27383 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.976 _reflns_number_total 6012 _reflns_number_gt 3657 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0655P)^2^+0.5641P] 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 6012 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.395 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.078 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 Cu1 Cu 0.64736(4) 0.53390(5) 0.13035(5) 0.03150(19) Uani 1 1 d . . . Cl1 Cl 0.51924(10) 0.65618(11) 0.14855(11) 0.0457(3) Uani 1 1 d . . . S1 S 0.73222(10) 0.71505(10) 0.55719(10) 0.0348(3) Uani 1 1 d . . . S2 S 0.87675(9) 0.42535(10) 0.18055(10) 0.0338(3) Uani 1 1 d . . . O1 O 0.7708(2) 0.6275(2) 0.3107(2) 0.0302(7) Uani 1 1 d . . . O2 O 0.6149(2) 0.7000(3) 0.4966(3) 0.0421(8) Uani 1 1 d . . . O3 O 0.7625(3) 0.7356(3) 0.6821(3) 0.0459(9) Uani 1 1 d . . . O4 O 0.9233(3) 0.3185(3) 0.1472(3) 0.0448(9) Uani 1 1 d . . . O5 O 0.9353(2) 0.5225(3) 0.1768(3) 0.0373(8) Uani 1 1 d . . . N1 N 0.7921(3) 0.8259(3) 0.5514(3) 0.0341(9) Uani 1 1 d . . . N2 N 0.6831(3) 1.0438(4) 0.4555(4) 0.0525(12) Uani 1 1 d . . . N4 N 0.7452(3) 0.3966(3) 0.0786(3) 0.0294(9) Uani 1 1 d . . . N5 N 0.5761(3) 0.4309(3) 0.1848(3) 0.0319(9) Uani 1 1 d . . . N6 N 0.7153(3) 0.5841(3) 0.0308(3) 0.0339(9) Uani 1 1 d . . . C1 C 0.8020(3) 0.5653(4) 0.3671(4) 0.0276(10) Uani 1 1 d . . . C2 C 0.7905(3) 0.5916(4) 0.4837(4) 0.0279(10) Uani 1 1 d . . . C3 C 0.8166(4) 0.5157(4) 0.5371(4) 0.0345(11) Uani 1 1 d . . . H3A H 0.8070 0.5364 0.6147 0.041 Uiso 1 1 calc R . . C4 C 0.8559(3) 0.4118(4) 0.4826(4) 0.0318(11) Uani 1 1 d . . . C5 C 0.8719(3) 0.3854(4) 0.3711(4) 0.0347(11) Uani 1 1 d . . . H5A H 0.8996 0.3153 0.3312 0.042 Uiso 1 1 calc R . . C6 C 0.8479(3) 0.4607(4) 0.3165(4) 0.0289(10) Uani 1 1 d . . . C7 C 0.8804(4) 0.3312(4) 0.5427(5) 0.0474(13) Uani 1 1 d . . . H7A H 0.8581 0.2495 0.4818 0.071 Uiso 1 1 calc R . . H7B H 0.8377 0.3461 0.6016 0.071 Uiso 1 1 calc R . . H7C H 0.9613 0.3456 0.5837 0.071 Uiso 1 1 calc R . . C8 C 0.7387(4) 0.8681(4) 0.4621(4) 0.0416(12) Uani 1 1 d . . . H8A H 0.6771 0.8064 0.3982 0.050 Uiso 1 1 calc R . . H8B H 0.7952 0.8822 0.4241 0.050 Uiso 1 1 calc R . . C9 C 0.6912(4) 0.9792(4) 0.5163(4) 0.0385(12) Uani 1 1 d . . . C10 C 0.6538(4) 1.0102(4) 0.6172(5) 0.0489(14) Uani 1 1 d . . . H10A H 0.6623 0.9631 0.6597 0.059 Uiso 1 1 calc R . . C11 C 0.6046(4) 1.1084(5) 0.6563(5) 0.0589(16) Uani 1 1 d . . . H11A H 0.5767 1.1291 0.7243 0.071 Uiso 1 1 calc R . . C12 C 0.5963(5) 1.1760(5) 0.5958(6) 0.0641(17) Uani 1 1 d . . . H12A H 0.5637 1.2456 0.6216 0.077 Uiso 1 1 calc R . . C13 C 0.6356(5) 1.1420(5) 0.4973(6) 0.0674(17) Uani 1 1 d . . . H13A H 0.6294 1.1896 0.4555 0.081 Uiso 1 1 calc R . . C14 C 0.9140(4) 0.8620(4) 0.6074(4) 0.0453(13) Uani 1 1 d . A . H14A H 0.9527 0.8402 0.5435 0.054 Uiso 1 1 calc R . . H14B H 0.9407 0.8194 0.6563 0.054 Uiso 1 1 calc R . . C15 C 0.9453(4) 0.9918(4) 0.6864(4) 0.0381(12) Uani 1 1 d . . . N3 N 0.9936(4) 1.0610(4) 0.6457(4) 0.0446(11) Uani 0.50 1 d P A 1 C16 C 0.9220(4) 1.0354(4) 0.7936(4) 0.0514(13) Uani 0.50 1 d P A 1 H16 H 0.8881 0.9851 0.8191 0.062 Uiso 0.50 1 calc PR A 1 N3A N 0.9220(4) 1.0354(4) 0.7936(4) 0.0514(13) Uani 0.50 1 d P A 2 C16A C 0.9936(4) 1.0610(4) 0.6457(4) 0.0446(11) Uani 0.50 1 d P A 2 H16A H 1.0077 1.0279 0.5693 0.054 Uiso 0.50 1 calc PR A 2 C17 C 0.9482(4) 1.1527(5) 0.8637(5) 0.0583(16) Uani 1 1 d . . . H17A H 0.9334 1.1846 0.9398 0.070 Uiso 1 1 calc R A 1 C18 C 0.9957(4) 1.2259(5) 0.8267(5) 0.0505(14) Uani 1 1 d . A . H18A H 1.0110 1.3081 0.8754 0.061 Uiso 1 1 calc R . . C19 C 1.0211(4) 1.1794(5) 0.7181(5) 0.0497(14) Uani 1 1 d . . . H19A H 1.0575 1.2291 0.6937 0.060 Uiso 1 1 calc R A 1 C20 C 0.5135(4) 0.4661(4) 0.2621(4) 0.0397(12) Uani 1 1 d . . . H20B H 0.4923 0.5418 0.2841 0.048 Uiso 1 1 calc R . . C21 C 0.4793(4) 0.3971(5) 0.3101(5) 0.0490(14) Uani 1 1 d . . . H21A H 0.4344 0.4240 0.3639 0.059 Uiso 1 1 calc R . . C22 C 0.5101(4) 0.2896(5) 0.2803(5) 0.0564(15) Uani 1 1 d . . . H22A H 0.4866 0.2402 0.3127 0.068 Uiso 1 1 calc R . . C23 C 0.5762(4) 0.2522(5) 0.2020(5) 0.0497(14) Uani 1 1 d . . . H23A H 0.5994 0.1775 0.1808 0.060 Uiso 1 1 calc R . . C24 C 0.6072(4) 0.3253(4) 0.1558(4) 0.0341(11) Uani 1 1 d . . . C25 C 0.6760(4) 0.2911(4) 0.0665(4) 0.0381(12) Uani 1 1 d . . . H25A H 0.7262 0.2365 0.0808 0.046 Uiso 1 1 calc R . . H25B H 0.6247 0.2500 -0.0164 0.046 Uiso 1 1 calc R . . C26 C 0.7620(4) 0.3878(4) -0.0374(4) 0.0354(12) Uani 1 1 d . . . H26A H 0.8330 0.3569 -0.0472 0.042 Uiso 1 1 calc R . . H26B H 0.6989 0.3322 -0.1057 0.042 Uiso 1 1 calc R . . C27 C 0.7673(3) 0.5051(4) -0.0395(4) 0.0322(11) Uani 1 1 d . . . C28 C 0.8190(4) 0.5306(5) -0.1124(4) 0.0430(13) Uani 1 1 d . . . H28A H 0.8573 0.4748 -0.1598 0.052 Uiso 1 1 calc R . . C29 C 0.8152(4) 0.6367(5) -0.1164(5) 0.0537(15) Uani 1 1 d . . . H29A H 0.8496 0.6547 -0.1674 0.064 Uiso 1 1 calc R . . C30 C 0.7608(4) 0.7168(5) -0.0454(5) 0.0513(14) Uani 1 1 d . . . H30A H 0.7567 0.7908 -0.0468 0.062 Uiso 1 1 calc R . . C31 C 0.7131(4) 0.6878(4) 0.0268(4) 0.0422(12) Uani 1 1 d . . . H31A H 0.6766 0.7437 0.0765 0.051 Uiso 1 1 calc R . . O1W O 0.4719(7) 0.9621(5) 0.0834(6) 0.184(3) Uani 1 1 d . . . H1W H 0.4893 0.9839 0.0348 0.276 Uiso 0.50 1 d PR . . H1W' H 0.4125 0.9868 0.0970 0.276 Uiso 0.50 1 d PR . . H2W H 0.5385 0.9683 0.1238 0.276 Uiso 1 1 d R . . O2W O 0.7329(8) 0.9530(5) 0.8721(6) 0.213(4) Uani 1 1 d . . . H3W H 0.6714 0.9708 0.8443 0.320 Uiso 0.50 1 d PR . . H3W' H 0.7815 0.9992 0.8693 0.320 Uiso 0.50 1 d PR . . H4W H 0.7349 0.8879 0.8170 0.320 Uiso 1 1 d R . . O3W O 0.8243(7) 0.0558(6) 0.1175(7) 0.194(3) Uani 1 1 d . . . H5W H 0.8495 0.1221 0.1256 0.292 Uiso 1 1 d R . . H6W H 0.7963 0.0237 0.0423 0.292 Uiso 1 1 d R . . O4W O 0.6921(7) 0.9815(6) 0.2191(6) 0.185(3) Uani 1 1 d . . . H7W H 0.7331 1.0049 0.1857 0.277 Uiso 1 1 d R . . H8W H 0.6890 0.9997 0.2896 0.277 Uiso 1 1 d 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 Cu1 0.0280(3) 0.0370(4) 0.0310(3) 0.0126(3) 0.0141(2) 0.0111(3) Cl1 0.0407(7) 0.0543(8) 0.0458(8) 0.0198(7) 0.0194(6) 0.0250(6) S1 0.0408(7) 0.0354(7) 0.0286(7) 0.0101(6) 0.0168(6) 0.0109(6) S2 0.0291(7) 0.0405(8) 0.0266(7) 0.0078(6) 0.0102(5) 0.0136(6) O1 0.0343(17) 0.0291(18) 0.0269(17) 0.0092(15) 0.0127(14) 0.0106(14) O2 0.0313(19) 0.045(2) 0.046(2) 0.0139(17) 0.0147(16) 0.0102(15) O3 0.062(2) 0.047(2) 0.0270(18) 0.0092(16) 0.0220(16) 0.0157(17) O4 0.0412(19) 0.050(2) 0.0339(19) 0.0070(16) 0.0123(15) 0.0272(17) O5 0.0314(17) 0.049(2) 0.0288(18) 0.0122(16) 0.0130(14) 0.0076(15) N1 0.033(2) 0.032(2) 0.035(2) 0.0110(19) 0.0121(18) 0.0083(18) N2 0.044(3) 0.048(3) 0.072(3) 0.031(3) 0.017(2) 0.018(2) N4 0.030(2) 0.036(2) 0.020(2) 0.0091(17) 0.0094(16) 0.0044(17) N5 0.029(2) 0.035(2) 0.028(2) 0.0111(18) 0.0073(17) 0.0049(18) N6 0.027(2) 0.040(2) 0.032(2) 0.012(2) 0.0083(17) 0.0072(18) C1 0.021(2) 0.027(3) 0.030(3) 0.008(2) 0.007(2) 0.003(2) C2 0.023(2) 0.033(3) 0.023(2) 0.008(2) 0.0056(19) 0.004(2) C3 0.035(3) 0.043(3) 0.023(3) 0.013(2) 0.007(2) 0.003(2) C4 0.030(3) 0.032(3) 0.029(3) 0.010(2) 0.006(2) 0.005(2) C5 0.029(3) 0.031(3) 0.032(3) 0.004(2) 0.005(2) 0.007(2) C6 0.029(3) 0.030(3) 0.022(2) 0.006(2) 0.0058(19) 0.008(2) C7 0.054(3) 0.042(3) 0.049(3) 0.023(3) 0.012(3) 0.014(3) C8 0.045(3) 0.038(3) 0.043(3) 0.015(3) 0.017(2) 0.011(2) C9 0.035(3) 0.034(3) 0.039(3) 0.010(2) 0.008(2) 0.009(2) C10 0.052(3) 0.044(3) 0.047(3) 0.012(3) 0.021(3) 0.020(3) C11 0.051(4) 0.055(4) 0.057(4) 0.009(3) 0.018(3) 0.015(3) C12 0.053(4) 0.046(4) 0.068(4) 0.001(3) 0.016(3) 0.015(3) C13 0.059(4) 0.057(4) 0.090(5) 0.041(4) 0.009(4) 0.017(3) C14 0.051(3) 0.037(3) 0.045(3) 0.012(3) 0.020(3) 0.013(3) C15 0.032(3) 0.044(3) 0.034(3) 0.011(3) 0.012(2) 0.012(2) N3 0.050(3) 0.046(3) 0.041(3) 0.019(3) 0.018(2) 0.009(2) C16 0.061(3) 0.043(3) 0.048(3) 0.010(3) 0.030(3) 0.007(2) N3A 0.061(3) 0.043(3) 0.048(3) 0.010(3) 0.030(3) 0.007(2) C16A 0.050(3) 0.046(3) 0.041(3) 0.019(3) 0.018(2) 0.009(2) C17 0.067(4) 0.050(4) 0.043(3) 0.000(3) 0.027(3) 0.006(3) C18 0.052(3) 0.042(3) 0.045(3) 0.008(3) 0.010(3) 0.009(3) C19 0.057(3) 0.046(4) 0.045(3) 0.019(3) 0.014(3) 0.009(3) C20 0.028(3) 0.050(3) 0.036(3) 0.012(3) 0.014(2) 0.005(2) C21 0.039(3) 0.066(4) 0.050(3) 0.027(3) 0.023(3) 0.006(3) C22 0.051(3) 0.076(4) 0.060(4) 0.045(3) 0.022(3) 0.004(3) C23 0.053(3) 0.050(3) 0.055(4) 0.032(3) 0.015(3) 0.007(3) C24 0.029(3) 0.038(3) 0.028(3) 0.011(2) 0.002(2) -0.003(2) C25 0.042(3) 0.036(3) 0.034(3) 0.012(2) 0.010(2) 0.012(2) C26 0.032(3) 0.046(3) 0.019(2) 0.004(2) 0.010(2) 0.010(2) C27 0.026(2) 0.044(3) 0.023(2) 0.010(2) 0.007(2) 0.008(2) C28 0.037(3) 0.057(4) 0.032(3) 0.016(3) 0.011(2) 0.006(3) C29 0.043(3) 0.080(4) 0.043(3) 0.034(3) 0.010(3) -0.003(3) C30 0.044(3) 0.058(4) 0.057(4) 0.036(3) 0.006(3) 0.002(3) C31 0.038(3) 0.044(3) 0.044(3) 0.021(3) 0.007(2) 0.006(2) O1W 0.274(9) 0.099(5) 0.123(5) 0.030(4) 0.007(5) -0.057(5) O2W 0.406(13) 0.113(5) 0.103(5) 0.033(4) 0.079(6) -0.031(6) O3W 0.248(9) 0.173(7) 0.188(8) 0.091(6) 0.076(7) 0.083(6) O4W 0.336(10) 0.159(6) 0.142(6) 0.090(5) 0.150(7) 0.131(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 Cu1 N6 1.963(4) . ? Cu1 N5 1.978(4) . ? Cu1 N4 2.132(3) . ? Cu1 O1 2.214(3) . ? Cu1 Cl1 2.2485(12) . ? S1 O2 1.432(3) . ? S1 O3 1.447(3) . ? S1 N1 1.600(4) . ? S1 C2 1.749(4) . ? S2 O5 1.428(3) . ? S2 O4 1.434(3) . ? S2 C6 1.730(4) . ? S2 N4 1.731(4) . ? O1 C1 1.280(5) . ? N1 C14 1.464(6) . ? N1 C8 1.476(6) . ? N2 C9 1.330(6) . ? N2 C13 1.357(7) . ? N4 C25 1.491(5) . ? N4 C26 1.500(5) . ? N5 C24 1.335(6) . ? N5 C20 1.343(5) . ? N6 C31 1.339(6) . ? N6 C27 1.346(5) . ? C1 C2 1.425(6) . ? C1 C6 1.426(6) . ? C2 C3 1.397(6) . ? C3 C4 1.384(6) . ? C3 H3A 0.950 . ? C4 C5 1.384(6) . ? C4 C7 1.508(6) . ? C5 C6 1.398(6) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.506(6) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.380(6) . ? C10 C11 1.368(7) . ? C10 H10A 0.950 . ? C11 C12 1.361(8) . ? C11 H11A 0.950 . ? C12 C13 1.364(8) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.505(6) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.354(6) . ? C15 N3 1.371(6) . ? N3 C19 1.372(6) . ? C16 C17 1.356(7) . ? C16 H16 0.950 . ? C17 C18 1.371(7) . ? C17 H17A 0.950 . ? C18 C19 1.382(7) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.362(6) . ? C20 H20B 0.950 . ? C21 C22 1.354(7) . ? C21 H21A 0.950 . ? C22 C23 1.387(7) . ? C22 H22A 0.950 . ? C23 C24 1.373(6) . ? C23 H23A 0.950 . ? C24 C25 1.515(6) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.498(6) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.377(6) . ? C28 C29 1.369(7) . ? C28 H28A 0.950 . ? C29 C30 1.377(7) . ? C29 H29A 0.950 . ? C30 C31 1.360(7) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? O1W H1W 0.840 . ? O1W H1W' 0.840 . ? O1W H2W 0.840 . ? O2W H3W 0.840 . ? O2W H3W' 0.840 . ? O2W H4W 0.840 . ? O3W H5W 0.840 . ? O3W H6W 0.840 . ? O4W H7W 0.840 . ? O4W H8W 0.840 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Cu1 N5 160.44(15) . . ? N6 Cu1 N4 82.54(14) . . ? N5 Cu1 N4 82.52(14) . . ? N6 Cu1 O1 102.28(13) . . ? N5 Cu1 O1 90.70(13) . . ? N4 Cu1 O1 91.67(11) . . ? N6 Cu1 Cl1 95.71(11) . . ? N5 Cu1 Cl1 96.40(11) . . ? N4 Cu1 Cl1 168.45(10) . . ? O1 Cu1 Cl1 99.85(8) . . ? O2 S1 O3 117.63(19) . . ? O2 S1 N1 106.37(19) . . ? O3 S1 N1 107.4(2) . . ? O2 S1 C2 110.60(19) . . ? O3 S1 C2 105.47(19) . . ? N1 S1 C2 109.11(19) . . ? O5 S2 O4 117.66(19) . . ? O5 S2 C6 112.95(19) . . ? O4 S2 C6 109.1(2) . . ? O5 S2 N4 104.35(18) . . ? O4 S2 N4 107.58(18) . . ? C6 S2 N4 104.02(18) . . ? C1 O1 Cu1 116.0(3) . . ? C14 N1 C8 117.3(4) . . ? C14 N1 S1 118.3(3) . . ? C8 N1 S1 121.5(3) . . ? C9 N2 C13 116.7(5) . . ? C25 N4 C26 114.2(3) . . ? C25 N4 S2 110.7(3) . . ? C26 N4 S2 108.2(3) . . ? C25 N4 Cu1 105.2(2) . . ? C26 N4 Cu1 104.8(2) . . ? S2 N4 Cu1 113.80(17) . . ? C24 N5 C20 118.7(4) . . ? C24 N5 Cu1 116.2(3) . . ? C20 N5 Cu1 124.4(3) . . ? C31 N6 C27 118.5(4) . . ? C31 N6 Cu1 125.8(3) . . ? C27 N6 Cu1 115.7(3) . . ? O1 C1 C2 123.4(4) . . ? O1 C1 C6 122.7(4) . . ? C2 C1 C6 113.8(4) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 S1 118.8(3) . . ? C1 C2 S1 119.7(3) . . ? C4 C3 C2 123.2(4) . . ? C4 C3 H3A 118.4 . . ? C2 C3 H3A 118.4 . . ? C5 C4 C3 117.1(4) . . ? C5 C4 C7 121.6(4) . . ? C3 C4 C7 121.3(4) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 123.7(4) . . ? C5 C6 S2 118.0(3) . . ? C1 C6 S2 118.3(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 112.9(4) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C10 122.0(5) . . ? N2 C9 C8 114.4(4) . . ? C10 C9 C8 123.6(5) . . ? C11 C10 C9 120.2(5) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 118.7(6) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? C11 C12 C13 118.7(6) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? N2 C13 C12 123.8(6) . . ? N2 C13 H13A 118.1 . . ? C12 C13 H13A 118.1 . . ? N1 C14 C15 112.3(4) . . ? N1 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N1 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 N3 122.9(4) . . ? C16 C15 C14 118.3(4) . . ? N3 C15 C14 118.8(4) . . ? C15 N3 C19 118.3(4) . . ? C15 C16 C17 118.3(5) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C16 C17 C18 121.1(5) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? N3 C19 C18 119.7(5) . . ? N3 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? N5 C20 C21 122.2(5) . . ? N5 C20 H20B 118.9 . . ? C21 C20 H20B 118.9 . . ? C22 C21 C20 119.3(5) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 119.4(5) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? N5 C24 C23 121.8(4) . . ? N5 C24 C25 115.5(4) . . ? C23 C24 C25 122.7(4) . . ? N4 C25 C24 110.8(3) . . ? N4 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? N4 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 N4 110.9(3) . . ? C27 C26 H26A 109.5 . . ? N4 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? N4 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? N6 C27 C28 121.1(4) . . ? N6 C27 C26 116.7(4) . . ? C28 C27 C26 122.2(4) . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 119.0(5) . . ? C28 C29 H29A 120.5 . . ? C30 C29 H29A 120.5 . . ? C31 C30 C29 118.8(5) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N6 C31 C30 122.9(5) . . ? N6 C31 H31A 118.5 . . ? C30 C31 H31A 118.5 . . ? H1W O1W H1W' 109.3 . . ? H1W O1W H2W 95.7 . . ? H1W' O1W H2W 136.9 . . ? H3W O2W H3W' 103.6 . . ? H3W O2W H4W 103.6 . . ? H3W' O2W H4W 103.6 . . ? H5W O3W H6W 98.3 . . ? H7W O4W H8W 136.7 . . ? 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 N6 Cu1 O1 C1 -131.4(3) . . . . ? N5 Cu1 O1 C1 33.8(3) . . . . ? N4 Cu1 O1 C1 -48.7(3) . . . . ? Cl1 Cu1 O1 C1 130.5(3) . . . . ? O2 S1 N1 C14 179.9(3) . . . . ? O3 S1 N1 C14 53.1(4) . . . . ? C2 S1 N1 C14 -60.8(4) . . . . ? O2 S1 N1 C8 -19.7(4) . . . . ? O3 S1 N1 C8 -146.5(3) . . . . ? C2 S1 N1 C8 99.6(3) . . . . ? O5 S2 N4 C25 176.3(3) . . . . ? O4 S2 N4 C25 50.6(3) . . . . ? C6 S2 N4 C25 -65.1(3) . . . . ? O5 S2 N4 C26 50.6(3) . . . . ? O4 S2 N4 C26 -75.2(3) . . . . ? C6 S2 N4 C26 169.2(3) . . . . ? O5 S2 N4 Cu1 -65.5(2) . . . . ? O4 S2 N4 Cu1 168.81(18) . . . . ? C6 S2 N4 Cu1 53.1(2) . . . . ? N6 Cu1 N4 C25 -145.2(3) . . . . ? N5 Cu1 N4 C25 22.1(3) . . . . ? O1 Cu1 N4 C25 112.6(3) . . . . ? Cl1 Cu1 N4 C25 -63.2(6) . . . . ? N6 Cu1 N4 C26 -24.5(3) . . . . ? N5 Cu1 N4 C26 142.8(3) . . . . ? O1 Cu1 N4 C26 -126.7(2) . . . . ? Cl1 Cu1 N4 C26 57.4(6) . . . . ? N6 Cu1 N4 S2 93.5(2) . . . . ? N5 Cu1 N4 S2 -99.2(2) . . . . ? O1 Cu1 N4 S2 -8.70(19) . . . . ? Cl1 Cu1 N4 S2 175.4(3) . . . . ? N6 Cu1 N5 C24 33.5(6) . . . . ? N4 Cu1 N5 C24 -7.0(3) . . . . ? O1 Cu1 N5 C24 -98.6(3) . . . . ? Cl1 Cu1 N5 C24 161.4(3) . . . . ? N6 Cu1 N5 C20 -156.8(4) . . . . ? N4 Cu1 N5 C20 162.7(4) . . . . ? O1 Cu1 N5 C20 71.1(3) . . . . ? Cl1 Cu1 N5 C20 -28.9(4) . . . . ? N5 Cu1 N6 C31 151.9(4) . . . . ? N4 Cu1 N6 C31 -167.6(4) . . . . ? O1 Cu1 N6 C31 -77.5(4) . . . . ? Cl1 Cu1 N6 C31 23.9(4) . . . . ? N5 Cu1 N6 C27 -27.6(6) . . . . ? N4 Cu1 N6 C27 12.9(3) . . . . ? O1 Cu1 N6 C27 103.0(3) . . . . ? Cl1 Cu1 N6 C27 -155.6(3) . . . . ? Cu1 O1 C1 C2 -123.0(4) . . . . ? Cu1 O1 C1 C6 54.6(4) . . . . ? O1 C1 C2 C3 174.4(4) . . . . ? C6 C1 C2 C3 -3.5(6) . . . . ? O1 C1 C2 S1 -0.6(6) . . . . ? C6 C1 C2 S1 -178.4(3) . . . . ? O2 S1 C2 C3 -106.9(4) . . . . ? O3 S1 C2 C3 21.3(4) . . . . ? N1 S1 C2 C3 136.4(3) . . . . ? O2 S1 C2 C1 68.1(4) . . . . ? O3 S1 C2 C1 -163.7(3) . . . . ? N1 S1 C2 C1 -48.5(4) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? S1 C2 C3 C4 175.5(3) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C2 C3 C4 C7 -178.5(4) . . . . ? C3 C4 C5 C6 -0.7(6) . . . . ? C7 C4 C5 C6 179.5(4) . . . . ? C4 C5 C6 C1 -2.5(7) . . . . ? C4 C5 C6 S2 176.8(3) . . . . ? O1 C1 C6 C5 -173.4(4) . . . . ? C2 C1 C6 C5 4.5(6) . . . . ? O1 C1 C6 S2 7.3(6) . . . . ? C2 C1 C6 S2 -174.9(3) . . . . ? O5 S2 C6 C5 -133.0(3) . . . . ? O4 S2 C6 C5 -0.2(4) . . . . ? N4 S2 C6 C5 114.4(3) . . . . ? O5 S2 C6 C1 46.4(4) . . . . ? O4 S2 C6 C1 179.3(3) . . . . ? N4 S2 C6 C1 -66.2(4) . . . . ? C14 N1 C8 C9 -94.0(5) . . . . ? S1 N1 C8 C9 105.4(4) . . . . ? C13 N2 C9 C10 -0.2(7) . . . . ? C13 N2 C9 C8 176.8(4) . . . . ? N1 C8 C9 N2 155.1(4) . . . . ? N1 C8 C9 C10 -28.0(6) . . . . ? N2 C9 C10 C11 1.3(8) . . . . ? C8 C9 C10 C11 -175.4(5) . . . . ? C9 C10 C11 C12 -1.8(8) . . . . ? C10 C11 C12 C13 1.1(8) . . . . ? C9 N2 C13 C12 -0.4(8) . . . . ? C11 C12 C13 N2 0.0(9) . . . . ? C8 N1 C14 C15 66.6(5) . . . . ? S1 N1 C14 C15 -132.2(4) . . . . ? N1 C14 C15 C16 73.2(6) . . . . ? N1 C14 C15 N3 -105.4(5) . . . . ? C16 C15 N3 C19 1.1(7) . . . . ? C14 C15 N3 C19 179.6(4) . . . . ? N3 C15 C16 C17 -0.3(8) . . . . ? C14 C15 C16 C17 -178.8(5) . . . . ? C15 C16 C17 C18 0.9(8) . . . . ? C16 C17 C18 C19 -2.4(8) . . . . ? C15 N3 C19 C18 -2.5(7) . . . . ? C17 C18 C19 N3 3.2(8) . . . . ? C24 N5 C20 C21 -1.1(7) . . . . ? Cu1 N5 C20 C21 -170.6(4) . . . . ? N5 C20 C21 C22 0.7(8) . . . . ? C20 C21 C22 C23 0.3(8) . . . . ? C21 C22 C23 C24 -0.8(8) . . . . ? C20 N5 C24 C23 0.5(6) . . . . ? Cu1 N5 C24 C23 170.9(4) . . . . ? C20 N5 C24 C25 179.0(4) . . . . ? Cu1 N5 C24 C25 -10.7(5) . . . . ? C22 C23 C24 N5 0.4(7) . . . . ? C22 C23 C24 C25 -177.9(4) . . . . ? C26 N4 C25 C24 -147.0(4) . . . . ? S2 N4 C25 C24 90.7(4) . . . . ? Cu1 N4 C25 C24 -32.7(4) . . . . ? N5 C24 C25 N4 30.5(5) . . . . ? C23 C24 C25 N4 -151.1(4) . . . . ? C25 N4 C26 C27 146.4(4) . . . . ? S2 N4 C26 C27 -89.9(3) . . . . ? Cu1 N4 C26 C27 31.8(4) . . . . ? C31 N6 C27 C28 1.2(6) . . . . ? Cu1 N6 C27 C28 -179.4(3) . . . . ? C31 N6 C27 C26 -176.6(4) . . . . ? Cu1 N6 C27 C26 2.9(5) . . . . ? N4 C26 C27 N6 -25.0(5) . . . . ? N4 C26 C27 C28 157.2(4) . . . . ? N6 C27 C28 C29 -1.8(7) . . . . ? C26 C27 C28 C29 175.9(4) . . . . ? C27 C28 C29 C30 1.0(7) . . . . ? C28 C29 C30 C31 0.3(7) . . . . ? C27 N6 C31 C30 0.2(7) . . . . ? Cu1 N6 C31 C30 -179.2(4) . . . . ? C29 C30 C31 N6 -0.9(7) . . . . ? 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 O1W H2W O4W 0.84 1.95 2.788(11) 179.1 . O1W H1W O1W 0.84 2.03 2.872(13) 178.8 2_675 O1W H1W' O2W 0.84 2.05 2.886(12) 179.1 2_676 O2W H4W O3 0.84 2.10 2.931(7) 171.9 . O2W H3W O1W 0.84 2.23 2.886(12) 134.6 2_676 O2W H3W' N3A 0.84 2.30 3.060(9) 151.2 . O3W H5W O4 0.84 2.50 3.338(8) 179.4 . O3W H6W O2W 0.84 1.90 2.743(10) 179.2 1_544 O4W H8W N2 0.84 1.97 2.809(8) 179.4 . O4W H7W O3W 0.84 1.82 2.673(10) 178.6 1_565 #======================================================================= data_5 _database_code_depnum_ccdc_archive 'CCDC 737975' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H30 Cl2 Cu N6 O5 S2, 2(C2 H3 N)' _chemical_formula_sum 'C35 H36 Cl2 Cu N8 O5 S2' _chemical_formula_weight 847.28 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.2665(16) _cell_length_b 23.398(3) _cell_length_c 9.6361(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.029(4) _cell_angle_gamma 90.00 _cell_volume 3741.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5835 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 20.01 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Lattice approximates orthorhombic-C and the crystal is pseudo-merohedrally twinned. Twin law: [1 0 1 0 -1 0 0 0 -1], refined BASF: 0.1453(6) The twin operation corresponds to 2-fold rotation around a* (i.e. the normal to the bc plane in direct space) in the monoclinic lattice as it is described here. H atom bound to N3 was visible in a difference Fourier map, but placed geometrically for final refinement. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 59920 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.07 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 6629 _reflns_number_gt 4884 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0463P)^2^] 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 6629 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.294 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.066 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 Cu1 Cu 0.80377(3) 0.432999(18) 0.17942(5) 0.02605(13) Uani 1 1 d . . . Cl1 Cl 0.90366(5) 0.36371(4) 0.27609(11) 0.0297(2) Uani 1 1 d . . . Cl2 Cl 0.81393(6) 0.49179(4) -0.00157(11) 0.0395(3) Uani 1 1 d . . . S1 S 0.43929(5) 0.32122(4) 0.53903(10) 0.0227(2) Uani 1 1 d . . . S2 S 0.64201(5) 0.45199(4) 0.31205(10) 0.0223(2) Uani 1 1 d . . . O1 O 0.53480(13) 0.34704(10) 0.3279(3) 0.0249(6) Uani 1 1 d . . . O2 O 0.47671(13) 0.26831(9) 0.5226(3) 0.0312(6) Uani 1 1 d . . . O3 O 0.40836(14) 0.32838(10) 0.6618(3) 0.0290(6) Uani 1 1 d . . . O4 O 0.59080(14) 0.43909(10) 0.1718(3) 0.0278(6) Uani 1 1 d . . . O5 O 0.67183(14) 0.50915(9) 0.3435(3) 0.0284(6) Uani 1 1 d . . . N1 N 0.36491(15) 0.33066(11) 0.3943(3) 0.0204(7) Uani 1 1 d . . . N2 N 0.16969(18) 0.33222(15) 0.2909(4) 0.0447(9) Uani 1 1 d . . . N3 N 0.40960(18) 0.34928(12) 0.1163(3) 0.0263(7) Uani 1 1 d . . . H3B H 0.4554 0.3443 0.1833 0.032 Uiso 1 1 calc R . . N4 N 0.72560(15) 0.41176(11) 0.3307(3) 0.0198(7) Uani 1 1 d . . . N5 N 0.72942(16) 0.37602(12) 0.0588(3) 0.0252(7) Uani 1 1 d . . . N6 N 0.85116(16) 0.48573(12) 0.3433(3) 0.0247(7) Uani 1 1 d . . . C1 C 0.54491(19) 0.38377(15) 0.4314(4) 0.0208(8) Uani 1 1 d . . . C2 C 0.59683(19) 0.43237(14) 0.4479(4) 0.0195(8) Uani 1 1 d . . . C3 C 0.60995(19) 0.46849(14) 0.5660(4) 0.0200(8) Uani 1 1 d . . . H3A H 0.6456 0.4999 0.5721 0.024 Uiso 1 1 calc R . . C4 C 0.5734(2) 0.46073(15) 0.6752(4) 0.0231(9) Uani 1 1 d . . . C5 C 0.5199(2) 0.41535(15) 0.6592(4) 0.0250(9) Uani 1 1 d . . . H5A H 0.4921 0.4096 0.7304 0.030 Uiso 1 1 calc R . . C6 C 0.50575(18) 0.37843(14) 0.5437(4) 0.0198(8) Uani 1 1 d . . . C7 C 0.5902(2) 0.49993(16) 0.8047(4) 0.0343(10) Uani 1 1 d . . . H7A H 0.6485 0.5053 0.8432 0.051 Uiso 1 1 d R . . H7B H 0.5687 0.4829 0.8793 0.051 Uiso 1 1 d R . . H7C H 0.5644 0.5370 0.7758 0.051 Uiso 1 1 d R . . C8 C 0.30133(19) 0.37171(14) 0.3983(4) 0.0220(8) Uani 1 1 d . . . H8A H 0.2881 0.3948 0.3087 0.026 Uiso 1 1 calc R . . H8B H 0.3215 0.3980 0.4809 0.026 Uiso 1 1 calc R . . C9 C 0.2259(2) 0.34260(15) 0.4124(4) 0.0276(9) Uani 1 1 d . . . C10 C 0.2178(2) 0.32789(18) 0.5469(5) 0.0418(11) Uani 1 1 d . . . H10A H 0.2598 0.3359 0.6318 0.050 Uiso 1 1 calc R . . C11 C 0.1481(3) 0.3015(2) 0.5560(6) 0.0608(15) Uani 1 1 d . . . H11A H 0.1407 0.2917 0.6472 0.073 Uiso 1 1 calc R . . C12 C 0.0896(3) 0.28976(19) 0.4309(7) 0.0583(15) Uani 1 1 d . . . H12A H 0.0412 0.2710 0.4332 0.070 Uiso 1 1 calc R . . C13 C 0.1025(2) 0.3056(2) 0.3033(6) 0.0598(15) Uani 1 1 d . . . H13A H 0.0615 0.2974 0.2172 0.072 Uiso 1 1 calc R . . C14 C 0.3509(2) 0.29199(15) 0.2707(4) 0.0243(9) Uani 1 1 d . . . H14A H 0.3010 0.2698 0.2628 0.029 Uiso 1 1 calc R . . H14B H 0.3963 0.2648 0.2856 0.029 Uiso 1 1 calc R . . C15 C 0.3428(2) 0.32472(15) 0.1339(4) 0.0257(9) Uani 1 1 d . . . C16 C 0.2705(2) 0.33373(18) 0.0314(4) 0.0400(11) Uani 1 1 d . . . H16A H 0.2225 0.3166 0.0415 0.048 Uiso 1 1 calc R . . C17 C 0.2687(3) 0.3680(2) -0.0865(5) 0.0502(12) Uani 1 1 d . . . H17A H 0.2190 0.3755 -0.1563 0.060 Uiso 1 1 calc R . . C18 C 0.3390(3) 0.39120(17) -0.1027(4) 0.0408(11) Uani 1 1 d . . . H18A H 0.3386 0.4139 -0.1847 0.049 Uiso 1 1 calc R . . C19 C 0.4092(3) 0.38090(16) 0.0012(4) 0.0349(10) Uani 1 1 d . . . H19A H 0.4582 0.3964 -0.0087 0.042 Uiso 1 1 calc R . . C20 C 0.7182(2) 0.36714(16) -0.0834(4) 0.0300(9) Uani 1 1 d . . . H20A H 0.7476 0.3896 -0.1333 0.036 Uiso 1 1 calc R . . C21 C 0.6654(2) 0.32653(16) -0.1589(4) 0.0337(10) Uani 1 1 d . . . H21A H 0.6599 0.3203 -0.2586 0.040 Uiso 1 1 calc R . . C22 C 0.6206(2) 0.29491(17) -0.0878(5) 0.0358(10) Uani 1 1 d . . . H22A H 0.5825 0.2675 -0.1381 0.043 Uiso 1 1 calc R . . C23 C 0.6324(2) 0.30404(15) 0.0579(4) 0.0290(9) Uani 1 1 d . . . H23A H 0.6022 0.2828 0.1090 0.035 Uiso 1 1 calc R . . C24 C 0.68753(19) 0.34358(14) 0.1288(4) 0.0199(8) Uani 1 1 d . . . C25 C 0.7077(2) 0.35054(14) 0.2891(4) 0.0240(9) Uani 1 1 d . . . H25A H 0.7551 0.3267 0.3357 0.029 Uiso 1 1 calc R . . H25B H 0.6618 0.3373 0.3237 0.029 Uiso 1 1 calc R . . C26 C 0.7857(2) 0.42102(15) 0.4717(4) 0.0249(9) Uani 1 1 d . . . H26A H 0.8212 0.3871 0.4961 0.030 Uiso 1 1 calc R . . H26B H 0.7575 0.4255 0.5477 0.030 Uiso 1 1 calc R . . C27 C 0.83654(19) 0.47367(15) 0.4692(4) 0.0241(9) Uani 1 1 d . . . C28 C 0.8688(2) 0.50497(16) 0.5920(4) 0.0325(10) Uani 1 1 d . . . H28A H 0.8557 0.4964 0.6792 0.039 Uiso 1 1 calc R . . C29 C 0.9211(2) 0.54945(17) 0.5859(5) 0.0380(11) Uani 1 1 d . . . H29A H 0.9461 0.5708 0.6703 0.046 Uiso 1 1 calc R . . C30 C 0.9361(2) 0.56219(16) 0.4579(5) 0.0358(10) Uani 1 1 d . . . H30A H 0.9709 0.5929 0.4516 0.043 Uiso 1 1 calc R . . C31 C 0.9003(2) 0.53017(15) 0.3383(5) 0.0299(9) Uani 1 1 d . . . H31A H 0.9104 0.5395 0.2489 0.036 Uiso 1 1 calc R . . N1S N 0.7963(3) 0.2967(2) 0.6582(6) 0.1034(19) Uani 1 1 d . . . C1S C 0.8365(3) 0.2742(2) 0.6029(5) 0.0547(13) Uani 1 1 d . . . C2S C 0.8855(3) 0.2469(2) 0.5259(5) 0.0640(14) Uani 1 1 d . . . H2S1 H 0.8530 0.2384 0.4274 0.096 Uiso 1 1 d R . . H2S2 H 0.9069 0.2112 0.5749 0.096 Uiso 1 1 d R . . H2S3 H 0.9301 0.2722 0.5225 0.096 Uiso 1 1 d R . . N2S N 0.9708(5) 0.6569(2) 0.1980(8) 0.138(3) Uani 1 1 d . . . C3S C 0.9837(3) 0.6271(2) 0.1161(7) 0.0676(16) Uani 1 1 d . . . C4S C 0.9980(4) 0.5890(3) 0.0115(7) 0.096(2) Uani 1 1 d . . . H4S1 H 1.0364 0.5595 0.0597 0.144 Uiso 1 1 d R . . H4S2 H 1.0203 0.6102 -0.0563 0.144 Uiso 1 1 d R . . H4S3 H 0.9472 0.5709 -0.0413 0.144 Uiso 1 1 d 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 Cu1 0.0233(2) 0.0239(2) 0.0309(3) -0.0013(2) 0.0073(2) -0.0065(2) Cl1 0.0198(5) 0.0266(5) 0.0413(6) -0.0034(4) 0.0061(4) -0.0004(4) Cl2 0.0398(6) 0.0392(6) 0.0398(6) 0.0074(5) 0.0113(5) -0.0118(5) S1 0.0185(4) 0.0221(5) 0.0285(6) 0.0064(4) 0.0083(4) 0.0006(4) S2 0.0190(5) 0.0208(5) 0.0290(6) 0.0031(4) 0.0100(4) -0.0003(4) O1 0.0230(13) 0.0241(14) 0.0330(15) -0.0072(12) 0.0165(11) -0.0051(11) O2 0.0250(13) 0.0193(14) 0.0494(17) 0.0082(13) 0.0107(12) 0.0049(11) O3 0.0252(13) 0.0394(16) 0.0261(15) 0.0086(12) 0.0135(12) -0.0043(12) O4 0.0202(13) 0.0364(16) 0.0273(15) 0.0044(12) 0.0072(12) 0.0030(11) O5 0.0272(13) 0.0191(14) 0.0416(16) 0.0038(12) 0.0142(12) -0.0030(11) N1 0.0178(14) 0.0212(16) 0.0240(17) -0.0041(14) 0.0092(13) 0.0029(13) N2 0.0216(18) 0.059(2) 0.052(2) -0.015(2) 0.0075(17) -0.0027(17) N3 0.0327(18) 0.0234(18) 0.0242(19) -0.0022(15) 0.0103(14) 0.0002(15) N4 0.0162(15) 0.0173(16) 0.0253(17) -0.0014(13) 0.0049(13) -0.0032(12) N5 0.0169(15) 0.0262(17) 0.032(2) -0.0003(15) 0.0059(14) -0.0008(13) N6 0.0191(16) 0.0212(17) 0.034(2) -0.0004(15) 0.0079(14) -0.0013(14) C1 0.0174(18) 0.022(2) 0.024(2) -0.0009(17) 0.0071(16) 0.0019(16) C2 0.0145(18) 0.021(2) 0.024(2) 0.0021(17) 0.0060(15) 0.0019(15) C3 0.0173(18) 0.0179(19) 0.023(2) -0.0017(17) 0.0032(16) 0.0002(15) C4 0.0164(19) 0.026(2) 0.026(2) -0.0021(17) 0.0049(17) 0.0041(16) C5 0.0193(19) 0.030(2) 0.028(2) 0.0052(18) 0.0107(17) 0.0066(17) C6 0.0142(17) 0.0181(19) 0.027(2) 0.0010(17) 0.0056(16) 0.0019(15) C7 0.028(2) 0.036(2) 0.038(2) -0.009(2) 0.0076(19) 0.0014(18) C8 0.0206(19) 0.0172(19) 0.029(2) 0.0003(17) 0.0088(16) 0.0027(15) C9 0.0193(19) 0.020(2) 0.043(3) 0.0015(19) 0.0084(19) 0.0068(16) C10 0.028(2) 0.054(3) 0.046(3) 0.015(2) 0.016(2) 0.000(2) C11 0.033(3) 0.062(3) 0.096(4) 0.030(3) 0.032(3) 0.010(2) C12 0.026(3) 0.040(3) 0.117(5) -0.001(3) 0.032(3) 0.000(2) C13 0.022(2) 0.070(3) 0.086(4) -0.037(3) 0.012(3) -0.008(2) C14 0.027(2) 0.020(2) 0.029(2) -0.0033(17) 0.0140(17) -0.0015(16) C15 0.031(2) 0.023(2) 0.025(2) -0.0062(17) 0.0101(18) 0.0046(18) C16 0.033(2) 0.053(3) 0.037(3) 0.000(2) 0.014(2) 0.001(2) C17 0.049(3) 0.071(3) 0.030(3) 0.011(2) 0.011(2) 0.022(3) C18 0.066(3) 0.035(2) 0.026(2) 0.007(2) 0.019(2) 0.009(2) C19 0.051(3) 0.030(2) 0.029(3) -0.004(2) 0.020(2) -0.003(2) C20 0.027(2) 0.038(2) 0.025(2) 0.0001(19) 0.0079(18) 0.0013(18) C21 0.031(2) 0.039(3) 0.027(2) -0.006(2) 0.0005(19) 0.004(2) C22 0.024(2) 0.031(2) 0.046(3) -0.010(2) -0.0013(19) -0.0022(18) C23 0.0204(19) 0.025(2) 0.042(3) -0.0032(19) 0.0082(18) -0.0030(17) C24 0.0167(17) 0.0173(18) 0.027(2) 0.0002(17) 0.0084(16) 0.0000(15) C25 0.0216(19) 0.017(2) 0.037(2) 0.0042(17) 0.0136(17) 0.0003(15) C26 0.025(2) 0.024(2) 0.026(2) 0.0012(17) 0.0081(17) -0.0012(16) C27 0.0172(19) 0.020(2) 0.033(2) -0.0052(18) 0.0040(17) 0.0011(16) C28 0.028(2) 0.032(2) 0.036(3) -0.0071(19) 0.0067(19) 0.0001(19) C29 0.029(2) 0.031(2) 0.049(3) -0.016(2) 0.002(2) -0.0021(19) C30 0.026(2) 0.023(2) 0.058(3) -0.006(2) 0.010(2) -0.0050(17) C31 0.0211(19) 0.023(2) 0.045(3) -0.003(2) 0.0097(18) -0.0012(18) N1S 0.129(5) 0.098(4) 0.108(4) 0.038(3) 0.074(4) 0.044(4) C1S 0.060(3) 0.051(3) 0.058(3) 0.026(3) 0.025(3) 0.011(3) C2S 0.074(3) 0.060(3) 0.065(4) 0.025(3) 0.031(3) 0.015(3) N2S 0.246(8) 0.068(4) 0.145(6) 0.000(4) 0.132(6) -0.010(4) C3S 0.092(4) 0.050(4) 0.080(4) 0.014(3) 0.055(4) -0.002(3) C4S 0.129(6) 0.082(4) 0.102(5) -0.011(4) 0.072(5) -0.015(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 Cu1 N5 1.988(3) . ? Cu1 N6 1.993(3) . ? Cu1 Cl2 2.2658(11) . ? Cu1 N4 2.298(3) . ? Cu1 Cl1 2.3631(10) . ? S1 O2 1.425(2) . ? S1 O3 1.436(3) . ? S1 N1 1.629(3) . ? S1 C6 1.756(3) . ? S2 O4 1.428(3) . ? S2 O5 1.435(2) . ? S2 N4 1.691(3) . ? S2 C2 1.760(3) . ? O1 C1 1.292(4) . ? N1 C14 1.461(4) . ? N1 C8 1.467(4) . ? N2 C9 1.320(5) . ? N2 C13 1.351(5) . ? N3 C19 1.332(5) . ? N3 C15 1.340(4) . ? N3 H3B 0.880 . ? N4 C26 1.480(4) . ? N4 C25 1.497(4) . ? N5 C20 1.346(5) . ? N5 C24 1.350(4) . ? N6 C27 1.336(4) . ? N6 C31 1.351(4) . ? C1 C2 1.429(5) . ? C1 C6 1.431(5) . ? C2 C3 1.385(5) . ? C3 C4 1.380(5) . ? C3 H3A 0.950 . ? C4 C5 1.388(5) . ? C4 C7 1.511(5) . ? C5 C6 1.376(5) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.509(5) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.385(5) . ? C10 C11 1.376(6) . ? C10 H10A 0.950 . ? C11 C12 1.370(7) . ? C11 H11A 0.950 . ? C12 C13 1.359(7) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.497(5) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.378(5) . ? C16 C17 1.383(6) . ? C16 H16A 0.950 . ? C17 C18 1.377(6) . ? C17 H17A 0.950 . ? C18 C19 1.364(5) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.377(5) . ? C20 H20A 0.950 . ? C21 C22 1.382(5) . ? C21 H21A 0.950 . ? C22 C23 1.378(5) . ? C22 H22A 0.950 . ? C23 C24 1.368(5) . ? C23 H23A 0.950 . ? C24 C25 1.495(5) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.517(5) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.372(5) . ? C28 C29 1.389(5) . ? C28 H28A 0.950 . ? C29 C30 1.361(6) . ? C29 H29A 0.950 . ? C30 C31 1.371(5) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? N1S C1S 1.116(6) . ? C1S C2S 1.421(7) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? N2S C3S 1.121(7) . ? C3S C4S 1.417(8) . ? C4S H4S1 0.980 . ? C4S H4S2 0.980 . ? C4S H4S3 0.980 . ? 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 N5 Cu1 N6 159.38(12) . . ? N5 Cu1 Cl2 97.59(9) . . ? N6 Cu1 Cl2 97.57(9) . . ? N5 Cu1 N4 80.11(11) . . ? N6 Cu1 N4 79.39(11) . . ? Cl2 Cu1 N4 143.47(7) . . ? N5 Cu1 Cl1 93.07(8) . . ? N6 Cu1 Cl1 90.98(8) . . ? Cl2 Cu1 Cl1 121.11(4) . . ? N4 Cu1 Cl1 95.40(7) . . ? O2 S1 O3 118.42(15) . . ? O2 S1 N1 107.28(14) . . ? O3 S1 N1 107.76(14) . . ? O2 S1 C6 110.61(15) . . ? O3 S1 C6 106.21(16) . . ? N1 S1 C6 105.89(15) . . ? O4 S2 O5 119.27(15) . . ? O4 S2 N4 105.69(14) . . ? O5 S2 N4 104.50(14) . . ? O4 S2 C2 111.28(15) . . ? O5 S2 C2 107.03(16) . . ? N4 S2 C2 108.45(15) . . ? C14 N1 C8 118.0(3) . . ? C14 N1 S1 121.9(2) . . ? C8 N1 S1 119.0(2) . . ? C9 N2 C13 116.4(4) . . ? C19 N3 C15 122.4(3) . . ? C19 N3 H3B 118.8 . . ? C15 N3 H3B 118.8 . . ? C26 N4 C25 115.3(3) . . ? C26 N4 S2 112.2(2) . . ? C25 N4 S2 113.4(2) . . ? C26 N4 Cu1 99.52(18) . . ? C25 N4 Cu1 98.71(19) . . ? S2 N4 Cu1 116.48(14) . . ? C20 N5 C24 118.4(3) . . ? C20 N5 Cu1 125.9(2) . . ? C24 N5 Cu1 115.7(2) . . ? C27 N6 C31 118.2(3) . . ? C27 N6 Cu1 116.7(2) . . ? C31 N6 Cu1 124.9(3) . . ? O1 C1 C2 124.2(3) . . ? O1 C1 C6 122.3(3) . . ? C2 C1 C6 113.5(3) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 S2 116.5(3) . . ? C1 C2 S2 121.2(3) . . ? C4 C3 C2 122.7(3) . . ? C4 C3 H3A 118.6 . . ? C2 C3 H3A 118.6 . . ? C3 C4 C5 116.5(3) . . ? C3 C4 C7 121.7(3) . . ? C5 C4 C7 121.8(3) . . ? C6 C5 C4 122.3(3) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C5 C6 C1 122.7(3) . . ? C5 C6 S1 117.9(3) . . ? C1 C6 S1 119.3(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 112.2(3) . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C10 123.0(3) . . ? N2 C9 C8 116.4(3) . . ? C10 C9 C8 120.6(3) . . ? C11 C10 C9 119.1(4) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 118.6(5) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? C13 C12 C11 118.5(4) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? N2 C13 C12 124.3(5) . . ? N2 C13 H13A 117.8 . . ? C12 C13 H13A 117.8 . . ? N1 C14 C15 110.8(3) . . ? N1 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N3 C15 C16 119.0(3) . . ? N3 C15 C14 117.2(3) . . ? C16 C15 C14 123.7(3) . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 118.6(4) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? N3 C19 C18 120.6(4) . . ? N3 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? N5 C20 C21 122.2(4) . . ? N5 C20 H20A 118.9 . . ? C21 C20 H20A 118.9 . . ? C20 C21 C22 119.1(4) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 118.4(4) . . ? C23 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? N5 C24 C23 121.7(3) . . ? N5 C24 C25 116.8(3) . . ? C23 C24 C25 121.4(3) . . ? C24 C25 N4 110.7(3) . . ? C24 C25 H25A 109.5 . . ? N4 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? N4 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N4 C26 C27 111.5(3) . . ? N4 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? N4 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? N6 C27 C28 122.5(3) . . ? N6 C27 C26 116.2(3) . . ? C28 C27 C26 121.2(3) . . ? C27 C28 C29 118.5(4) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? C30 C29 C28 119.4(4) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C29 C30 C31 119.2(4) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? N6 C31 C30 122.2(4) . . ? N6 C31 H31A 118.9 . . ? C30 C31 H31A 118.9 . . ? N1S C1S C2S 177.1(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.4 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.4 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 178.6(8) . . ? C3S C4S H4S1 109.4 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 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 O2 S1 N1 C14 -5.9(3) . . . . ? O3 S1 N1 C14 -134.5(2) . . . . ? C6 S1 N1 C14 112.2(3) . . . . ? O2 S1 N1 C8 161.7(2) . . . . ? O3 S1 N1 C8 33.2(3) . . . . ? C6 S1 N1 C8 -80.1(3) . . . . ? O4 S2 N4 C26 179.3(2) . . . . ? O5 S2 N4 C26 52.6(2) . . . . ? C2 S2 N4 C26 -61.3(2) . . . . ? O4 S2 N4 C25 -48.0(3) . . . . ? O5 S2 N4 C25 -174.7(2) . . . . ? C2 S2 N4 C25 71.4(3) . . . . ? O4 S2 N4 Cu1 65.56(17) . . . . ? O5 S2 N4 Cu1 -61.11(17) . . . . ? C2 S2 N4 Cu1 -175.02(15) . . . . ? N5 Cu1 N4 C26 149.7(2) . . . . ? N6 Cu1 N4 C26 -32.46(19) . . . . ? Cl2 Cu1 N4 C26 -120.88(18) . . . . ? Cl1 Cu1 N4 C26 57.53(18) . . . . ? N5 Cu1 N4 C25 32.09(19) . . . . ? N6 Cu1 N4 C25 -150.1(2) . . . . ? Cl2 Cu1 N4 C25 121.51(18) . . . . ? Cl1 Cu1 N4 C25 -60.09(18) . . . . ? N5 Cu1 N4 S2 -89.56(16) . . . . ? N6 Cu1 N4 S2 88.27(16) . . . . ? Cl2 Cu1 N4 S2 -0.1(2) . . . . ? Cl1 Cu1 N4 S2 178.26(13) . . . . ? N6 Cu1 N5 C20 158.4(3) . . . . ? Cl2 Cu1 N5 C20 21.4(3) . . . . ? N4 Cu1 N5 C20 164.5(3) . . . . ? Cl1 Cu1 N5 C20 -100.6(3) . . . . ? N6 Cu1 N5 C24 -22.1(5) . . . . ? Cl2 Cu1 N5 C24 -159.1(2) . . . . ? N4 Cu1 N5 C24 -16.0(2) . . . . ? Cl1 Cu1 N5 C24 79.0(2) . . . . ? N5 Cu1 N6 C27 25.0(5) . . . . ? Cl2 Cu1 N6 C27 162.0(2) . . . . ? N4 Cu1 N6 C27 18.9(2) . . . . ? Cl1 Cu1 N6 C27 -76.4(2) . . . . ? N5 Cu1 N6 C31 -159.1(3) . . . . ? Cl2 Cu1 N6 C31 -22.1(3) . . . . ? N4 Cu1 N6 C31 -165.2(3) . . . . ? Cl1 Cu1 N6 C31 99.5(3) . . . . ? O1 C1 C2 C3 -175.6(3) . . . . ? C6 C1 C2 C3 3.0(5) . . . . ? O1 C1 C2 S2 8.8(5) . . . . ? C6 C1 C2 S2 -172.6(2) . . . . ? O4 S2 C2 C3 -142.6(3) . . . . ? O5 S2 C2 C3 -10.7(3) . . . . ? N4 S2 C2 C3 101.5(3) . . . . ? O4 S2 C2 C1 33.2(3) . . . . ? O5 S2 C2 C1 165.1(3) . . . . ? N4 S2 C2 C1 -82.6(3) . . . . ? C1 C2 C3 C4 -0.8(5) . . . . ? S2 C2 C3 C4 175.0(3) . . . . ? C2 C3 C4 C5 -2.0(5) . . . . ? C2 C3 C4 C7 178.5(3) . . . . ? C3 C4 C5 C6 2.4(5) . . . . ? C7 C4 C5 C6 -178.2(3) . . . . ? C4 C5 C6 C1 0.1(5) . . . . ? C4 C5 C6 S1 177.8(3) . . . . ? O1 C1 C6 C5 175.9(3) . . . . ? C2 C1 C6 C5 -2.7(5) . . . . ? O1 C1 C6 S1 -1.8(4) . . . . ? C2 C1 C6 S1 179.6(2) . . . . ? O2 S1 C6 C5 -125.9(3) . . . . ? O3 S1 C6 C5 3.8(3) . . . . ? N1 S1 C6 C5 118.2(3) . . . . ? O2 S1 C6 C1 51.9(3) . . . . ? O3 S1 C6 C1 -178.4(3) . . . . ? N1 S1 C6 C1 -64.0(3) . . . . ? C14 N1 C8 C9 65.7(4) . . . . ? S1 N1 C8 C9 -102.4(3) . . . . ? C13 N2 C9 C10 -0.5(6) . . . . ? C13 N2 C9 C8 179.3(3) . . . . ? N1 C8 C9 N2 -94.2(4) . . . . ? N1 C8 C9 C10 85.6(4) . . . . ? N2 C9 C10 C11 -0.4(6) . . . . ? C8 C9 C10 C11 179.8(4) . . . . ? C9 C10 C11 C12 1.2(6) . . . . ? C10 C11 C12 C13 -1.1(7) . . . . ? C9 N2 C13 C12 0.6(6) . . . . ? C11 C12 C13 N2 0.3(7) . . . . ? C8 N1 C14 C15 63.7(4) . . . . ? S1 N1 C14 C15 -128.6(3) . . . . ? C19 N3 C15 C16 -1.9(5) . . . . ? C19 N3 C15 C14 -177.8(3) . . . . ? N1 C14 C15 N3 70.4(4) . . . . ? N1 C14 C15 C16 -105.4(4) . . . . ? N3 C15 C16 C17 -0.2(5) . . . . ? C14 C15 C16 C17 175.4(3) . . . . ? C15 C16 C17 C18 2.0(6) . . . . ? C16 C17 C18 C19 -1.7(6) . . . . ? C15 N3 C19 C18 2.2(5) . . . . ? C17 C18 C19 N3 -0.3(6) . . . . ? C24 N5 C20 C21 0.3(5) . . . . ? Cu1 N5 C20 C21 179.9(3) . . . . ? N5 C20 C21 C22 2.0(6) . . . . ? C20 C21 C22 C23 -2.1(6) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C20 N5 C24 C23 -2.6(5) . . . . ? Cu1 N5 C24 C23 177.9(2) . . . . ? C20 N5 C24 C25 174.0(3) . . . . ? Cu1 N5 C24 C25 -5.6(4) . . . . ? C22 C23 C24 N5 2.5(5) . . . . ? C22 C23 C24 C25 -174.0(3) . . . . ? N5 C24 C25 N4 37.5(4) . . . . ? C23 C24 C25 N4 -146.0(3) . . . . ? C26 N4 C25 C24 -148.0(3) . . . . ? S2 N4 C25 C24 80.8(3) . . . . ? Cu1 N4 C25 C24 -43.1(3) . . . . ? C25 N4 C26 C27 145.6(3) . . . . ? S2 N4 C26 C27 -82.6(3) . . . . ? Cu1 N4 C26 C27 41.2(3) . . . . ? C31 N6 C27 C28 0.7(5) . . . . ? Cu1 N6 C27 C28 176.8(3) . . . . ? C31 N6 C27 C26 -176.0(3) . . . . ? Cu1 N6 C27 C26 0.2(4) . . . . ? N4 C26 C27 N6 -32.5(4) . . . . ? N4 C26 C27 C28 150.8(3) . . . . ? N6 C27 C28 C29 -2.5(5) . . . . ? C26 C27 C28 C29 173.9(3) . . . . ? C27 C28 C29 C30 2.7(6) . . . . ? C28 C29 C30 C31 -1.1(6) . . . . ? C27 N6 C31 C30 1.1(5) . . . . ? Cu1 N6 C31 C30 -174.7(3) . . . . ? C29 C30 C31 N6 -0.8(5) . . . . ? 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 N3 H3B O1 0.88 1.66 2.529(4) 167.2 . #======================================================================= data_6 _database_code_depnum_ccdc_archive 'CCDC 737976' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C31 H29 Cl2 Cu2 N6 O5 S2 +), Cl4 Cu 2- ; _chemical_formula_sum 'C62 H58 Cl8 Cu5 N12 O10 S4' _chemical_formula_weight 1860.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.033(2) _cell_length_b 15.1201(11) _cell_length_c 17.8190(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7552.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7351 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 23.71 _exptl_crystal_description lath _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3756 _exptl_absorpt_coefficient_mu 1.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; This was the best result obtained from several crystals in the batch. Recrystallisation attempts failed. The problems might be related to multiple crystals: R(int) is high and all of the worst fitting reflections have F(obs) greater than F(calc). Modelling of the disorderd [CuCl~4~]^2-^ anion seems to be only a moderate problem. The large difference peaks lie in this area, but application of SQUEEZE with the anion removed improves wR2 to only about 25%. The SQUEEZED model was not therefore retained. There are solvent accessible voids of ca 80 \%A^3^, but nothing further can be resolved, and the failure to improve the situation using SQUEEZE again suggests that this is not the major problem. #--------------------------------------------------------------------- ** THE STRUCTURE SHOULD BE CONSIDERED AS PROOF OF CONNECTIVITY ONLY ** #--------------------------------------------------------------------- ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 58312 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.13 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 6692 _reflns_number_gt 4948 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0522P)^2^+315.0045P] 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 6692 _refine_ls_number_parameters 476 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1498 _refine_ls_R_factor_gt 0.1239 _refine_ls_wR_factor_ref 0.3048 _refine_ls_wR_factor_gt 0.2938 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.561 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.208 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 Cu1 Cu 0.21151(6) 0.26372(12) 0.38110(9) 0.0293(4) Uani 1 1 d . . . Cu2 Cu 0.21396(6) -0.01683(12) 0.42426(8) 0.0270(4) Uani 1 1 d . . . Cl1 Cl 0.25530(13) 0.2809(3) 0.48612(18) 0.0354(9) Uani 1 1 d . . . Cl2 Cl 0.26086(14) -0.0364(3) 0.3235(2) 0.0396(9) Uani 1 1 d . . . S1 S 0.14335(13) 0.1714(2) 0.25560(18) 0.0296(8) Uani 1 1 d . . . S2 S 0.14056(15) 0.0672(3) 0.5479(2) 0.0382(10) Uani 1 1 d . . . O11 O 0.1105(4) 0.1911(7) 0.1978(5) 0.040(3) Uani 1 1 d . . . O12 O 0.1807(4) 0.1119(7) 0.2418(5) 0.038(2) Uani 1 1 d . . . O21 O 0.1053(5) 0.0399(8) 0.6026(7) 0.060(4) Uani 1 1 d . . . O22 O 0.1751(5) 0.1308(7) 0.5696(5) 0.047(3) Uani 1 1 d . . . O1 O 0.1868(3) 0.1206(6) 0.4036(5) 0.025(2) Uani 1 1 d . . . N1 N 0.1734(4) 0.2697(8) 0.2788(6) 0.028(3) Uani 1 1 d . . . N2 N 0.1511(4) 0.3185(8) 0.4186(6) 0.032(3) Uani 1 1 d . . . N3 N 0.2654(4) 0.2334(8) 0.3146(6) 0.031(3) Uani 1 1 d . . . N4 N 0.1731(5) -0.0271(8) 0.5252(6) 0.035(3) Uani 1 1 d . . . N5 N 0.2658(4) 0.0135(7) 0.4937(6) 0.028(3) Uani 1 1 d . . . N6 N 0.1574(4) -0.0752(8) 0.3808(6) 0.028(3) Uani 1 1 d . . . C1 C 0.1393(5) 0.1180(9) 0.4027(7) 0.024(3) Uani 1 1 d . . . C2 C 0.1125(5) 0.1442(10) 0.3367(7) 0.028(3) Uani 1 1 d . . . C3 C 0.0630(5) 0.1466(12) 0.3370(9) 0.042(4) Uani 1 1 d . . . H3A H 0.0463 0.1685 0.2945 0.050 Uiso 1 1 calc R . . C4 C 0.0380(5) 0.1169(12) 0.3990(11) 0.047(4) Uani 1 1 d . . . C5 C 0.0618(6) 0.0930(12) 0.4615(10) 0.054(5) Uani 1 1 d . . . H5A H 0.0442 0.0761 0.5048 0.064 Uiso 1 1 calc R . . C6 C 0.1116(5) 0.0924(10) 0.4643(8) 0.032(3) Uani 1 1 d . . . C7 C -0.0169(6) 0.1136(18) 0.3948(13) 0.081(8) Uani 1 1 d . . . H7A H -0.0273 0.1313 0.3445 0.121 Uiso 1 1 d R . . H7B H -0.0304 0.1541 0.4320 0.121 Uiso 1 1 d R . . H7C H -0.0278 0.0533 0.4051 0.121 Uiso 1 1 d R . . C8 C 0.1379(6) 0.3436(11) 0.2879(8) 0.038(4) Uani 1 1 d . . . H8A H 0.1100 0.3329 0.2552 0.046 Uiso 1 1 calc R . . H8B H 0.1527 0.4004 0.2727 0.046 Uiso 1 1 calc R . . C9 C 0.1221(6) 0.3489(10) 0.3688(8) 0.035(3) Uani 1 1 d . . . C10 C 0.0784(7) 0.3838(14) 0.3871(8) 0.063(6) Uani 1 1 d . . . H10A H 0.0579 0.4050 0.3487 0.075 Uiso 1 1 calc R . . C11 C 0.0639(6) 0.3882(13) 0.4627(9) 0.053(5) Uani 1 1 d . . . H11A H 0.0342 0.4137 0.4770 0.063 Uiso 1 1 calc R . . C12 C 0.0951(6) 0.3536(12) 0.5147(9) 0.045(4) Uani 1 1 d . . . H12A H 0.0865 0.3527 0.5662 0.054 Uiso 1 1 calc R . . C13 C 0.1383(5) 0.3204(10) 0.4930(8) 0.033(3) Uani 1 1 d . . . H13A H 0.1598 0.2985 0.5298 0.040 Uiso 1 1 calc R . . C14 C 0.2093(5) 0.2854(10) 0.2186(7) 0.032(3) Uani 1 1 d . . . H14A H 0.2136 0.3499 0.2113 0.038 Uiso 1 1 calc R . . H14B H 0.1977 0.2599 0.1709 0.038 Uiso 1 1 calc R . . C15 C 0.2577(5) 0.2431(10) 0.2395(8) 0.034(4) Uani 1 1 d . . . C16 C 0.2887(6) 0.2182(13) 0.1864(9) 0.051(5) Uani 1 1 d . . . H16A H 0.2809 0.2227 0.1347 0.062 Uiso 1 1 calc R . . C17 C 0.3327(6) 0.1855(13) 0.2096(9) 0.047(4) Uani 1 1 d . . . H17A H 0.3559 0.1694 0.1733 0.057 Uiso 1 1 calc R . . C18 C 0.3429(5) 0.1762(11) 0.2849(8) 0.035(4) Uani 1 1 d . . . H18A H 0.3726 0.1535 0.3016 0.042 Uiso 1 1 calc R . . C19 C 0.3074(5) 0.2017(9) 0.3355(8) 0.031(3) Uani 1 1 d . . . H19A H 0.3137 0.1959 0.3876 0.037 Uiso 1 1 calc R . . C20 C 0.2093(6) -0.0430(10) 0.5863(7) 0.035(4) Uani 1 1 d . . . H20A H 0.1973 -0.0178 0.6340 0.042 Uiso 1 1 calc R . . H20B H 0.2135 -0.1074 0.5935 0.042 Uiso 1 1 calc R . . C21 C 0.2567(6) -0.0018(10) 0.5677(7) 0.035(4) Uani 1 1 d . . . C22 C 0.2917(6) 0.0080(12) 0.6203(10) 0.050(5) Uani 1 1 d . . . H22A H 0.2855 -0.0071 0.6711 0.060 Uiso 1 1 calc R . . C23 C 0.3368(7) 0.0402(13) 0.5997(11) 0.062(6) Uani 1 1 d . . . H23A H 0.3609 0.0508 0.6361 0.074 Uiso 1 1 calc R . . C24 C 0.3443(7) 0.0551(13) 0.5274(11) 0.056(5) Uani 1 1 d . . . H24A H 0.3747 0.0760 0.5121 0.068 Uiso 1 1 calc R . . C25 C 0.3101(5) 0.0414(10) 0.4739(10) 0.040(4) Uani 1 1 d . . . H25A H 0.3173 0.0516 0.4225 0.047 Uiso 1 1 calc R . . C26 C 0.1423(5) -0.1067(10) 0.5150(7) 0.031(3) Uani 1 1 d . . . H26A H 0.1141 -0.1027 0.5483 0.037 Uiso 1 1 calc R . . H26B H 0.1603 -0.1607 0.5285 0.037 Uiso 1 1 calc R . . C27 C 0.1256(5) -0.1121(10) 0.4299(8) 0.030(3) Uani 1 1 d . . . C28 C 0.0857(6) -0.1506(12) 0.4100(10) 0.048(4) Uani 1 1 d . . . H28A H 0.0648 -0.1741 0.4469 0.058 Uiso 1 1 calc R . . C29 C 0.0739(6) -0.1568(13) 0.3316(12) 0.058(5) Uani 1 1 d . . . H29A H 0.0462 -0.1873 0.3149 0.069 Uiso 1 1 calc R . . C30 C 0.1032(7) -0.1181(11) 0.2843(10) 0.051(5) Uani 1 1 d . . . H30A H 0.0953 -0.1166 0.2325 0.061 Uiso 1 1 calc R . . C31 C 0.1448(6) -0.0802(10) 0.3077(9) 0.038(4) Uani 1 1 d . . . H31A H 0.1657 -0.0562 0.2710 0.046 Uiso 1 1 calc R . . Cu3 Cu 0.0000 0.5860(2) 0.2500 0.0935(17) Uani 1 2 d SD . . Cl31 Cl 0.0397(3) 0.4768(6) 0.1841(5) 0.053(2) Uani 0.50 1 d PD . . Cl34 Cl 0.0326(3) 0.7038(6) 0.1882(4) 0.049(2) Uani 0.50 1 d PD . . Cl33 Cl 0.0287(4) 0.6200(7) 0.3731(4) 0.061(3) Uani 0.50 1 d PD . . Cl32 Cl -0.0686(3) 0.5301(8) 0.2773(7) 0.079(3) Uani 0.50 1 d PD . . 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 Cu1 0.0322(9) 0.0395(10) 0.0162(8) -0.0019(7) -0.0028(7) 0.0009(8) Cu2 0.0283(9) 0.0383(10) 0.0144(8) -0.0011(7) 0.0028(7) -0.0004(8) Cl1 0.0350(19) 0.054(2) 0.0178(16) -0.0028(16) -0.0035(14) -0.0032(17) Cl2 0.043(2) 0.050(2) 0.0262(18) 0.0015(17) 0.0130(16) 0.0045(18) S1 0.0377(19) 0.037(2) 0.0142(15) -0.0006(14) -0.0040(14) -0.0053(16) S2 0.049(2) 0.049(2) 0.0172(17) 0.0065(16) 0.0141(16) 0.016(2) O11 0.052(7) 0.050(7) 0.018(5) 0.006(5) -0.015(5) -0.014(5) O12 0.044(6) 0.041(6) 0.028(5) -0.011(5) 0.007(5) 0.000(5) O21 0.070(8) 0.066(8) 0.045(7) 0.031(6) 0.034(6) 0.033(7) O22 0.088(9) 0.040(6) 0.012(5) -0.001(4) 0.010(5) 0.010(6) O1 0.018(4) 0.038(5) 0.018(4) 0.001(4) -0.002(4) 0.001(4) N1 0.027(6) 0.039(7) 0.016(5) -0.004(5) 0.001(5) -0.005(5) N2 0.040(7) 0.032(7) 0.023(6) 0.003(5) -0.006(5) 0.001(6) N3 0.036(7) 0.043(7) 0.015(5) 0.002(5) 0.004(5) -0.002(6) N4 0.052(8) 0.028(7) 0.023(6) 0.005(5) 0.013(6) 0.001(6) N5 0.043(7) 0.026(6) 0.016(5) -0.004(5) -0.004(5) -0.003(5) N6 0.027(6) 0.032(6) 0.025(6) 0.003(5) -0.004(5) 0.002(5) C1 0.030(7) 0.023(7) 0.020(6) 0.001(5) 0.014(6) -0.001(6) C2 0.032(7) 0.036(8) 0.018(7) 0.000(6) 0.004(6) 0.004(6) C3 0.019(7) 0.064(11) 0.043(9) 0.015(8) 0.008(7) 0.002(7) C4 0.013(7) 0.060(11) 0.067(12) 0.011(9) -0.002(7) 0.002(7) C5 0.052(11) 0.062(12) 0.047(10) 0.022(9) 0.031(9) 0.021(9) C6 0.040(8) 0.035(8) 0.021(7) 0.009(6) 0.009(6) 0.007(7) C7 0.036(10) 0.13(2) 0.072(15) 0.040(15) -0.006(10) 0.009(12) C8 0.056(10) 0.042(9) 0.017(7) 0.006(6) -0.008(7) 0.000(8) C9 0.044(9) 0.037(8) 0.023(7) -0.011(7) -0.002(7) -0.001(7) C10 0.082(14) 0.092(15) 0.014(8) -0.006(9) -0.015(8) 0.045(12) C11 0.039(9) 0.084(14) 0.034(9) -0.003(9) 0.013(8) 0.033(9) C12 0.055(10) 0.055(11) 0.026(8) -0.007(8) 0.004(7) 0.007(9) C13 0.040(8) 0.041(9) 0.019(7) -0.007(6) 0.009(6) -0.009(7) C14 0.046(9) 0.037(8) 0.012(6) 0.005(6) 0.003(6) -0.003(7) C15 0.038(8) 0.039(8) 0.026(7) 0.002(7) -0.020(7) -0.013(7) C16 0.059(11) 0.072(13) 0.024(8) -0.010(8) 0.005(8) -0.018(10) C17 0.039(9) 0.072(13) 0.031(8) -0.003(8) 0.009(7) -0.013(9) C18 0.028(8) 0.051(10) 0.025(7) 0.008(7) 0.001(6) -0.007(7) C19 0.034(8) 0.030(8) 0.030(8) 0.010(6) -0.003(6) 0.000(6) C20 0.056(10) 0.038(8) 0.012(6) -0.001(6) 0.008(6) -0.012(7) C21 0.066(10) 0.026(8) 0.013(6) 0.002(6) -0.009(7) 0.011(7) C22 0.064(12) 0.053(11) 0.034(9) -0.011(8) -0.008(9) 0.025(10) C23 0.063(13) 0.074(14) 0.048(11) -0.034(10) -0.033(10) 0.013(11) C24 0.047(10) 0.062(12) 0.060(12) -0.028(10) -0.008(9) -0.019(9) C25 0.031(8) 0.034(9) 0.053(10) 0.001(8) -0.009(7) -0.008(7) C26 0.031(8) 0.045(9) 0.017(7) 0.006(6) 0.006(6) -0.004(7) C27 0.024(7) 0.039(8) 0.026(7) -0.003(6) -0.007(6) -0.005(6) C28 0.035(9) 0.056(11) 0.053(11) 0.007(9) 0.008(8) -0.007(8) C29 0.031(9) 0.065(13) 0.076(14) -0.017(11) -0.006(9) -0.004(9) C30 0.060(11) 0.044(10) 0.049(10) 0.000(8) -0.033(9) -0.009(9) C31 0.041(9) 0.037(9) 0.036(9) 0.008(7) -0.002(7) 0.006(7) Cu3 0.166(5) 0.048(2) 0.067(3) 0.000 0.075(3) 0.000 Cl31 0.048(5) 0.054(5) 0.058(5) -0.010(4) 0.009(4) 0.000(4) Cl34 0.040(4) 0.059(5) 0.047(5) 0.001(4) 0.004(4) -0.009(4) Cl33 0.079(7) 0.070(6) 0.034(4) -0.003(4) 0.003(4) -0.015(5) Cl32 0.045(5) 0.107(9) 0.083(8) -0.031(7) 0.014(5) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.975(11) . ? Cu1 N2 2.000(12) . ? Cu1 N1 2.114(11) . ? Cu1 Cl1 2.253(4) . ? Cu1 O1 2.307(10) . ? Cu2 N5 1.963(11) . ? Cu2 N6 1.973(11) . ? Cu2 N4 2.138(11) . ? Cu2 O1 2.244(10) . ? Cu2 Cl2 2.245(4) . ? S1 O12 1.402(11) . ? S1 O11 1.414(10) . ? S1 C2 1.733(13) . ? S1 N1 1.758(12) . ? S2 O22 1.418(13) . ? S2 O21 1.448(11) . ? S2 C6 1.739(14) . ? S2 N4 1.740(12) . ? O1 C1 1.332(15) . ? N1 C14 1.491(16) . ? N1 C8 1.505(19) . ? N2 C9 1.287(18) . ? N2 C13 1.374(17) . ? N3 C19 1.323(18) . ? N3 C15 1.363(17) . ? N4 C26 1.493(18) . ? N4 C20 1.507(19) . ? N5 C25 1.357(18) . ? N5 C21 1.364(17) . ? N6 C31 1.352(19) . ? N6 C27 1.369(18) . ? C1 C6 1.400(18) . ? C1 C2 1.450(19) . ? C2 C3 1.389(19) . ? C3 C4 1.38(2) . ? C3 H3A 0.95 . ? C4 C5 1.35(2) . ? C4 C7 1.54(2) . ? C5 C6 1.40(2) . ? C5 H5A 0.95 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.511(19) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.37(2) . ? C10 C11 1.41(2) . ? C10 H10A 0.95 . ? C11 C12 1.38(2) . ? C11 H11A 0.95 . ? C12 C13 1.37(2) . ? C12 H12A 0.95 . ? C13 H13A 0.95 . ? C14 C15 1.55(2) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.34(2) . ? C16 C17 1.39(2) . ? C16 H16A 0.95 . ? C17 C18 1.38(2) . ? C17 H17A 0.95 . ? C18 C19 1.40(2) . ? C18 H18A 0.95 . ? C19 H19A 0.95 . ? C20 C21 1.50(2) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.36(2) . ? C22 C23 1.40(3) . ? C22 H22A 0.95 . ? C23 C24 1.32(3) . ? C23 H23A 0.95 . ? C24 C25 1.37(2) . ? C24 H24A 0.95 . ? C25 H25A 0.95 . ? C26 C27 1.590(18) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.31(2) . ? C28 C29 1.44(3) . ? C28 H28A 0.95 . ? C29 C30 1.32(3) . ? C29 H29A 0.95 . ? C30 C31 1.36(2) . ? C30 H30A 0.95 . ? C31 H31A 0.95 . ? Cu3 Cl32 2.157(8) 3 ? Cu3 Cl32 2.157(8) . ? Cu3 Cl34 2.286(7) 3 ? Cu3 Cl34 2.286(7) . ? Cu3 Cl31 2.312(7) 3 ? Cu3 Cl31 2.312(7) . ? Cu3 Cl33 2.392(7) 3 ? Cu3 Cl33 2.392(7) . ? Cl31 Cl32 1.334(15) 3 ? Cl34 Cl33 2.398(13) 3 ? Cl33 Cl34 2.398(13) 3 ? Cl32 Cl31 1.334(15) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 160.9(5) . . ? N3 Cu1 N1 83.1(4) . . ? N2 Cu1 N1 80.9(4) . . ? N3 Cu1 Cl1 96.2(3) . . ? N2 Cu1 Cl1 97.8(3) . . ? N1 Cu1 Cl1 170.5(4) . . ? N3 Cu1 O1 96.7(4) . . ? N2 Cu1 O1 94.4(4) . . ? N1 Cu1 O1 92.2(4) . . ? Cl1 Cu1 O1 97.3(2) . . ? N5 Cu2 N6 161.3(5) . . ? N5 Cu2 N4 83.3(5) . . ? N6 Cu2 N4 82.4(5) . . ? N5 Cu2 O1 98.0(4) . . ? N6 Cu2 O1 94.4(4) . . ? N4 Cu2 O1 91.3(4) . . ? N5 Cu2 Cl2 95.8(4) . . ? N6 Cu2 Cl2 95.6(4) . . ? N4 Cu2 Cl2 167.7(3) . . ? O1 Cu2 Cl2 100.9(2) . . ? O12 S1 O11 119.6(7) . . ? O12 S1 C2 111.5(7) . . ? O11 S1 C2 109.4(7) . . ? O12 S1 N1 103.1(6) . . ? O11 S1 N1 107.8(6) . . ? C2 S1 N1 104.1(6) . . ? O22 S2 O21 118.4(8) . . ? O22 S2 C6 113.8(7) . . ? O21 S2 C6 108.7(7) . . ? O22 S2 N4 105.1(7) . . ? O21 S2 N4 106.3(7) . . ? C6 S2 N4 103.1(6) . . ? C1 O1 Cu2 108.3(8) . . ? C1 O1 Cu1 109.0(8) . . ? Cu2 O1 Cu1 142.7(4) . . ? C14 N1 C8 113.8(11) . . ? C14 N1 S1 106.8(9) . . ? C8 N1 S1 109.7(9) . . ? C14 N1 Cu1 106.6(8) . . ? C8 N1 Cu1 105.9(8) . . ? S1 N1 Cu1 114.2(6) . . ? C9 N2 C13 119.6(13) . . ? C9 N2 Cu1 116.9(10) . . ? C13 N2 Cu1 123.5(10) . . ? C19 N3 C15 117.2(13) . . ? C19 N3 Cu1 126.6(9) . . ? C15 N3 Cu1 116.2(10) . . ? C26 N4 C20 110.4(11) . . ? C26 N4 S2 112.7(10) . . ? C20 N4 S2 108.4(9) . . ? C26 N4 Cu2 105.4(8) . . ? C20 N4 Cu2 105.0(8) . . ? S2 N4 Cu2 114.6(6) . . ? C25 N5 C21 118.4(13) . . ? C25 N5 Cu2 125.9(10) . . ? C21 N5 Cu2 115.5(10) . . ? C31 N6 C27 115.0(12) . . ? C31 N6 Cu2 127.9(10) . . ? C27 N6 Cu2 117.1(9) . . ? O1 C1 C6 123.6(13) . . ? O1 C1 C2 121.3(11) . . ? C6 C1 C2 115.0(12) . . ? C3 C2 C1 121.5(13) . . ? C3 C2 S1 119.7(11) . . ? C1 C2 S1 118.9(10) . . ? C4 C3 C2 120.1(14) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 119.7(14) . . ? C5 C4 C7 121.8(16) . . ? C3 C4 C7 118.5(16) . . ? C4 C5 C6 121.7(14) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 121.8(14) . . ? C5 C6 S2 119.9(11) . . ? C1 C6 S2 118.2(11) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 109.5(11) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C10 122.4(14) . . ? N2 C9 C8 117.0(14) . . ? C10 C9 C8 120.6(14) . . ? C9 C10 C11 120.3(15) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 116.1(15) . . ? C12 C11 H11A 121.9 . . ? C10 C11 H11A 121.9 . . ? C13 C12 C11 120.9(15) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 N2 120.7(15) . . ? C12 C13 H13A 119.6 . . ? N2 C13 H13A 119.6 . . ? N1 C14 C15 110.7(11) . . ? N1 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 N3 124.0(15) . . ? C16 C15 C14 121.1(13) . . ? N3 C15 C14 114.9(13) . . ? C15 C16 C17 117.7(15) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C18 C17 C16 120.6(15) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 116.9(15) . . ? C17 C18 H18A 121.6 . . ? C19 C18 H18A 121.6 . . ? N3 C19 C18 123.5(13) . . ? N3 C19 H19A 118.3 . . ? C18 C19 H19A 118.3 . . ? C21 C20 N4 111.7(11) . . ? C21 C20 H20A 109.3 . . ? N4 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? N4 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? N5 C21 C22 120.7(16) . . ? N5 C21 C20 116.6(12) . . ? C22 C21 C20 121.9(14) . . ? C21 C22 C23 120.4(16) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C24 C23 C22 117.2(16) . . ? C24 C23 H23A 121.4 . . ? C22 C23 H23A 121.4 . . ? C23 C24 C25 122.6(18) . . ? C23 C24 H24A 118.7 . . ? C25 C24 H24A 118.7 . . ? N5 C25 C24 120.5(16) . . ? N5 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? N4 C26 C27 109.2(11) . . ? N4 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? N4 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C28 C27 N6 124.4(14) . . ? C28 C27 C26 122.2(14) . . ? N6 C27 C26 113.3(11) . . ? C27 C28 C29 119.3(16) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C30 C29 C28 116.7(16) . . ? C30 C29 H29A 121.7 . . ? C28 C29 H29A 121.7 . . ? C29 C30 C31 121.7(17) . . ? C29 C30 H30A 119.1 . . ? C31 C30 H30A 119.1 . . ? N6 C31 C30 122.8(16) . . ? N6 C31 H31A 118.6 . . ? C30 C31 H31A 118.6 . . ? Cl32 Cu3 Cl32 133.9(7) 3 . ? Cl32 Cu3 Cl34 140.4(4) 3 3 ? Cl32 Cu3 Cl34 80.8(4) . 3 ? Cl32 Cu3 Cl34 80.8(4) 3 . ? Cl32 Cu3 Cl34 140.4(4) . . ? Cl34 Cu3 Cl34 77.6(5) 3 . ? Cl32 Cu3 Cl31 105.3(4) 3 3 ? Cl32 Cu3 Cl31 34.5(4) . 3 ? Cl34 Cu3 Cl31 96.9(3) 3 3 ? Cl34 Cu3 Cl31 173.8(3) . 3 ? Cl32 Cu3 Cl31 34.5(4) 3 . ? Cl32 Cu3 Cl31 105.3(4) . . ? Cl34 Cu3 Cl31 173.8(3) 3 . ? Cl34 Cu3 Cl31 96.9(3) . . ? Cl31 Cu3 Cl31 88.8(5) 3 . ? Cl32 Cu3 Cl33 100.2(4) 3 3 ? Cl32 Cu3 Cl33 89.5(4) . 3 ? Cl34 Cu3 Cl33 98.0(3) 3 3 ? Cl34 Cu3 Cl33 61.6(3) . 3 ? Cl31 Cu3 Cl33 117.2(4) 3 3 ? Cl31 Cu3 Cl33 81.4(3) . 3 ? Cl32 Cu3 Cl33 89.5(4) 3 . ? Cl32 Cu3 Cl33 100.2(4) . . ? Cl34 Cu3 Cl33 61.6(3) 3 . ? Cl34 Cu3 Cl33 98.0(3) . . ? Cl31 Cu3 Cl33 81.4(3) 3 . ? Cl31 Cu3 Cl33 117.2(4) . . ? Cl33 Cu3 Cl33 155.2(5) 3 . ? Cl32 Cl31 Cu3 66.4(4) 3 . ? Cu3 Cl34 Cl33 61.4(3) . 3 ? Cu3 Cl33 Cl34 57.0(3) . 3 ? Cl31 Cl32 Cu3 79.1(5) 3 . ? 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 N5 Cu2 O1 C1 -139.2(8) . . . . ? N6 Cu2 O1 C1 26.7(8) . . . . ? N4 Cu2 O1 C1 -55.8(8) . . . . ? Cl2 Cu2 O1 C1 123.3(8) . . . . ? N5 Cu2 O1 Cu1 42.6(7) . . . . ? N6 Cu2 O1 Cu1 -151.5(7) . . . . ? N4 Cu2 O1 Cu1 126.1(7) . . . . ? Cl2 Cu2 O1 Cu1 -54.9(7) . . . . ? N3 Cu1 O1 C1 -139.3(8) . . . . ? N2 Cu1 O1 C1 25.0(8) . . . . ? N1 Cu1 O1 C1 -56.0(8) . . . . ? Cl1 Cu1 O1 C1 123.5(8) . . . . ? N3 Cu1 O1 Cu2 38.8(7) . . . . ? N2 Cu1 O1 Cu2 -156.9(7) . . . . ? N1 Cu1 O1 Cu2 122.1(7) . . . . ? Cl1 Cu1 O1 Cu2 -58.4(7) . . . . ? O12 S1 N1 C14 50.5(10) . . . . ? O11 S1 N1 C14 -76.9(10) . . . . ? C2 S1 N1 C14 166.9(9) . . . . ? O12 S1 N1 C8 174.3(8) . . . . ? O11 S1 N1 C8 46.9(10) . . . . ? C2 S1 N1 C8 -69.2(10) . . . . ? O12 S1 N1 Cu1 -67.1(7) . . . . ? O11 S1 N1 Cu1 165.5(6) . . . . ? C2 S1 N1 Cu1 49.4(8) . . . . ? N3 Cu1 N1 C14 -22.7(9) . . . . ? N2 Cu1 N1 C14 146.7(9) . . . . ? O1 Cu1 N1 C14 -119.2(9) . . . . ? N3 Cu1 N1 C8 -144.3(9) . . . . ? N2 Cu1 N1 C8 25.2(9) . . . . ? O1 Cu1 N1 C8 119.2(9) . . . . ? N3 Cu1 N1 S1 95.0(7) . . . . ? N2 Cu1 N1 S1 -95.6(7) . . . . ? O1 Cu1 N1 S1 -1.5(6) . . . . ? N3 Cu1 N2 C9 20(2) . . . . ? N1 Cu1 N2 C9 -13.5(11) . . . . ? Cl1 Cu1 N2 C9 157.0(11) . . . . ? O1 Cu1 N2 C9 -105.0(11) . . . . ? N3 Cu1 N2 C13 -163.6(13) . . . . ? N1 Cu1 N2 C13 162.7(12) . . . . ? Cl1 Cu1 N2 C13 -26.9(12) . . . . ? O1 Cu1 N2 C13 71.1(11) . . . . ? N2 Cu1 N3 C19 159.0(14) . . . . ? N1 Cu1 N3 C19 -167.5(13) . . . . ? Cl1 Cu1 N3 C19 22.0(13) . . . . ? O1 Cu1 N3 C19 -76.1(12) . . . . ? N2 Cu1 N3 C15 -24(2) . . . . ? N1 Cu1 N3 C15 9.7(11) . . . . ? Cl1 Cu1 N3 C15 -160.7(10) . . . . ? O1 Cu1 N3 C15 101.1(11) . . . . ? O22 S2 N4 C26 169.0(9) . . . . ? O21 S2 N4 C26 42.7(11) . . . . ? C6 S2 N4 C26 -71.5(10) . . . . ? O22 S2 N4 C20 46.5(10) . . . . ? O21 S2 N4 C20 -79.8(11) . . . . ? C6 S2 N4 C20 166.0(9) . . . . ? O22 S2 N4 Cu2 -70.4(8) . . . . ? O21 S2 N4 Cu2 163.3(8) . . . . ? C6 S2 N4 Cu2 49.1(9) . . . . ? N5 Cu2 N4 C26 -139.2(9) . . . . ? N6 Cu2 N4 C26 28.7(9) . . . . ? O1 Cu2 N4 C26 123.0(9) . . . . ? Cl2 Cu2 N4 C26 -53(2) . . . . ? N5 Cu2 N4 C20 -22.5(9) . . . . ? N6 Cu2 N4 C20 145.3(9) . . . . ? O1 Cu2 N4 C20 -120.4(9) . . . . ? Cl2 Cu2 N4 C20 64(2) . . . . ? N5 Cu2 N4 S2 96.3(7) . . . . ? N6 Cu2 N4 S2 -95.8(7) . . . . ? O1 Cu2 N4 S2 -1.5(7) . . . . ? Cl2 Cu2 N4 S2 -177.2(12) . . . . ? N6 Cu2 N5 C25 146.4(14) . . . . ? N4 Cu2 N5 C25 -173.1(12) . . . . ? O1 Cu2 N5 C25 -82.7(12) . . . . ? Cl2 Cu2 N5 C25 19.2(12) . . . . ? N6 Cu2 N5 C21 -29(2) . . . . ? N4 Cu2 N5 C21 12.0(10) . . . . ? O1 Cu2 N5 C21 102.4(10) . . . . ? Cl2 Cu2 N5 C21 -155.7(9) . . . . ? N5 Cu2 N6 C31 -156.6(14) . . . . ? N4 Cu2 N6 C31 162.8(13) . . . . ? O1 Cu2 N6 C31 72.1(12) . . . . ? Cl2 Cu2 N6 C31 -29.4(12) . . . . ? N5 Cu2 N6 C27 27(2) . . . . ? N4 Cu2 N6 C27 -14.0(10) . . . . ? O1 Cu2 N6 C27 -104.8(10) . . . . ? Cl2 Cu2 N6 C27 153.7(10) . . . . ? Cu2 O1 C1 C6 62.2(15) . . . . ? Cu1 O1 C1 C6 -119.0(13) . . . . ? Cu2 O1 C1 C2 -119.5(12) . . . . ? Cu1 O1 C1 C2 59.3(14) . . . . ? O1 C1 C2 C3 -176.1(14) . . . . ? C6 C1 C2 C3 2(2) . . . . ? O1 C1 C2 S1 5.0(18) . . . . ? C6 C1 C2 S1 -176.6(11) . . . . ? O12 S1 C2 C3 -136.0(13) . . . . ? O11 S1 C2 C3 -1.5(16) . . . . ? N1 S1 C2 C3 113.5(14) . . . . ? O12 S1 C2 C1 42.9(13) . . . . ? O11 S1 C2 C1 177.5(11) . . . . ? N1 S1 C2 C1 -67.5(12) . . . . ? C1 C2 C3 C4 -5(3) . . . . ? S1 C2 C3 C4 173.8(14) . . . . ? C2 C3 C4 C5 6(3) . . . . ? C2 C3 C4 C7 -175.2(18) . . . . ? C3 C4 C5 C6 -4(3) . . . . ? C7 C4 C5 C6 177.2(19) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C4 C5 C6 S2 176.3(15) . . . . ? O1 C1 C6 C5 178.1(15) . . . . ? C2 C1 C6 C5 0(2) . . . . ? O1 C1 C6 S2 3(2) . . . . ? C2 C1 C6 S2 -175.6(10) . . . . ? O22 S2 C6 C5 -127.8(14) . . . . ? O21 S2 C6 C5 6.5(16) . . . . ? N4 S2 C6 C5 118.9(14) . . . . ? O22 S2 C6 C1 47.7(14) . . . . ? O21 S2 C6 C1 -178.1(12) . . . . ? N4 S2 C6 C1 -65.6(13) . . . . ? C14 N1 C8 C9 -149.4(12) . . . . ? S1 N1 C8 C9 91.0(12) . . . . ? Cu1 N1 C8 C9 -32.6(14) . . . . ? C13 N2 C9 C10 0(2) . . . . ? Cu1 N2 C9 C10 176.5(14) . . . . ? C13 N2 C9 C8 -179.1(13) . . . . ? Cu1 N2 C9 C8 -2.8(18) . . . . ? N1 C8 C9 N2 25.2(19) . . . . ? N1 C8 C9 C10 -154.1(16) . . . . ? N2 C9 C10 C11 1(3) . . . . ? C8 C9 C10 C11 179.8(18) . . . . ? C9 C10 C11 C12 -2(3) . . . . ? C10 C11 C12 C13 3(3) . . . . ? C11 C12 C13 N2 -2(3) . . . . ? C9 N2 C13 C12 0(2) . . . . ? Cu1 N2 C13 C12 -175.6(12) . . . . ? C8 N1 C14 C15 147.2(12) . . . . ? S1 N1 C14 C15 -91.6(11) . . . . ? Cu1 N1 C14 C15 30.8(13) . . . . ? C19 N3 C15 C16 4(2) . . . . ? Cu1 N3 C15 C16 -173.8(13) . . . . ? C19 N3 C15 C14 -176.6(12) . . . . ? Cu1 N3 C15 C14 5.9(16) . . . . ? N1 C14 C15 C16 154.0(14) . . . . ? N1 C14 C15 N3 -25.7(17) . . . . ? N3 C15 C16 C17 -4(3) . . . . ? C14 C15 C16 C17 176.2(15) . . . . ? C15 C16 C17 C18 2(3) . . . . ? C16 C17 C18 C19 -1(3) . . . . ? C15 N3 C19 C18 -2(2) . . . . ? Cu1 N3 C19 C18 175.7(11) . . . . ? C17 C18 C19 N3 0(2) . . . . ? C26 N4 C20 C21 142.3(12) . . . . ? S2 N4 C20 C21 -93.8(12) . . . . ? Cu2 N4 C20 C21 29.2(13) . . . . ? C25 N5 C21 C22 -2(2) . . . . ? Cu2 N5 C21 C22 173.1(12) . . . . ? C25 N5 C21 C20 -172.9(13) . . . . ? Cu2 N5 C21 C20 2.5(16) . . . . ? N4 C20 C21 N5 -22.9(18) . . . . ? N4 C20 C21 C22 166.6(14) . . . . ? N5 C21 C22 C23 5(2) . . . . ? C20 C21 C22 C23 174.9(16) . . . . ? C21 C22 C23 C24 -4(3) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C21 N5 C25 C24 -1(2) . . . . ? Cu2 N5 C25 C24 -175.7(13) . . . . ? C23 C24 C25 N5 2(3) . . . . ? C20 N4 C26 C27 -149.8(11) . . . . ? S2 N4 C26 C27 88.8(12) . . . . ? Cu2 N4 C26 C27 -36.9(13) . . . . ? C31 N6 C27 C28 0(2) . . . . ? Cu2 N6 C27 C28 177.7(13) . . . . ? C31 N6 C27 C26 178.8(12) . . . . ? Cu2 N6 C27 C26 -4.0(16) . . . . ? N4 C26 C27 C28 -152.7(15) . . . . ? N4 C26 C27 N6 28.9(17) . . . . ? N6 C27 C28 C29 1(3) . . . . ? C26 C27 C28 C29 -177.1(16) . . . . ? C27 C28 C29 C30 -4(3) . . . . ? C28 C29 C30 C31 5(3) . . . . ? C27 N6 C31 C30 1(2) . . . . ? Cu2 N6 C31 C30 -176.2(12) . . . . ? C29 C30 C31 N6 -4(3) . . . . ? Cl32 Cu3 Cl31 Cl32 -150.4(6) . . . 3 ? Cl34 Cu3 Cl31 Cl32 62.6(7) . . . 3 ? Cl31 Cu3 Cl31 Cl32 -119.8(7) 3 . . 3 ? Cl33 Cu3 Cl31 Cl32 122.5(7) 3 . . 3 ? Cl33 Cu3 Cl31 Cl32 -40.1(7) . . . 3 ? Cl32 Cu3 Cl34 Cl33 106.9(5) 3 . . 3 ? Cl32 Cu3 Cl34 Cl33 -48.0(6) . . . 3 ? Cl34 Cu3 Cl34 Cl33 -106.4(4) 3 . . 3 ? Cl31 Cu3 Cl34 Cl33 76.3(4) . . . 3 ? Cl33 Cu3 Cl34 Cl33 -164.9(3) . . . 3 ? Cl32 Cu3 Cl33 Cl34 151.7(4) 3 . . 3 ? Cl32 Cu3 Cl33 Cl34 -73.6(4) . . . 3 ? Cl34 Cu3 Cl33 Cl34 71.1(5) . . . 3 ? Cl31 Cu3 Cl33 Cl34 -102.7(4) 3 . . 3 ? Cl31 Cu3 Cl33 Cl34 173.2(4) . . . 3 ? Cl33 Cu3 Cl33 Cl34 38.0(3) 3 . . 3 ? Cl32 Cu3 Cl32 Cl31 41.3(6) 3 . . 3 ? Cl34 Cu3 Cl32 Cl31 -116.7(7) 3 . . 3 ? Cl34 Cu3 Cl32 Cl31 -174.1(6) . . . 3 ? Cl31 Cu3 Cl32 Cl31 64.2(8) . . . 3 ? Cl33 Cu3 Cl32 Cl31 145.1(7) 3 . . 3 ? Cl33 Cu3 Cl32 Cl31 -57.9(7) . . . 3 ? #======================================================================= data_7 _database_code_depnum_ccdc_archive 'CCDC 737977' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C35 H35 Mn2 N6 O9 S2 +, Cl O4 -, C2 H3 N ; _chemical_formula_sum 'C37 H38 Cl Mn2 N7 O13 S2' _chemical_formula_weight 998.19 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3700(4) _cell_length_b 13.7747(6) _cell_length_c 28.8164(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.712(2) _cell_angle_gamma 90.00 _cell_volume 4111.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7403 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 24.83 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Geometry of acetonitrile molecules is restrained: C---N= 1.15(1) \%A, C---C = 1.45(1) \%A and C...N = 2.60(2) \%A. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 29239 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 7244 _reflns_number_gt 5470 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0777P)^2^+1.1075P] 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 7244 _refine_ls_number_parameters 559 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.733 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.085 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 Mn1 Mn 0.21458(4) 0.40253(4) 0.399897(16) 0.02212(14) Uani 1 1 d . . . Mn2 Mn 0.53117(4) 0.32766(3) 0.414612(16) 0.02263(14) Uani 1 1 d . . . S1 S 0.32321(7) 0.52870(6) 0.30311(3) 0.02385(19) Uani 1 1 d . . . S2 S 0.43850(7) 0.14570(6) 0.33789(3) 0.0242(2) Uani 1 1 d . . . O11 O 0.2948(2) 0.58746(16) 0.26284(8) 0.0323(5) Uani 1 1 d . . . O12 O 0.41682(19) 0.56411(16) 0.33707(8) 0.0285(5) Uani 1 1 d . . . O21 O 0.4677(2) 0.06258(16) 0.31048(8) 0.0313(5) Uani 1 1 d . . . O22 O 0.3381(2) 0.13698(16) 0.36990(7) 0.0289(5) Uani 1 1 d . . . O1 O 0.37786(18) 0.35351(15) 0.36323(7) 0.0219(5) Uani 1 1 d . . . O2 O 0.3285(2) 0.50789(16) 0.43665(7) 0.0278(5) Uani 1 1 d . . . O3 O 0.5377(2) 0.46757(16) 0.44062(8) 0.0286(5) Uani 1 1 d . . . O4 O 0.1906(2) 0.29384(17) 0.44751(8) 0.0342(6) Uani 1 1 d . . . O5 O 0.3994(2) 0.25746(17) 0.45657(7) 0.0327(5) Uani 1 1 d . . . N1 N 0.1853(2) 0.51121(18) 0.33157(8) 0.0223(6) Uani 1 1 d . . . N2 N 0.0901(2) 0.31974(19) 0.34437(9) 0.0244(6) Uani 1 1 d . . . N3 N 0.0467(2) 0.5010(2) 0.41130(9) 0.0262(6) Uani 1 1 d . . . N4 N 0.5720(2) 0.18118(19) 0.36980(9) 0.0231(6) Uani 1 1 d . . . N5 N 0.6875(2) 0.2455(2) 0.45308(9) 0.0253(6) Uani 1 1 d . . . N6 N 0.6679(2) 0.37030(19) 0.35642(9) 0.0242(6) Uani 1 1 d . . . C1 C 0.3831(3) 0.3373(2) 0.31841(10) 0.0209(7) Uani 1 1 d . . . C2 C 0.3576(3) 0.4104(2) 0.28473(10) 0.0219(7) Uani 1 1 d . . . C3 C 0.3602(3) 0.3925(2) 0.23731(11) 0.0264(7) Uani 1 1 d . . . H3A H 0.3412 0.4437 0.2160 0.032 Uiso 1 1 calc R . . C4 C 0.3899(3) 0.3015(2) 0.22065(11) 0.0275(8) Uani 1 1 d . . . C5 C 0.4167(3) 0.2286(2) 0.25284(10) 0.0255(7) Uani 1 1 d . . . H5A H 0.4386 0.1658 0.2421 0.031 Uiso 1 1 calc R . . C6 C 0.4126(3) 0.2448(2) 0.30023(10) 0.0220(7) Uani 1 1 d . . . C7 C 0.3895(4) 0.2815(3) 0.16925(11) 0.0420(9) Uani 1 1 d . . . H7A H 0.4089 0.3414 0.1527 0.063 Uiso 1 1 calc R . . H7B H 0.3042 0.2575 0.1585 0.063 Uiso 1 1 calc R . . H7C H 0.4550 0.2324 0.1631 0.063 Uiso 1 1 calc R . . C8 C 0.0808(3) 0.4695(2) 0.30002(11) 0.0257(7) Uani 1 1 d . . . H8A H -0.0035 0.4956 0.3089 0.031 Uiso 1 1 calc R . . H8B H 0.0946 0.4904 0.2678 0.031 Uiso 1 1 calc R . . C9 C 0.0765(3) 0.3612(2) 0.30164(11) 0.0250(7) Uani 1 1 d . . . C10 C 0.0531(3) 0.3068(3) 0.26206(12) 0.0340(8) Uani 1 1 d . . . H10A H 0.0463 0.3372 0.2324 0.041 Uiso 1 1 calc R . . C11 C 0.0395(4) 0.2074(3) 0.26603(13) 0.0432(9) Uani 1 1 d . . . H11A H 0.0239 0.1687 0.2391 0.052 Uiso 1 1 calc R . . C12 C 0.0488(4) 0.1647(3) 0.30915(13) 0.0393(9) Uani 1 1 d . . . H12A H 0.0375 0.0967 0.3126 0.047 Uiso 1 1 calc R . . C13 C 0.0750(3) 0.2235(3) 0.34734(12) 0.0310(8) Uani 1 1 d . . . H13A H 0.0826 0.1941 0.3772 0.037 Uiso 1 1 calc R . . C14 C 0.1465(3) 0.6032(2) 0.35436(11) 0.0254(7) Uani 1 1 d . . . H14A H 0.1159 0.6504 0.3304 0.030 Uiso 1 1 calc R . . H14B H 0.2221 0.6317 0.3717 0.030 Uiso 1 1 calc R . . C15 C 0.0405(3) 0.5839(2) 0.38733(11) 0.0241(7) Uani 1 1 d . . . C16 C -0.0560(3) 0.6523(3) 0.39325(12) 0.0326(8) Uani 1 1 d . . . H16A H -0.0595 0.7102 0.3753 0.039 Uiso 1 1 calc R . . C17 C -0.1465(3) 0.6344(3) 0.42568(12) 0.0336(8) Uani 1 1 d . . . H17A H -0.2118 0.6809 0.4311 0.040 Uiso 1 1 calc R . . C18 C -0.1418(3) 0.5482(3) 0.45034(12) 0.0343(8) Uani 1 1 d . . . H18A H -0.2039 0.5339 0.4725 0.041 Uiso 1 1 calc R . . C19 C -0.0438(3) 0.4834(3) 0.44171(11) 0.0318(8) Uani 1 1 d . . . H19A H -0.0407 0.4236 0.4582 0.038 Uiso 1 1 calc R . . C20 C 0.6023(3) 0.1090(2) 0.40772(11) 0.0277(7) Uani 1 1 d . . . H20A H 0.6380 0.0492 0.3943 0.033 Uiso 1 1 calc R . . H20B H 0.5221 0.0916 0.4231 0.033 Uiso 1 1 calc R . . C21 C 0.6989(3) 0.1512(2) 0.44299(11) 0.0255(7) Uani 1 1 d . . . C22 C 0.7916(3) 0.0924(3) 0.46484(12) 0.0349(8) Uani 1 1 d . . . H22A H 0.7978 0.0257 0.4569 0.042 Uiso 1 1 calc R . . C23 C 0.8745(3) 0.1324(3) 0.49833(13) 0.0438(10) Uani 1 1 d . . . H23A H 0.9393 0.0938 0.5137 0.053 Uiso 1 1 calc R . . C24 C 0.8624(3) 0.2295(3) 0.50935(13) 0.0412(9) Uani 1 1 d . . . H24A H 0.9177 0.2584 0.5327 0.049 Uiso 1 1 calc R . . C25 C 0.7691(3) 0.2834(3) 0.48604(11) 0.0317(8) Uani 1 1 d . . . H25A H 0.7616 0.3503 0.4934 0.038 Uiso 1 1 calc R . . C26 C 0.6841(3) 0.1982(2) 0.34019(11) 0.0271(7) Uani 1 1 d . . . H26A H 0.6759 0.1557 0.3125 0.033 Uiso 1 1 calc R . . H26B H 0.7647 0.1803 0.3579 0.033 Uiso 1 1 calc R . . C27 C 0.6930(3) 0.3021(2) 0.32468(11) 0.0241(7) Uani 1 1 d . . . C28 C 0.7295(3) 0.3252(3) 0.28049(12) 0.0303(8) Uani 1 1 d . . . H28A H 0.7447 0.2754 0.2586 0.036 Uiso 1 1 calc R . . C29 C 0.7435(3) 0.4215(3) 0.26857(12) 0.0366(9) Uani 1 1 d . . . H29A H 0.7679 0.4392 0.2383 0.044 Uiso 1 1 calc R . . C30 C 0.7214(3) 0.4916(3) 0.30138(12) 0.0333(8) Uani 1 1 d . . . H30A H 0.7326 0.5584 0.2944 0.040 Uiso 1 1 calc R . . C31 C 0.6827(3) 0.4632(2) 0.34448(12) 0.0283(8) Uani 1 1 d . . . H31A H 0.6658 0.5119 0.3667 0.034 Uiso 1 1 calc R . . C32 C 0.4467(3) 0.5289(2) 0.44057(10) 0.0240(7) Uani 1 1 d . . . C33 C 0.4845(3) 0.6338(2) 0.44491(12) 0.0329(8) Uani 1 1 d . . . H33A H 0.5360 0.6436 0.4739 0.049 Uiso 1 1 calc R . . H33B H 0.4067 0.6741 0.4451 0.049 Uiso 1 1 calc R . . H33C H 0.5357 0.6522 0.4186 0.049 Uiso 1 1 calc R . . C34 C 0.2817(3) 0.2383(3) 0.46124(11) 0.0284(8) Uani 1 1 d . . . C35 C 0.2475(4) 0.1450(3) 0.48373(14) 0.0464(10) Uani 1 1 d . . . H35A H 0.3254 0.1158 0.4984 0.070 Uiso 1 1 calc R . . H35B H 0.2099 0.1006 0.4602 0.070 Uiso 1 1 calc R . . H35C H 0.1846 0.1573 0.5074 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.06488(9) 0.43518(7) 0.12564(3) 0.0397(2) Uani 1 1 d . . . O1A O 0.1265(3) 0.3787(2) 0.09200(10) 0.0589(8) Uani 1 1 d . . . O1B O -0.0222(3) 0.5017(2) 0.10295(10) 0.0599(8) Uani 1 1 d . . . O1C O -0.0058(3) 0.3717(3) 0.15420(10) 0.0737(10) Uani 1 1 d . . . O1D O 0.1574(3) 0.4866(3) 0.15359(15) 0.0976(14) Uani 1 1 d . . . N1S N 0.4634(8) 0.9150(6) 0.4566(3) 0.095(2) Uiso 0.60 1 d PD A 1 C1S C 0.3997(8) 0.8999(6) 0.4244(3) 0.061(2) Uiso 0.60 1 d PD A 1 C2S C 0.3070(9) 0.8892(8) 0.3852(4) 0.080(3) Uiso 0.60 1 d PD A 1 H21S H 0.2268 0.9226 0.3922 0.120 Uiso 0.60 1 d PR A 1 H22S H 0.2892 0.8202 0.3798 0.120 Uiso 0.60 1 d PR A 1 H23S H 0.3421 0.9178 0.3573 0.120 Uiso 0.60 1 d PR A 1 N2S N 0.2838(12) 0.8068(9) 0.3338(4) 0.099(4) Uiso 0.40 1 d PD B 2 C3S C 0.3078(11) 0.8525(9) 0.3662(4) 0.055(3) Uiso 0.40 1 d PD B 2 C4S C 0.3352(15) 0.9070(10) 0.4083(4) 0.068(4) Uiso 0.40 1 d PD B 2 H41S H 0.2728 0.8900 0.4315 0.103 Uiso 0.40 1 d PR B 2 H42S H 0.3292 0.9766 0.4014 0.103 Uiso 0.40 1 d PR B 2 H43S H 0.4226 0.8915 0.4205 0.103 Uiso 0.40 1 d PR B 2 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 Mn1 0.0182(2) 0.0235(3) 0.0245(3) 0.0017(2) -0.00082(19) 0.0007(2) Mn2 0.0201(3) 0.0226(3) 0.0248(3) -0.0014(2) -0.00281(19) 0.0014(2) S1 0.0226(4) 0.0231(4) 0.0259(4) 0.0025(3) 0.0019(3) -0.0026(3) S2 0.0227(4) 0.0218(4) 0.0275(4) -0.0013(3) -0.0030(3) -0.0009(3) O11 0.0399(13) 0.0254(13) 0.0319(13) 0.0087(10) 0.0050(10) 0.0011(11) O12 0.0228(11) 0.0267(13) 0.0358(13) -0.0033(10) -0.0003(10) -0.0061(10) O21 0.0334(13) 0.0238(13) 0.0360(13) -0.0069(10) -0.0045(10) 0.0005(10) O22 0.0255(11) 0.0287(13) 0.0323(13) 0.0032(10) 0.0002(10) -0.0038(10) O1 0.0196(11) 0.0260(13) 0.0198(11) -0.0004(9) -0.0013(9) 0.0013(9) O2 0.0216(11) 0.0318(13) 0.0298(12) -0.0048(10) -0.0011(9) -0.0012(10) O3 0.0244(12) 0.0255(13) 0.0355(13) -0.0055(10) -0.0031(10) 0.0023(10) O4 0.0356(13) 0.0330(14) 0.0340(13) 0.0085(11) 0.0025(11) 0.0010(11) O5 0.0307(13) 0.0386(15) 0.0286(12) 0.0005(11) -0.0003(10) -0.0093(11) N1 0.0173(13) 0.0223(15) 0.0269(14) -0.0001(11) -0.0016(10) -0.0016(11) N2 0.0174(13) 0.0264(16) 0.0291(15) 0.0022(12) -0.0022(11) -0.0024(11) N3 0.0214(14) 0.0278(16) 0.0293(15) 0.0014(12) 0.0005(11) 0.0007(12) N4 0.0207(13) 0.0239(15) 0.0243(14) 0.0018(11) -0.0030(11) -0.0009(11) N5 0.0203(13) 0.0280(16) 0.0270(14) 0.0034(12) -0.0028(11) -0.0038(12) N6 0.0165(13) 0.0222(15) 0.0334(15) -0.0007(12) -0.0036(11) 0.0009(11) C1 0.0154(15) 0.0229(18) 0.0243(17) 0.0004(13) 0.0003(12) -0.0029(13) C2 0.0177(15) 0.0247(18) 0.0232(16) 0.0028(13) 0.0002(12) -0.0012(13) C3 0.0228(16) 0.028(2) 0.0279(18) 0.0060(14) -0.0002(13) -0.0022(14) C4 0.0225(16) 0.034(2) 0.0265(17) -0.0018(15) 0.0008(13) -0.0029(14) C5 0.0194(16) 0.0288(19) 0.0281(17) -0.0057(14) -0.0003(13) -0.0005(14) C6 0.0173(15) 0.0227(17) 0.0256(16) -0.0009(13) -0.0014(12) -0.0005(13) C7 0.051(2) 0.050(3) 0.0246(18) -0.0062(17) 0.0014(16) 0.006(2) C8 0.0192(16) 0.0277(19) 0.0295(18) 0.0039(14) -0.0069(13) -0.0030(14) C9 0.0186(16) 0.0264(18) 0.0296(18) 0.0005(14) -0.0043(13) -0.0039(14) C10 0.0365(19) 0.034(2) 0.0311(19) 0.0025(15) -0.0071(15) -0.0053(16) C11 0.048(2) 0.039(2) 0.041(2) -0.0096(18) -0.0141(18) -0.0074(19) C12 0.044(2) 0.025(2) 0.048(2) 0.0017(17) -0.0070(18) -0.0110(17) C13 0.0239(17) 0.034(2) 0.0343(19) 0.0063(16) -0.0050(14) -0.0046(15) C14 0.0238(16) 0.0188(17) 0.0331(18) 0.0010(14) -0.0028(14) 0.0002(13) C15 0.0205(16) 0.0246(19) 0.0267(17) -0.0024(14) -0.0041(13) -0.0020(14) C16 0.0318(19) 0.027(2) 0.038(2) -0.0058(15) -0.0051(15) 0.0043(15) C17 0.0220(17) 0.034(2) 0.045(2) -0.0101(17) 0.0005(15) 0.0071(15) C18 0.0234(17) 0.043(2) 0.037(2) -0.0094(17) 0.0072(15) -0.0004(16) C19 0.0249(17) 0.036(2) 0.0348(19) 0.0012(16) 0.0007(14) -0.0014(16) C20 0.0314(18) 0.0206(18) 0.0306(18) 0.0059(14) -0.0041(14) 0.0020(14) C21 0.0256(17) 0.0250(19) 0.0260(17) 0.0030(14) 0.0003(13) -0.0008(14) C22 0.0323(19) 0.035(2) 0.037(2) 0.0043(16) -0.0028(16) 0.0047(16) C23 0.032(2) 0.054(3) 0.044(2) 0.006(2) -0.0130(17) 0.0109(19) C24 0.0316(19) 0.052(3) 0.039(2) -0.0027(18) -0.0126(16) -0.0039(18) C25 0.0236(17) 0.037(2) 0.0342(19) -0.0002(16) -0.0046(14) -0.0058(15) C26 0.0206(16) 0.0292(19) 0.0316(18) -0.0045(14) 0.0018(13) 0.0038(14) C27 0.0131(15) 0.0271(19) 0.0317(18) -0.0010(14) -0.0026(13) 0.0005(13) C28 0.0257(17) 0.035(2) 0.0305(18) -0.0024(15) 0.0022(14) 0.0000(15) C29 0.0313(19) 0.046(2) 0.032(2) 0.0080(17) 0.0040(15) -0.0039(17) C30 0.0221(17) 0.030(2) 0.048(2) 0.0092(17) -0.0015(15) -0.0035(15) C31 0.0187(16) 0.0231(19) 0.042(2) -0.0027(15) -0.0049(14) -0.0011(14) C32 0.0278(18) 0.0252(18) 0.0187(16) -0.0030(13) -0.0029(13) 0.0003(15) C33 0.0326(19) 0.0275(19) 0.039(2) -0.0052(16) 0.0050(15) -0.0019(16) C34 0.0329(19) 0.031(2) 0.0219(17) -0.0008(14) 0.0025(14) -0.0031(16) C35 0.042(2) 0.044(2) 0.054(2) 0.021(2) 0.0051(19) -0.0040(19) Cl1 0.0417(5) 0.0368(5) 0.0397(5) -0.0069(4) -0.0065(4) 0.0025(4) O1A 0.078(2) 0.0410(17) 0.0592(19) -0.0037(14) 0.0237(16) 0.0068(16) O1B 0.0600(19) 0.057(2) 0.0614(19) 0.0032(15) -0.0137(15) 0.0190(15) O1C 0.092(2) 0.085(2) 0.0462(18) 0.0178(17) 0.0188(17) 0.011(2) O1D 0.069(2) 0.074(3) 0.143(4) -0.051(2) -0.061(2) 0.0138(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 Mn1 O4 2.054(2) . ? Mn1 O2 2.122(2) . ? Mn1 O1 2.147(2) . ? Mn1 N3 2.243(3) . ? Mn1 N2 2.309(3) . ? Mn1 N1 2.481(3) . ? Mn2 O3 2.068(2) . ? Mn2 O5 2.103(2) . ? Mn2 O1 2.150(2) . ? Mn2 N5 2.228(3) . ? Mn2 N6 2.322(3) . ? Mn2 N4 2.443(3) . ? S1 O12 1.431(2) . ? S1 O11 1.434(2) . ? S1 N1 1.699(2) . ? S1 C2 1.755(3) . ? S2 O22 1.428(2) . ? S2 O21 1.431(2) . ? S2 N4 1.697(3) . ? S2 C6 1.756(3) . ? O1 C1 1.314(3) . ? O2 C32 1.260(4) . ? O3 C32 1.267(4) . ? O4 C34 1.264(4) . ? O5 C34 1.262(4) . ? N1 C14 1.492(4) . ? N1 C8 1.496(4) . ? N2 C13 1.338(4) . ? N2 C9 1.359(4) . ? N3 C15 1.334(4) . ? N3 C19 1.336(4) . ? N4 C26 1.493(4) . ? N4 C20 1.499(4) . ? N5 C21 1.337(4) . ? N5 C25 1.347(4) . ? N6 C31 1.335(4) . ? N6 C27 1.346(4) . ? C1 C2 1.415(4) . ? C1 C6 1.417(4) . ? C2 C3 1.390(4) . ? C3 C4 1.382(5) . ? C3 H3A 0.950 . ? C4 C5 1.387(5) . ? C4 C7 1.506(4) . ? C5 C6 1.386(4) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.493(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.377(5) . ? C10 C11 1.382(5) . ? C10 H10A 0.950 . ? C11 C12 1.374(5) . ? C11 H11A 0.950 . ? C12 C13 1.383(5) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.510(4) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.392(4) . ? C16 C17 1.378(5) . ? C16 H16A 0.950 . ? C17 C18 1.383(5) . ? C17 H17A 0.950 . ? C18 C19 1.384(5) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.509(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.386(5) . ? C22 C23 1.377(5) . ? C22 H22A 0.950 . ? C23 C24 1.382(6) . ? C23 H23A 0.950 . ? C24 C25 1.370(5) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.503(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.383(5) . ? C28 C29 1.380(5) . ? C28 H28A 0.950 . ? C29 C30 1.377(5) . ? C29 H29A 0.950 . ? C30 C31 1.380(5) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C32 C33 1.501(4) . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 C35 1.490(5) . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? Cl1 O1D 1.414(3) . ? Cl1 O1A 1.419(3) . ? Cl1 O1B 1.423(3) . ? Cl1 O1C 1.427(3) . ? N1S C1S 1.133(7) . ? C1S C2S 1.456(7) . ? C2S H21S 0.980 . ? C2S H22S 0.980 . ? C2S H23S 0.980 . ? N2S C3S 1.143(7) . ? C3S C4S 1.444(8) . ? C4S H41S 0.980 . ? C4S H42S 0.980 . ? C4S H43S 0.980 . ? 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 O4 Mn1 O2 104.31(9) . . ? O4 Mn1 O1 102.87(9) . . ? O2 Mn1 O1 91.57(8) . . ? O4 Mn1 N3 102.94(9) . . ? O2 Mn1 N3 86.02(9) . . ? O1 Mn1 N3 153.87(9) . . ? O4 Mn1 N2 91.24(9) . . ? O2 Mn1 N2 164.40(9) . . ? O1 Mn1 N2 86.09(8) . . ? N3 Mn1 N2 89.31(9) . . ? O4 Mn1 N1 162.96(9) . . ? O2 Mn1 N1 91.58(8) . . ? O1 Mn1 N1 82.46(8) . . ? N3 Mn1 N1 71.62(9) . . ? N2 Mn1 N1 72.83(8) . . ? O3 Mn2 O5 103.37(9) . . ? O3 Mn2 O1 96.06(8) . . ? O5 Mn2 O1 89.58(8) . . ? O3 Mn2 N5 106.40(9) . . ? O5 Mn2 N5 87.58(9) . . ? O1 Mn2 N5 157.41(9) . . ? O3 Mn2 N6 90.88(9) . . ? O5 Mn2 N6 165.30(9) . . ? O1 Mn2 N6 85.28(8) . . ? N5 Mn2 N6 91.89(9) . . ? O3 Mn2 N4 163.28(9) . . ? O5 Mn2 N4 93.32(9) . . ? O1 Mn2 N4 85.06(8) . . ? N5 Mn2 N4 72.75(9) . . ? N6 Mn2 N4 72.55(9) . . ? O12 S1 O11 117.90(14) . . ? O12 S1 N1 106.11(12) . . ? O11 S1 N1 108.97(13) . . ? O12 S1 C2 112.45(14) . . ? O11 S1 C2 108.46(14) . . ? N1 S1 C2 101.64(13) . . ? O22 S2 O21 117.95(14) . . ? O22 S2 N4 105.96(13) . . ? O21 S2 N4 109.93(13) . . ? O22 S2 C6 111.71(14) . . ? O21 S2 C6 108.10(14) . . ? N4 S2 C6 102.00(14) . . ? C1 O1 Mn1 127.41(18) . . ? C1 O1 Mn2 125.78(18) . . ? Mn1 O1 Mn2 106.73(8) . . ? C32 O2 Mn1 135.9(2) . . ? C32 O3 Mn2 127.58(19) . . ? C34 O4 Mn1 122.5(2) . . ? C34 O5 Mn2 144.6(2) . . ? C14 N1 C8 113.0(2) . . ? C14 N1 S1 110.04(19) . . ? C8 N1 S1 111.31(19) . . ? C14 N1 Mn1 100.88(17) . . ? C8 N1 Mn1 107.96(17) . . ? S1 N1 Mn1 113.24(12) . . ? C13 N2 C9 117.8(3) . . ? C13 N2 Mn1 120.6(2) . . ? C9 N2 Mn1 116.8(2) . . ? C15 N3 C19 118.5(3) . . ? C15 N3 Mn1 117.4(2) . . ? C19 N3 Mn1 124.1(2) . . ? C26 N4 C20 112.3(2) . . ? C26 N4 S2 111.9(2) . . ? C20 N4 S2 110.0(2) . . ? C26 N4 Mn2 109.38(18) . . ? C20 N4 Mn2 101.41(18) . . ? S2 N4 Mn2 111.51(12) . . ? C21 N5 C25 118.1(3) . . ? C21 N5 Mn2 117.0(2) . . ? C25 N5 Mn2 124.9(2) . . ? C31 N6 C27 117.8(3) . . ? C31 N6 Mn2 120.7(2) . . ? C27 N6 Mn2 117.3(2) . . ? O1 C1 C2 122.5(3) . . ? O1 C1 C6 122.4(3) . . ? C2 C1 C6 115.0(3) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 S1 118.4(2) . . ? C1 C2 S1 119.2(2) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C7 121.2(3) . . ? C5 C4 C7 121.1(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 S2 118.2(2) . . ? C1 C6 S2 120.0(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 N1 112.7(2) . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? N1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C10 121.9(3) . . ? N2 C9 C8 116.5(3) . . ? C10 C9 C8 121.5(3) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 118.2(3) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? N2 C13 C12 123.3(3) . . ? N2 C13 H13A 118.4 . . ? C12 C13 H13A 118.4 . . ? N1 C14 C15 110.3(2) . . ? N1 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N1 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N3 C15 C16 122.2(3) . . ? N3 C15 C14 117.3(3) . . ? C16 C15 C14 120.4(3) . . ? C17 C16 C15 118.6(3) . . ? C17 C16 H16A 120.7 . . ? C15 C16 H16A 120.7 . . ? C16 C17 C18 119.6(3) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C19 118.0(3) . . ? C17 C18 H18A 121.0 . . ? C19 C18 H18A 121.0 . . ? N3 C19 C18 123.0(3) . . ? N3 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? N4 C20 C21 110.2(3) . . ? N4 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? N4 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N5 C21 C22 122.4(3) . . ? N5 C21 C20 117.2(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C25 C24 C23 118.8(3) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? N5 C25 C24 122.8(3) . . ? N5 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? N4 C26 C27 112.3(2) . . ? N4 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? N4 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? N6 C27 C28 122.4(3) . . ? N6 C27 C26 116.5(3) . . ? C28 C27 C26 121.1(3) . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C30 C29 C28 118.6(3) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? C29 C30 C31 119.0(3) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? N6 C31 C30 123.0(3) . . ? N6 C31 H31A 118.5 . . ? C30 C31 H31A 118.5 . . ? O2 C32 O3 124.6(3) . . ? O2 C32 C33 118.6(3) . . ? O3 C32 C33 116.8(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O5 C34 O4 123.5(3) . . ? O5 C34 C35 118.6(3) . . ? O4 C34 C35 117.9(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1D Cl1 O1A 110.4(2) . . ? O1D Cl1 O1B 109.7(2) . . ? O1A Cl1 O1B 109.61(19) . . ? O1D Cl1 O1C 109.4(3) . . ? O1A Cl1 O1C 108.55(19) . . ? O1B Cl1 O1C 109.1(2) . . ? N1S C1S C2S 173.0(11) . . ? N1S C1S H41S 115.5 . . ? C1S C2S H21S 109.1 . . ? C1S C2S H22S 109.5 . . ? C1S C2S H23S 109.8 . . ? H21S C2S H22S 109.5 . . ? H21S C2S H23S 109.5 . . ? H22S C2S H23S 109.5 . . ? N2S C3S C4S 177.4(14) . . ? C3S C4S H41S 109.8 . . ? C3S C4S H42S 109.3 . . ? C3S C4S H43S 109.3 . . ? H41S C4S H42S 109.5 . . ? H41S C4S H43S 109.5 . . ? H42S C4S H43S 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 O4 Mn1 O1 C1 121.9(2) . . . . ? O2 Mn1 O1 C1 -133.0(2) . . . . ? N3 Mn1 O1 C1 -48.9(3) . . . . ? N2 Mn1 O1 C1 31.5(2) . . . . ? N1 Mn1 O1 C1 -41.7(2) . . . . ? O4 Mn1 O1 Mn2 -54.96(11) . . . . ? O2 Mn1 O1 Mn2 50.10(10) . . . . ? N3 Mn1 O1 Mn2 134.26(18) . . . . ? N2 Mn1 O1 Mn2 -145.34(10) . . . . ? N1 Mn1 O1 Mn2 141.49(10) . . . . ? O3 Mn2 O1 C1 124.0(2) . . . . ? O5 Mn2 O1 C1 -132.6(2) . . . . ? N5 Mn2 O1 C1 -50.0(3) . . . . ? N6 Mn2 O1 C1 33.6(2) . . . . ? N4 Mn2 O1 C1 -39.3(2) . . . . ? O3 Mn2 O1 Mn1 -59.11(10) . . . . ? O5 Mn2 O1 Mn1 44.29(10) . . . . ? N5 Mn2 O1 Mn1 127.0(2) . . . . ? N6 Mn2 O1 Mn1 -149.50(10) . . . . ? N4 Mn2 O1 Mn1 137.65(10) . . . . ? O4 Mn1 O2 C32 96.7(3) . . . . ? O1 Mn1 O2 C32 -7.0(3) . . . . ? N3 Mn1 O2 C32 -161.0(3) . . . . ? N2 Mn1 O2 C32 -88.1(4) . . . . ? N1 Mn1 O2 C32 -89.5(3) . . . . ? O5 Mn2 O3 C32 -64.0(3) . . . . ? O1 Mn2 O3 C32 27.0(3) . . . . ? N5 Mn2 O3 C32 -155.4(2) . . . . ? N6 Mn2 O3 C32 112.4(3) . . . . ? N4 Mn2 O3 C32 120.0(3) . . . . ? O2 Mn1 O4 C34 -71.1(3) . . . . ? O1 Mn1 O4 C34 24.0(3) . . . . ? N3 Mn1 O4 C34 -160.2(2) . . . . ? N2 Mn1 O4 C34 110.2(3) . . . . ? N1 Mn1 O4 C34 130.6(3) . . . . ? O3 Mn2 O5 C34 88.3(4) . . . . ? O1 Mn2 O5 C34 -7.9(4) . . . . ? N5 Mn2 O5 C34 -165.5(4) . . . . ? N6 Mn2 O5 C34 -77.3(6) . . . . ? N4 Mn2 O5 C34 -92.9(4) . . . . ? O12 S1 N1 C14 56.5(2) . . . . ? O11 S1 N1 C14 -71.4(2) . . . . ? C2 S1 N1 C14 174.3(2) . . . . ? O12 S1 N1 C8 -177.3(2) . . . . ? O11 S1 N1 C8 54.8(2) . . . . ? C2 S1 N1 C8 -59.6(2) . . . . ? O12 S1 N1 Mn1 -55.49(16) . . . . ? O11 S1 N1 Mn1 176.60(12) . . . . ? C2 S1 N1 Mn1 62.23(15) . . . . ? O4 Mn1 N1 C14 110.6(3) . . . . ? O2 Mn1 N1 C14 -48.48(17) . . . . ? O1 Mn1 N1 C14 -139.85(17) . . . . ? N3 Mn1 N1 C14 36.80(16) . . . . ? N2 Mn1 N1 C14 131.93(18) . . . . ? O4 Mn1 N1 C8 -8.2(4) . . . . ? O2 Mn1 N1 C8 -167.23(18) . . . . ? O1 Mn1 N1 C8 101.39(18) . . . . ? N3 Mn1 N1 C8 -81.95(19) . . . . ? N2 Mn1 N1 C8 13.18(18) . . . . ? O4 Mn1 N1 S1 -131.9(3) . . . . ? O2 Mn1 N1 S1 69.06(13) . . . . ? O1 Mn1 N1 S1 -22.31(13) . . . . ? N3 Mn1 N1 S1 154.34(15) . . . . ? N2 Mn1 N1 S1 -110.53(14) . . . . ? O4 Mn1 N2 C13 -22.7(2) . . . . ? O2 Mn1 N2 C13 161.9(3) . . . . ? O1 Mn1 N2 C13 80.1(2) . . . . ? N3 Mn1 N2 C13 -125.7(2) . . . . ? N1 Mn1 N2 C13 163.4(3) . . . . ? O4 Mn1 N2 C9 -177.7(2) . . . . ? O2 Mn1 N2 C9 6.9(5) . . . . ? O1 Mn1 N2 C9 -74.9(2) . . . . ? N3 Mn1 N2 C9 79.4(2) . . . . ? N1 Mn1 N2 C9 8.5(2) . . . . ? O4 Mn1 N3 C15 175.2(2) . . . . ? O2 Mn1 N3 C15 71.4(2) . . . . ? O1 Mn1 N3 C15 -14.1(4) . . . . ? N2 Mn1 N3 C15 -93.7(2) . . . . ? N1 Mn1 N3 C15 -21.6(2) . . . . ? O4 Mn1 N3 C19 -2.2(3) . . . . ? O2 Mn1 N3 C19 -106.0(3) . . . . ? O1 Mn1 N3 C19 168.6(2) . . . . ? N2 Mn1 N3 C19 88.9(3) . . . . ? N1 Mn1 N3 C19 161.0(3) . . . . ? O22 S2 N4 C26 -177.1(2) . . . . ? O21 S2 N4 C26 54.4(2) . . . . ? C6 S2 N4 C26 -60.1(2) . . . . ? O22 S2 N4 C20 57.4(2) . . . . ? O21 S2 N4 C20 -71.1(2) . . . . ? C6 S2 N4 C20 174.4(2) . . . . ? O22 S2 N4 Mn2 -54.24(15) . . . . ? O21 S2 N4 Mn2 177.28(12) . . . . ? C6 S2 N4 Mn2 62.76(15) . . . . ? O3 Mn2 N4 C26 6.4(4) . . . . ? O5 Mn2 N4 C26 -169.71(18) . . . . ? O1 Mn2 N4 C26 101.00(18) . . . . ? N5 Mn2 N4 C26 -83.29(19) . . . . ? N6 Mn2 N4 C26 14.40(18) . . . . ? O3 Mn2 N4 C20 125.1(3) . . . . ? O5 Mn2 N4 C20 -50.98(18) . . . . ? O1 Mn2 N4 C20 -140.28(18) . . . . ? N5 Mn2 N4 C20 35.44(17) . . . . ? N6 Mn2 N4 C20 133.13(19) . . . . ? O3 Mn2 N4 S2 -117.9(3) . . . . ? O5 Mn2 N4 S2 66.00(13) . . . . ? O1 Mn2 N4 S2 -23.29(12) . . . . ? N5 Mn2 N4 S2 152.42(15) . . . . ? N6 Mn2 N4 S2 -109.89(14) . . . . ? O3 Mn2 N5 C21 177.9(2) . . . . ? O5 Mn2 N5 C21 74.6(2) . . . . ? O1 Mn2 N5 C21 -8.4(4) . . . . ? N6 Mn2 N5 C21 -90.7(2) . . . . ? N4 Mn2 N5 C21 -19.6(2) . . . . ? O3 Mn2 N5 C25 -0.9(3) . . . . ? O5 Mn2 N5 C25 -104.2(2) . . . . ? O1 Mn2 N5 C25 172.8(2) . . . . ? N6 Mn2 N5 C25 90.5(2) . . . . ? N4 Mn2 N5 C25 161.6(3) . . . . ? O3 Mn2 N6 C31 -19.8(2) . . . . ? O5 Mn2 N6 C31 146.1(3) . . . . ? O1 Mn2 N6 C31 76.2(2) . . . . ? N5 Mn2 N6 C31 -126.2(2) . . . . ? N4 Mn2 N6 C31 162.5(2) . . . . ? O3 Mn2 N6 C27 -176.0(2) . . . . ? O5 Mn2 N6 C27 -10.1(5) . . . . ? O1 Mn2 N6 C27 -80.0(2) . . . . ? N5 Mn2 N6 C27 77.6(2) . . . . ? N4 Mn2 N6 C27 6.3(2) . . . . ? Mn1 O1 C1 C2 59.6(4) . . . . ? Mn2 O1 C1 C2 -124.2(3) . . . . ? Mn1 O1 C1 C6 -119.3(3) . . . . ? Mn2 O1 C1 C6 57.0(3) . . . . ? O1 C1 C2 C3 -178.4(3) . . . . ? C6 C1 C2 C3 0.5(4) . . . . ? O1 C1 C2 S1 2.4(4) . . . . ? C6 C1 C2 S1 -178.7(2) . . . . ? O12 S1 C2 C3 -128.6(2) . . . . ? O11 S1 C2 C3 3.6(3) . . . . ? N1 S1 C2 C3 118.3(2) . . . . ? O12 S1 C2 C1 50.6(3) . . . . ? O11 S1 C2 C1 -177.2(2) . . . . ? N1 S1 C2 C1 -62.4(3) . . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? S1 C2 C3 C4 178.3(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C2 C3 C4 C7 178.5(3) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C7 C4 C5 C6 -177.4(3) . . . . ? C4 C5 C6 C1 -1.2(5) . . . . ? C4 C5 C6 S2 176.1(2) . . . . ? O1 C1 C6 C5 179.4(3) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? O1 C1 C6 S2 2.1(4) . . . . ? C2 C1 C6 S2 -176.8(2) . . . . ? O22 S2 C6 C5 -128.1(2) . . . . ? O21 S2 C6 C5 3.2(3) . . . . ? N4 S2 C6 C5 119.1(2) . . . . ? O22 S2 C6 C1 49.3(3) . . . . ? O21 S2 C6 C1 -179.3(2) . . . . ? N4 S2 C6 C1 -63.5(3) . . . . ? C14 N1 C8 C9 -142.7(3) . . . . ? S1 N1 C8 C9 92.9(3) . . . . ? Mn1 N1 C8 C9 -32.0(3) . . . . ? C13 N2 C9 C10 -2.6(5) . . . . ? Mn1 N2 C9 C10 153.1(3) . . . . ? C13 N2 C9 C8 174.1(3) . . . . ? Mn1 N2 C9 C8 -30.3(3) . . . . ? N1 C8 C9 N2 43.1(4) . . . . ? N1 C8 C9 C10 -140.3(3) . . . . ? N2 C9 C10 C11 1.8(5) . . . . ? C8 C9 C10 C11 -174.7(3) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? C10 C11 C12 C13 -1.6(6) . . . . ? C9 N2 C13 C12 1.3(5) . . . . ? Mn1 N2 C13 C12 -153.5(3) . . . . ? C11 C12 C13 N2 0.8(5) . . . . ? C8 N1 C14 C15 66.1(3) . . . . ? S1 N1 C14 C15 -168.7(2) . . . . ? Mn1 N1 C14 C15 -48.9(2) . . . . ? C19 N3 C15 C16 0.5(5) . . . . ? Mn1 N3 C15 C16 -177.0(2) . . . . ? C19 N3 C15 C14 178.1(3) . . . . ? Mn1 N3 C15 C14 0.6(4) . . . . ? N1 C14 C15 N3 37.1(4) . . . . ? N1 C14 C15 C16 -145.3(3) . . . . ? N3 C15 C16 C17 1.3(5) . . . . ? C14 C15 C16 C17 -176.2(3) . . . . ? C15 C16 C17 C18 -2.0(5) . . . . ? C16 C17 C18 C19 0.9(5) . . . . ? C15 N3 C19 C18 -1.7(5) . . . . ? Mn1 N3 C19 C18 175.6(2) . . . . ? C17 C18 C19 N3 1.0(5) . . . . ? C26 N4 C20 C21 68.7(3) . . . . ? S2 N4 C20 C21 -166.1(2) . . . . ? Mn2 N4 C20 C21 -48.0(3) . . . . ? C25 N5 C21 C22 -0.6(5) . . . . ? Mn2 N5 C21 C22 -179.5(2) . . . . ? C25 N5 C21 C20 177.0(3) . . . . ? Mn2 N5 C21 C20 -1.9(4) . . . . ? N4 C20 C21 N5 37.6(4) . . . . ? N4 C20 C21 C22 -144.7(3) . . . . ? N5 C21 C22 C23 0.4(5) . . . . ? C20 C21 C22 C23 -177.1(3) . . . . ? C21 C22 C23 C24 0.4(5) . . . . ? C22 C23 C24 C25 -0.9(6) . . . . ? C21 N5 C25 C24 0.0(5) . . . . ? Mn2 N5 C25 C24 178.8(3) . . . . ? C23 C24 C25 N5 0.7(5) . . . . ? C20 N4 C26 C27 -143.7(3) . . . . ? S2 N4 C26 C27 92.1(3) . . . . ? Mn2 N4 C26 C27 -32.0(3) . . . . ? C31 N6 C27 C28 -1.8(4) . . . . ? Mn2 N6 C27 C28 155.1(2) . . . . ? C31 N6 C27 C26 176.0(3) . . . . ? Mn2 N6 C27 C26 -27.0(3) . . . . ? N4 C26 C27 N6 40.5(4) . . . . ? N4 C26 C27 C28 -141.6(3) . . . . ? N6 C27 C28 C29 1.4(5) . . . . ? C26 C27 C28 C29 -176.4(3) . . . . ? C27 C28 C29 C30 0.4(5) . . . . ? C28 C29 C30 C31 -1.7(5) . . . . ? C27 N6 C31 C30 0.4(4) . . . . ? Mn2 N6 C31 C30 -155.7(2) . . . . ? C29 C30 C31 N6 1.4(5) . . . . ? Mn1 O2 C32 O3 -35.3(5) . . . . ? Mn1 O2 C32 C33 143.9(3) . . . . ? Mn2 O3 C32 O2 21.0(4) . . . . ? Mn2 O3 C32 C33 -158.1(2) . . . . ? Mn2 O5 C34 O4 -31.3(6) . . . . ? Mn2 O5 C34 C35 148.1(3) . . . . ? Mn1 O4 C34 O5 17.9(4) . . . . ? Mn1 O4 C34 C35 -161.5(2) . . . . ? #======================================================================= data_8 _database_code_depnum_ccdc_archive 'CCDC 737978' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C35 H35 Co2 N6 O9 S2 +, Cl O4 -, C H4 O, 2(H2 O) ; _chemical_formula_sum 'C36 H43 Cl Co2 N6 O16 S2' _chemical_formula_weight 1033.19 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.4899(9) _cell_length_b 17.0596(5) _cell_length_c 18.0011(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.150(1) _cell_angle_gamma 90.00 _cell_volume 8713.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9419 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.90 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The perchlorate anion is modelled as disordered over two orientations, with restrained geometry and an isotropic displacement parameter common to all O atoms. The site occupancies of the O atoms were refined, then subsequently fixed. ** The O atom positions are approximate ** Atom O1F in particular lies too close to O2W. ** The model is an approximation to a spherically disordered perchlorate ** H atoms involved with the lattice water and ethanol molecules were placed along the O...O vectors so as to form a reasonable H-bond network, then allowed to ride on their parent O atoms. ; _diffrn_ambient_temperature 180(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 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 79861 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 8879 _reflns_number_gt 7092 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _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^)+(0.0722P)^2^+30.9053P] 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 8879 _refine_ls_number_parameters 546 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.077 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.089 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 0.097508(15) 0.38727(3) 0.07812(3) 0.02229(13) Uani 1 1 d . . . Co2 Co 0.168882(15) 0.54517(3) 0.10241(3) 0.02022(12) Uani 1 1 d . . . S1 S 0.18613(3) 0.30221(5) 0.24492(5) 0.02436(19) Uani 1 1 d . . . S2 S 0.20852(3) 0.44756(5) -0.00716(5) 0.02469(19) Uani 1 1 d . . . O1 O 0.16385(7) 0.42361(13) 0.10569(14) 0.0207(5) Uani 1 1 d . . . O2 O 0.09370(9) 0.46813(14) 0.16063(16) 0.0308(6) Uani 1 1 d . . . O3 O 0.13621(8) 0.57377(14) 0.16881(16) 0.0285(5) Uani 1 1 d . . . O4 O 0.05987(8) 0.45425(14) -0.02570(16) 0.0316(6) Uani 1 1 d . . . O5 O 0.10837(8) 0.55236(14) -0.01377(15) 0.0284(5) Uani 1 1 d . . . O11 O 0.20626(9) 0.23401(16) 0.29710(16) 0.0340(6) Uani 1 1 d . . . O12 O 0.18694(9) 0.37428(15) 0.28604(15) 0.0301(5) Uani 1 1 d . . . O21 O 0.24221(10) 0.44169(16) -0.03659(17) 0.0358(6) Uani 1 1 d . . . O22 O 0.15977(9) 0.43941(14) -0.06732(15) 0.0302(5) Uani 1 1 d . . . N1 N 0.12885(9) 0.28460(16) 0.17346(18) 0.0241(6) Uani 1 1 d . . . N2 N 0.10017(10) 0.29297(17) 0.00234(18) 0.0267(6) Uani 1 1 d . . . N3 N 0.03875(10) 0.33621(17) 0.07876(19) 0.0274(6) Uani 1 1 d . . . N4 N 0.21463(10) 0.53646(16) 0.03995(17) 0.0223(6) Uani 1 1 d . . . N5 N 0.17647(10) 0.66310(16) 0.07261(18) 0.0247(6) Uani 1 1 d . . . N6 N 0.23748(10) 0.53646(16) 0.20924(17) 0.0223(6) Uani 1 1 d . . . C1 C 0.19837(11) 0.37523(18) 0.1201(2) 0.0207(6) Uani 1 1 d . . . C2 C 0.21183(11) 0.31298(19) 0.1791(2) 0.0227(7) Uani 1 1 d . . . C3 C 0.24795(12) 0.2609(2) 0.1927(2) 0.0261(7) Uani 1 1 d . . . H3A H 0.2547 0.2185 0.2311 0.031 Uiso 1 1 calc R . . C4 C 0.27434(12) 0.2697(2) 0.1512(2) 0.0278(7) Uani 1 1 d . . . C5 C 0.26199(12) 0.3305(2) 0.0934(2) 0.0261(7) Uani 1 1 d . . . H5A H 0.2793 0.3379 0.0640 0.031 Uiso 1 1 calc R . . C6 C 0.22502(11) 0.38129(19) 0.0769(2) 0.0225(7) Uani 1 1 d . . . C7 C 0.31505(14) 0.2168(2) 0.1691(3) 0.0398(9) Uani 1 1 d . . . H7A H 0.3169 0.2091 0.1168 0.060 Uiso 1 1 calc R . . H7B H 0.3105 0.1660 0.1896 0.060 Uiso 1 1 calc R . . H7C H 0.3444 0.2407 0.2126 0.060 Uiso 1 1 calc R . . C8 C 0.12322(13) 0.2099(2) 0.1264(2) 0.0287(7) Uani 1 1 d . . . H8A H 0.0974 0.1790 0.1265 0.034 Uiso 1 1 calc R . . H8B H 0.1526 0.1789 0.1569 0.034 Uiso 1 1 calc R . . C9 C 0.11252(13) 0.2215(2) 0.0359(2) 0.0304(8) Uani 1 1 d . . . C10 C 0.1141(2) 0.1584(3) -0.0107(3) 0.0570(13) Uani 1 1 d . . . H10A H 0.1236 0.1082 0.0151 0.068 Uiso 1 1 calc R . . C11 C 0.1017(2) 0.1688(3) -0.0945(3) 0.0674(16) Uani 1 1 d . . . H11A H 0.1024 0.1259 -0.1275 0.081 Uiso 1 1 calc R . . C12 C 0.08833(18) 0.2421(3) -0.1303(3) 0.0514(12) Uani 1 1 d . . . H12A H 0.0792 0.2506 -0.1884 0.062 Uiso 1 1 calc R . . C13 C 0.08842(14) 0.3027(2) -0.0800(2) 0.0347(8) Uani 1 1 d . . . H13A H 0.0799 0.3536 -0.1042 0.042 Uiso 1 1 calc R . . C14 C 0.09834(12) 0.2873(2) 0.2145(2) 0.0302(8) Uani 1 1 d . . . H14A H 0.1059 0.3344 0.2510 0.036 Uiso 1 1 calc R . . H14B H 0.1039 0.2403 0.2504 0.036 Uiso 1 1 calc R . . C15 C 0.04770(13) 0.2899(2) 0.1452(3) 0.0319(8) Uani 1 1 d . . . C16 C 0.01232(15) 0.2483(2) 0.1494(3) 0.0432(10) Uani 1 1 d . . . H16A H 0.0193 0.2153 0.1965 0.052 Uiso 1 1 calc R . . C17 C -0.03351(15) 0.2558(3) 0.0833(3) 0.0529(12) Uani 1 1 d . . . H17A H -0.0584 0.2276 0.0846 0.063 Uiso 1 1 calc R . . C18 C -0.04274(14) 0.3045(3) 0.0159(3) 0.0460(11) Uani 1 1 d . . . H18A H -0.0740 0.3113 -0.0294 0.055 Uiso 1 1 calc R . . C19 C -0.00566(13) 0.3429(2) 0.0159(3) 0.0359(9) Uani 1 1 d . . . H19A H -0.0118 0.3759 -0.0309 0.043 Uiso 1 1 calc R . . C20 C 0.19583(13) 0.5992(2) -0.0266(2) 0.0288(8) Uani 1 1 d . . . H20A H 0.1658 0.5818 -0.0756 0.035 Uiso 1 1 calc R . . H20B H 0.2186 0.6097 -0.0471 0.035 Uiso 1 1 calc R . . C21 C 0.18784(12) 0.6726(2) 0.0108(2) 0.0257(7) Uani 1 1 d . . . C22 C 0.19046(14) 0.7463(2) -0.0192(2) 0.0361(9) Uani 1 1 d . . . H22A H 0.1989 0.7519 -0.0626 0.043 Uiso 1 1 calc R . . C23 C 0.18062(15) 0.8115(2) 0.0151(3) 0.0430(10) Uani 1 1 d . . . H23A H 0.1823 0.8626 -0.0044 0.052 Uiso 1 1 calc R . . C24 C 0.16832(14) 0.8015(2) 0.0778(3) 0.0398(9) Uani 1 1 d . . . H24A H 0.1611 0.8454 0.1019 0.048 Uiso 1 1 calc R . . C25 C 0.16666(12) 0.7265(2) 0.1049(2) 0.0289(7) Uani 1 1 d . . . H25A H 0.1582 0.7197 0.1482 0.035 Uiso 1 1 calc R . . C26 C 0.26428(12) 0.5525(2) 0.1060(2) 0.0262(7) Uani 1 1 d . . . H26A H 0.2711 0.6088 0.1045 0.031 Uiso 1 1 calc R . . H26B H 0.2857 0.5222 0.0924 0.031 Uiso 1 1 calc R . . C27 C 0.27401(11) 0.53153(19) 0.1940(2) 0.0238(7) Uani 1 1 d . . . C28 C 0.31900(12) 0.5122(2) 0.2569(2) 0.0306(8) Uani 1 1 d . . . H28A H 0.3440 0.5073 0.2440 0.037 Uiso 1 1 calc R . . C29 C 0.32703(13) 0.5003(2) 0.3390(2) 0.0329(8) Uani 1 1 d . . . H29A H 0.3577 0.4876 0.3834 0.039 Uiso 1 1 calc R . . C30 C 0.28986(13) 0.5070(2) 0.3555(2) 0.0303(8) Uani 1 1 d . . . H30A H 0.2946 0.4999 0.4115 0.036 Uiso 1 1 calc R . . C31 C 0.24586(13) 0.5242(2) 0.2893(2) 0.0262(7) Uani 1 1 d . . . H31A H 0.2202 0.5275 0.3006 0.031 Uiso 1 1 calc R . . C32 C 0.10595(11) 0.53764(19) 0.1800(2) 0.0226(7) Uani 1 1 d . . . C33 C 0.08295(13) 0.5836(2) 0.2218(2) 0.0326(8) Uani 1 1 d . . . H33A H 0.0503 0.5660 0.1994 0.049 Uiso 1 1 calc R . . H33B H 0.0832 0.6396 0.2096 0.049 Uiso 1 1 calc R . . H33C H 0.1004 0.5752 0.2834 0.049 Uiso 1 1 calc R . . C34 C 0.07137(12) 0.5132(2) -0.0533(2) 0.0250(7) Uani 1 1 d . . . C35 C 0.03697(14) 0.5384(3) -0.1424(2) 0.0401(9) Uani 1 1 d . . . H35A H 0.0483 0.5865 -0.1561 0.060 Uiso 1 1 calc R . . H35B H 0.0061 0.5482 -0.1468 0.060 Uiso 1 1 calc R . . H35C H 0.0340 0.4970 -0.1824 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.09596(5) 0.06035(8) 0.34423(13) 0.0862(5) Uani 1 1 d D . . O1D O 0.1267(2) 0.1142(3) 0.3263(4) 0.0706(14) Uiso 0.70 1 d PD A 1 O1C O 0.0806(2) 0.0026(4) 0.2780(4) 0.0861(18) Uiso 0.70 1 d PD A 1 O1B O 0.1244(3) 0.0272(5) 0.4241(4) 0.108(2) Uiso 0.70 1 d PD A 1 O1A O 0.0601(3) 0.1103(4) 0.3339(5) 0.112(2) Uiso 0.70 1 d PD A 1 O1E O 0.1372(3) 0.0158(6) 0.3955(7) 0.056(3) Uiso 0.30 1 d PD A 2 O1F O 0.0877(8) 0.0664(12) 0.4215(10) 0.164(9) Uiso 0.30 1 d PD A 2 O1G O 0.0566(5) 0.0083(9) 0.3022(10) 0.121(6) Uiso 0.30 1 d PD A 2 O1H O 0.0950(7) 0.1383(6) 0.3310(11) 0.120(6) Uiso 0.30 1 d PD A 2 O1W O 0.0426(4) 0.0595(6) 0.0982(7) 0.217(2) Uiso 1 1 d . . . H1W H 0.0532 0.0437 0.1485 0.326 Uiso 1 1 d R . . H2W H 0.0131 0.0617 0.0683 0.326 Uiso 1 1 d R . . O2W O 0.0518(4) 0.0653(6) 0.4996(7) 0.217(2) Uiso 1 1 d . . . H3W H 0.0491 0.0289 0.5285 0.326 Uiso 1 1 d R . . H4W H 0.0655 0.0651 0.4704 0.326 Uiso 1 1 d R . . O1S O 0.0723(4) 0.8288(6) 0.1548(7) 0.217(2) Uiso 1 1 d . . . H1S H 0.0669 0.8571 0.1128 0.326 Uiso 1 1 d R . . C1S C 0.0255(6) 0.8270(9) 0.1354(11) 0.217(2) Uiso 1 1 d . . . H1S1 H 0.0207 0.8636 0.1725 0.326 Uiso 1 1 calc R . . H1S2 H 0.0173 0.7738 0.1443 0.326 Uiso 1 1 calc R . . H1S3 H 0.0054 0.8422 0.0759 0.326 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 0.0204(2) 0.0201(2) 0.0245(2) 0.00000(17) 0.00945(19) -0.00054(17) Co2 0.0206(2) 0.0204(2) 0.0198(2) 0.00048(17) 0.00992(18) -0.00062(17) S1 0.0236(4) 0.0293(4) 0.0198(4) 0.0049(3) 0.0103(3) 0.0018(3) S2 0.0314(4) 0.0267(4) 0.0191(4) 0.0000(3) 0.0148(3) 0.0012(3) O1 0.0197(11) 0.0191(11) 0.0232(11) 0.0018(9) 0.0103(9) 0.0018(9) O2 0.0358(14) 0.0268(13) 0.0376(14) -0.0067(11) 0.0239(12) -0.0046(11) O3 0.0299(13) 0.0278(13) 0.0351(14) -0.0055(10) 0.0216(11) -0.0050(10) O4 0.0252(12) 0.0271(13) 0.0320(13) 0.0057(11) 0.0058(11) 0.0012(10) O5 0.0243(12) 0.0273(13) 0.0254(12) 0.0037(10) 0.0055(10) -0.0001(10) O11 0.0311(13) 0.0397(15) 0.0290(13) 0.0151(11) 0.0130(11) 0.0064(11) O12 0.0324(13) 0.0378(14) 0.0218(12) -0.0032(10) 0.0146(11) -0.0034(11) O21 0.0472(16) 0.0401(15) 0.0345(14) 0.0002(12) 0.0311(13) 0.0029(12) O22 0.0355(14) 0.0304(13) 0.0199(12) -0.0018(10) 0.0098(10) -0.0006(10) N1 0.0226(14) 0.0243(14) 0.0258(14) 0.0022(12) 0.0120(12) 0.0000(11) N2 0.0276(15) 0.0236(14) 0.0265(15) -0.0005(12) 0.0112(12) -0.0013(12) N3 0.0233(14) 0.0230(14) 0.0351(16) -0.0021(12) 0.0134(13) -0.0006(11) N4 0.0257(14) 0.0241(14) 0.0193(13) 0.0023(11) 0.0125(11) 0.0005(11) N5 0.0233(14) 0.0233(14) 0.0243(14) 0.0007(11) 0.0092(12) -0.0016(11) N6 0.0249(14) 0.0224(14) 0.0202(13) -0.0018(11) 0.0117(12) -0.0032(11) C1 0.0203(15) 0.0217(16) 0.0193(15) -0.0036(13) 0.0090(13) -0.0026(12) C2 0.0214(15) 0.0249(17) 0.0206(16) 0.0004(13) 0.0092(13) 0.0006(13) C3 0.0255(17) 0.0251(17) 0.0233(16) 0.0019(14) 0.0083(14) 0.0038(14) C4 0.0269(17) 0.0291(18) 0.0263(17) -0.0014(14) 0.0121(15) 0.0056(14) C5 0.0265(17) 0.0296(18) 0.0256(17) -0.0036(14) 0.0154(14) 0.0010(14) C6 0.0261(16) 0.0232(16) 0.0190(15) -0.0001(13) 0.0116(13) 0.0006(13) C7 0.040(2) 0.040(2) 0.043(2) 0.0051(18) 0.0231(19) 0.0160(18) C8 0.0299(18) 0.0205(17) 0.0324(19) 0.0022(14) 0.0125(15) 0.0003(14) C9 0.0337(19) 0.0242(17) 0.0332(19) -0.0010(15) 0.0161(16) -0.0004(15) C10 0.095(4) 0.028(2) 0.052(3) 0.000(2) 0.039(3) 0.010(2) C11 0.120(5) 0.037(3) 0.054(3) -0.009(2) 0.049(3) 0.010(3) C12 0.077(3) 0.044(3) 0.036(2) -0.0077(19) 0.030(2) -0.002(2) C13 0.045(2) 0.0287(19) 0.0293(19) -0.0001(15) 0.0172(17) -0.0026(16) C14 0.0293(18) 0.034(2) 0.0323(19) 0.0069(15) 0.0190(16) 0.0015(15) C15 0.0301(18) 0.0262(18) 0.044(2) -0.0010(16) 0.0215(17) -0.0009(15) C16 0.037(2) 0.037(2) 0.064(3) 0.008(2) 0.032(2) -0.0004(17) C17 0.035(2) 0.046(3) 0.085(4) -0.007(2) 0.035(2) -0.0090(19) C18 0.0258(19) 0.042(2) 0.062(3) -0.006(2) 0.0155(19) -0.0025(17) C19 0.0263(18) 0.033(2) 0.043(2) -0.0058(17) 0.0121(17) 0.0004(15) C20 0.0371(19) 0.0297(18) 0.0218(17) 0.0065(14) 0.0160(15) 0.0002(15) C21 0.0237(16) 0.0267(17) 0.0233(17) 0.0039(14) 0.0087(14) -0.0006(14) C22 0.039(2) 0.033(2) 0.034(2) 0.0092(16) 0.0163(17) -0.0040(16) C23 0.049(2) 0.0240(19) 0.053(3) 0.0068(18) 0.023(2) -0.0038(17) C24 0.043(2) 0.0251(19) 0.050(2) -0.0013(17) 0.022(2) -0.0010(16) C25 0.0240(17) 0.0264(18) 0.0322(19) -0.0034(15) 0.0105(15) -0.0026(14) C26 0.0244(17) 0.0321(19) 0.0238(17) 0.0020(14) 0.0131(14) -0.0011(14) C27 0.0227(16) 0.0239(17) 0.0243(17) -0.0028(13) 0.0111(14) -0.0033(13) C28 0.0257(18) 0.036(2) 0.0304(19) -0.0002(15) 0.0139(15) 0.0021(15) C29 0.0281(18) 0.034(2) 0.0264(18) 0.0004(15) 0.0050(15) 0.0008(15) C30 0.039(2) 0.0290(19) 0.0217(17) 0.0022(14) 0.0140(16) 0.0022(15) C31 0.0332(18) 0.0245(17) 0.0243(17) -0.0014(13) 0.0167(15) -0.0009(14) C32 0.0200(15) 0.0274(17) 0.0193(15) -0.0003(13) 0.0086(13) 0.0011(13) C33 0.0310(19) 0.039(2) 0.034(2) -0.0108(16) 0.0199(16) -0.0041(16) C34 0.0281(17) 0.0229(17) 0.0211(16) -0.0003(13) 0.0097(14) 0.0038(14) C35 0.038(2) 0.043(2) 0.0238(19) 0.0009(17) 0.0030(16) -0.0006(18) Cl1 0.0604(8) 0.0506(8) 0.1262(14) -0.0283(8) 0.0287(9) 0.0020(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.017(2) . ? Co1 O1 2.058(2) . ? Co1 O2 2.074(2) . ? Co1 N3 2.104(3) . ? Co1 N2 2.138(3) . ? Co1 N1 2.312(3) . ? Co2 O3 2.007(2) . ? Co2 O5 2.061(2) . ? Co2 O1 2.083(2) . ? Co2 N6 2.124(3) . ? Co2 N5 2.127(3) . ? Co2 N4 2.263(3) . ? S1 O12 1.429(3) . ? S1 O11 1.437(3) . ? S1 N1 1.696(3) . ? S1 C2 1.760(3) . ? S2 O22 1.425(3) . ? S2 O21 1.433(3) . ? S2 N4 1.701(3) . ? S2 C6 1.751(3) . ? O1 C1 1.313(4) . ? O2 C32 1.245(4) . ? O3 C32 1.257(4) . ? O4 C34 1.255(4) . ? O5 C34 1.251(4) . ? N1 C8 1.492(4) . ? N1 C14 1.499(4) . ? N2 C9 1.333(5) . ? N2 C13 1.348(5) . ? N3 C19 1.336(5) . ? N3 C15 1.342(5) . ? N4 C26 1.491(4) . ? N4 C20 1.497(4) . ? N5 C25 1.339(5) . ? N5 C21 1.341(4) . ? N6 C27 1.345(4) . ? N6 C31 1.347(4) . ? C1 C2 1.413(5) . ? C1 C6 1.422(4) . ? C2 C3 1.395(5) . ? C3 C4 1.393(5) . ? C3 H3A 0.9500 . ? C4 C5 1.384(5) . ? C4 C7 1.501(5) . ? C5 C6 1.390(5) . ? C5 H5A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.504(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.381(6) . ? C10 C11 1.370(7) . ? C10 H10A 0.9500 . ? C11 C12 1.376(7) . ? C11 H11A 0.9500 . ? C12 C13 1.373(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.505(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.384(5) . ? C16 C17 1.387(6) . ? C16 H16A 0.9500 . ? C17 C18 1.378(7) . ? C17 H17A 0.9500 . ? C18 C19 1.371(6) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.504(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.387(5) . ? C22 C23 1.383(6) . ? C22 H22A 0.9500 . ? C23 C24 1.380(6) . ? C23 H23A 0.9500 . ? C24 C25 1.379(5) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.499(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.384(5) . ? C28 C29 1.385(5) . ? C28 H28A 0.9500 . ? C29 C30 1.382(5) . ? C29 H29A 0.9500 . ? C30 C31 1.375(5) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.512(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.505(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? Cl1 O1H 1.349(9) . ? Cl1 O1A 1.381(7) . ? Cl1 O1B 1.395(6) . ? Cl1 O1E 1.422(8) . ? Cl1 O1G 1.433(9) . ? Cl1 O1C 1.436(6) . ? Cl1 O1D 1.503(5) . ? Cl1 O1F 1.543(10) . ? O1W H1W 0.840 . ? O1W H2W 0.840 . ? O2W H3W 0.840 . ? O2W H4W 0.840 . ? O1S C1S 1.385(16) . ? O1S H1S 0.840 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 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 O4 Co1 O1 98.27(9) . . ? O4 Co1 O2 93.78(10) . . ? O1 Co1 O2 92.74(9) . . ? O4 Co1 N3 95.59(11) . . ? O1 Co1 N3 165.99(10) . . ? O2 Co1 N3 84.29(10) . . ? O4 Co1 N2 91.71(11) . . ? O1 Co1 N2 91.00(10) . . ? O2 Co1 N2 172.85(10) . . ? N3 Co1 N2 90.62(11) . . ? O4 Co1 N1 165.00(10) . . ? O1 Co1 N1 91.05(9) . . ? O2 Co1 N1 97.51(10) . . ? N3 Co1 N1 75.82(10) . . ? N2 Co1 N1 76.32(10) . . ? O3 Co2 O5 94.02(10) . . ? O3 Co2 O1 98.83(9) . . ? O5 Co2 O1 92.22(9) . . ? O3 Co2 N6 95.96(10) . . ? O5 Co2 N6 169.85(10) . . ? O1 Co2 N6 88.10(9) . . ? O3 Co2 N5 94.60(10) . . ? O5 Co2 N5 81.85(10) . . ? O1 Co2 N5 165.68(10) . . ? N6 Co2 N5 95.46(10) . . ? O3 Co2 N4 167.79(10) . . ? O5 Co2 N4 91.86(10) . . ? O1 Co2 N4 91.62(9) . . ? N6 Co2 N4 77.98(10) . . ? N5 Co2 N4 75.64(10) . . ? O12 S1 O11 118.06(16) . . ? O12 S1 N1 106.37(14) . . ? O11 S1 N1 109.53(15) . . ? O12 S1 C2 111.34(15) . . ? O11 S1 C2 108.08(15) . . ? N1 S1 C2 102.30(14) . . ? O22 S2 O21 118.60(16) . . ? O22 S2 N4 106.42(14) . . ? O21 S2 N4 108.78(15) . . ? O22 S2 C6 110.67(15) . . ? O21 S2 C6 107.86(16) . . ? N4 S2 C6 103.45(14) . . ? C1 O1 Co1 123.50(19) . . ? C1 O1 Co2 124.08(19) . . ? Co1 O1 Co2 112.36(10) . . ? C32 O2 Co1 135.3(2) . . ? C32 O3 Co2 131.1(2) . . ? C34 O4 Co1 131.1(2) . . ? C34 O5 Co2 136.2(2) . . ? C8 N1 C14 112.3(3) . . ? C8 N1 S1 111.6(2) . . ? C14 N1 S1 111.4(2) . . ? C8 N1 Co1 109.8(2) . . ? C14 N1 Co1 100.65(19) . . ? S1 N1 Co1 110.65(14) . . ? C9 N2 C13 118.2(3) . . ? C9 N2 Co1 119.7(2) . . ? C13 N2 Co1 122.0(2) . . ? C19 N3 C15 118.8(3) . . ? C19 N3 Co1 124.6(3) . . ? C15 N3 Co1 116.5(2) . . ? C26 N4 C20 111.6(3) . . ? C26 N4 S2 112.3(2) . . ? C20 N4 S2 109.6(2) . . ? C26 N4 Co2 107.99(19) . . ? C20 N4 Co2 103.9(2) . . ? S2 N4 Co2 111.14(13) . . ? C25 N5 C21 118.8(3) . . ? C25 N5 Co2 125.0(2) . . ? C21 N5 Co2 115.9(2) . . ? C27 N6 C31 118.1(3) . . ? C27 N6 Co2 117.4(2) . . ? C31 N6 Co2 123.8(2) . . ? O1 C1 C2 122.9(3) . . ? O1 C1 C6 122.4(3) . . ? C2 C1 C6 114.7(3) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 S1 116.8(3) . . ? C1 C2 S1 120.7(2) . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C7 121.0(3) . . ? C3 C4 C7 121.9(3) . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 122.1(3) . . ? C5 C6 S2 117.1(2) . . ? C1 C6 S2 120.5(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 113.7(3) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C10 122.0(4) . . ? N2 C9 C8 118.2(3) . . ? C10 C9 C8 119.9(3) . . ? C11 C10 C9 119.3(4) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C10 C11 C12 119.3(4) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C13 C12 C11 118.5(4) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? N2 C13 C12 122.7(4) . . ? N2 C13 H13A 118.7 . . ? C12 C13 H13A 118.7 . . ? N1 C14 C15 108.1(3) . . ? N1 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? N1 C14 H14B 110.1 . . ? C15 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N3 C15 C16 121.7(4) . . ? N3 C15 C14 115.5(3) . . ? C16 C15 C14 122.8(4) . . ? C15 C16 C17 118.7(4) . . ? C15 C16 H16A 120.7 . . ? C17 C16 H16A 120.7 . . ? C18 C17 C16 119.5(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C19 C18 C17 118.3(4) . . ? C19 C18 H18A 120.9 . . ? C17 C18 H18A 120.9 . . ? N3 C19 C18 123.1(4) . . ? N3 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? N4 C20 C21 109.2(3) . . ? N4 C20 H20A 109.8 . . ? C21 C20 H20A 109.8 . . ? N4 C20 H20B 109.8 . . ? C21 C20 H20B 109.8 . . ? H20A C20 H20B 108.3 . . ? N5 C21 C22 121.8(3) . . ? N5 C21 C20 116.6(3) . . ? C22 C21 C20 121.5(3) . . ? C23 C22 C21 118.9(4) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C24 C23 C22 119.2(4) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C23 118.8(4) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? N5 C25 C24 122.5(4) . . ? N5 C25 H25A 118.8 . . ? C24 C25 H25A 118.8 . . ? N4 C26 C27 112.9(3) . . ? N4 C26 H26A 109.0 . . ? C27 C26 H26A 109.0 . . ? N4 C26 H26B 109.0 . . ? C27 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N6 C27 C28 122.2(3) . . ? N6 C27 C26 116.6(3) . . ? C28 C27 C26 121.1(3) . . ? C27 C28 C29 118.9(3) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C30 C29 C28 119.2(3) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C31 C30 C29 118.7(3) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? N6 C31 C30 122.9(3) . . ? N6 C31 H31A 118.5 . . ? C30 C31 H31A 118.5 . . ? O2 C32 O3 126.2(3) . . ? O2 C32 C33 117.7(3) . . ? O3 C32 C33 116.1(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O5 C34 O4 126.3(3) . . ? O5 C34 C35 117.5(3) . . ? O4 C34 C35 116.2(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O1A Cl1 O1B 118.7(5) . . ? O1A Cl1 O1C 112.5(4) . . ? O1B Cl1 O1C 111.4(4) . . ? O1A Cl1 O1D 101.4(4) . . ? O1B Cl1 O1D 107.2(4) . . ? O1C Cl1 O1D 103.8(4) . . ? O1H Cl1 O1E 125.2(9) . . ? O1H Cl1 O1G 125.4(10) . . ? O1E Cl1 O1G 109.1(8) . . ? O1H Cl1 O1F 95.3(9) . . ? O1E Cl1 O1F 88.5(8) . . ? O1G Cl1 O1F 90.9(9) . . ? H1W O1W H2W 116.5 . . ? H3W O2W H4W 129.1 . . ? C1S O1S H1S 93.6 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 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 O4 Co1 O1 C1 -130.3(2) . . . . ? O2 Co1 O1 C1 135.5(2) . . . . ? N3 Co1 O1 C1 58.1(5) . . . . ? N2 Co1 O1 C1 -38.5(2) . . . . ? N1 Co1 O1 C1 37.9(2) . . . . ? O4 Co1 O1 Co2 46.97(12) . . . . ? O2 Co1 O1 Co2 -47.26(12) . . . . ? N3 Co1 O1 Co2 -124.6(4) . . . . ? N2 Co1 O1 Co2 138.84(12) . . . . ? N1 Co1 O1 Co2 -144.82(11) . . . . ? O3 Co2 O1 C1 -136.9(2) . . . . ? O5 Co2 O1 C1 128.6(2) . . . . ? N6 Co2 O1 C1 -41.2(2) . . . . ? N5 Co2 O1 C1 63.6(5) . . . . ? N4 Co2 O1 C1 36.7(2) . . . . ? O3 Co2 O1 Co1 45.80(12) . . . . ? O5 Co2 O1 Co1 -48.62(12) . . . . ? N6 Co2 O1 Co1 141.54(12) . . . . ? N5 Co2 O1 Co1 -113.7(4) . . . . ? N4 Co2 O1 Co1 -140.55(11) . . . . ? O4 Co1 O2 C32 -59.1(3) . . . . ? O1 Co1 O2 C32 39.4(3) . . . . ? N3 Co1 O2 C32 -154.4(3) . . . . ? N1 Co1 O2 C32 130.8(3) . . . . ? O5 Co2 O3 C32 67.4(3) . . . . ? O1 Co2 O3 C32 -25.4(3) . . . . ? N6 Co2 O3 C32 -114.4(3) . . . . ? N5 Co2 O3 C32 149.6(3) . . . . ? N4 Co2 O3 C32 -174.0(4) . . . . ? O1 Co1 O4 C34 -15.6(3) . . . . ? O2 Co1 O4 C34 77.8(3) . . . . ? N3 Co1 O4 C34 162.4(3) . . . . ? N2 Co1 O4 C34 -106.8(3) . . . . ? N1 Co1 O4 C34 -143.4(4) . . . . ? O3 Co2 O5 C34 -71.2(3) . . . . ? O1 Co2 O5 C34 27.9(3) . . . . ? N6 Co2 O5 C34 119.5(6) . . . . ? N5 Co2 O5 C34 -165.2(3) . . . . ? N4 Co2 O5 C34 119.6(3) . . . . ? O12 S1 N1 C8 -179.5(2) . . . . ? O11 S1 N1 C8 -50.9(3) . . . . ? C2 S1 N1 C8 63.6(2) . . . . ? O12 S1 N1 C14 -53.2(3) . . . . ? O11 S1 N1 C14 75.5(3) . . . . ? C2 S1 N1 C14 -170.0(2) . . . . ? O12 S1 N1 Co1 57.95(17) . . . . ? O11 S1 N1 Co1 -173.41(14) . . . . ? C2 S1 N1 Co1 -58.93(17) . . . . ? O4 Co1 N1 C8 25.6(5) . . . . ? O1 Co1 N1 C8 -103.1(2) . . . . ? O2 Co1 N1 C8 164.0(2) . . . . ? N3 Co1 N1 C8 81.9(2) . . . . ? N2 Co1 N1 C8 -12.3(2) . . . . ? O4 Co1 N1 C14 -92.9(4) . . . . ? O1 Co1 N1 C14 138.4(2) . . . . ? O2 Co1 N1 C14 45.6(2) . . . . ? N3 Co1 N1 C14 -36.6(2) . . . . ? N2 Co1 N1 C14 -130.8(2) . . . . ? O4 Co1 N1 S1 149.2(3) . . . . ? O1 Co1 N1 S1 20.52(14) . . . . ? O2 Co1 N1 S1 -72.38(15) . . . . ? N3 Co1 N1 S1 -154.52(17) . . . . ? N2 Co1 N1 S1 111.30(16) . . . . ? O4 Co1 N2 C9 -164.5(3) . . . . ? O1 Co1 N2 C9 97.2(3) . . . . ? N3 Co1 N2 C9 -68.9(3) . . . . ? N1 Co1 N2 C9 6.4(3) . . . . ? O4 Co1 N2 C13 13.7(3) . . . . ? O1 Co1 N2 C13 -84.7(3) . . . . ? N3 Co1 N2 C13 109.3(3) . . . . ? N1 Co1 N2 C13 -175.5(3) . . . . ? O4 Co1 N3 C19 10.1(3) . . . . ? O1 Co1 N3 C19 -178.3(3) . . . . ? O2 Co1 N3 C19 103.4(3) . . . . ? N2 Co1 N3 C19 -81.7(3) . . . . ? N1 Co1 N3 C19 -157.4(3) . . . . ? O4 Co1 N3 C15 -174.2(3) . . . . ? O1 Co1 N3 C15 -2.6(6) . . . . ? O2 Co1 N3 C15 -81.0(3) . . . . ? N2 Co1 N3 C15 94.0(3) . . . . ? N1 Co1 N3 C15 18.3(2) . . . . ? O22 S2 N4 C26 179.1(2) . . . . ? O21 S2 N4 C26 -52.0(3) . . . . ? C6 S2 N4 C26 62.4(2) . . . . ? O22 S2 N4 C20 -56.2(2) . . . . ? O21 S2 N4 C20 72.6(3) . . . . ? C6 S2 N4 C20 -172.9(2) . . . . ? O22 S2 N4 Co2 58.02(17) . . . . ? O21 S2 N4 Co2 -173.13(14) . . . . ? C6 S2 N4 Co2 -58.65(17) . . . . ? O3 Co2 N4 C26 45.5(6) . . . . ? O5 Co2 N4 C26 164.3(2) . . . . ? O1 Co2 N4 C26 -103.4(2) . . . . ? N6 Co2 N4 C26 -15.7(2) . . . . ? N5 Co2 N4 C26 83.2(2) . . . . ? O3 Co2 N4 C20 -73.1(5) . . . . ? O5 Co2 N4 C20 45.7(2) . . . . ? O1 Co2 N4 C20 137.9(2) . . . . ? N6 Co2 N4 C20 -134.3(2) . . . . ? N5 Co2 N4 C20 -35.4(2) . . . . ? O3 Co2 N4 S2 169.1(4) . . . . ? O5 Co2 N4 S2 -72.10(14) . . . . ? O1 Co2 N4 S2 20.18(14) . . . . ? N6 Co2 N4 S2 107.89(15) . . . . ? N5 Co2 N4 S2 -153.20(16) . . . . ? O3 Co2 N5 C25 8.2(3) . . . . ? O5 Co2 N5 C25 101.6(3) . . . . ? O1 Co2 N5 C25 167.9(3) . . . . ? N6 Co2 N5 C25 -88.3(3) . . . . ? N4 Co2 N5 C25 -164.4(3) . . . . ? O3 Co2 N5 C21 -165.5(2) . . . . ? O5 Co2 N5 C21 -72.0(2) . . . . ? O1 Co2 N5 C21 -5.8(5) . . . . ? N6 Co2 N5 C21 98.1(2) . . . . ? N4 Co2 N5 C21 22.0(2) . . . . ? O3 Co2 N6 C27 -168.2(2) . . . . ? O5 Co2 N6 C27 1.1(7) . . . . ? O1 Co2 N6 C27 93.1(2) . . . . ? N5 Co2 N6 C27 -73.0(2) . . . . ? N4 Co2 N6 C27 1.0(2) . . . . ? O3 Co2 N6 C31 21.9(3) . . . . ? O5 Co2 N6 C31 -168.8(5) . . . . ? O1 Co2 N6 C31 -76.8(3) . . . . ? N5 Co2 N6 C31 117.1(3) . . . . ? N4 Co2 N6 C31 -168.9(3) . . . . ? Co1 O1 C1 C2 -51.0(4) . . . . ? Co2 O1 C1 C2 132.0(3) . . . . ? Co1 O1 C1 C6 128.7(3) . . . . ? Co2 O1 C1 C6 -48.3(4) . . . . ? O1 C1 C2 C3 178.7(3) . . . . ? C6 C1 C2 C3 -1.0(5) . . . . ? O1 C1 C2 S1 -6.0(4) . . . . ? C6 C1 C2 S1 174.3(2) . . . . ? O12 S1 C2 C3 126.2(3) . . . . ? O11 S1 C2 C3 -5.0(3) . . . . ? N1 S1 C2 C3 -120.5(3) . . . . ? O12 S1 C2 C1 -49.3(3) . . . . ? O11 S1 C2 C1 179.4(3) . . . . ? N1 S1 C2 C1 63.9(3) . . . . ? C1 C2 C3 C4 3.0(5) . . . . ? S1 C2 C3 C4 -172.5(3) . . . . ? C2 C3 C4 C5 -2.4(5) . . . . ? C2 C3 C4 C7 176.4(3) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C7 C4 C5 C6 -178.7(3) . . . . ? C4 C5 C6 C1 1.8(5) . . . . ? C4 C5 C6 S2 -172.1(3) . . . . ? O1 C1 C6 C5 179.0(3) . . . . ? C2 C1 C6 C5 -1.3(5) . . . . ? O1 C1 C6 S2 -7.3(4) . . . . ? C2 C1 C6 S2 172.4(2) . . . . ? O22 S2 C6 C5 124.0(3) . . . . ? O21 S2 C6 C5 -7.3(3) . . . . ? N4 S2 C6 C5 -122.4(3) . . . . ? O22 S2 C6 C1 -50.0(3) . . . . ? O21 S2 C6 C1 178.8(3) . . . . ? N4 S2 C6 C1 63.7(3) . . . . ? C14 N1 C8 C9 127.7(3) . . . . ? S1 N1 C8 C9 -106.4(3) . . . . ? Co1 N1 C8 C9 16.7(3) . . . . ? C13 N2 C9 C10 0.8(6) . . . . ? Co1 N2 C9 C10 179.0(3) . . . . ? C13 N2 C9 C8 -177.0(3) . . . . ? Co1 N2 C9 C8 1.2(4) . . . . ? N1 C8 C9 N2 -12.8(5) . . . . ? N1 C8 C9 C10 169.3(4) . . . . ? N2 C9 C10 C11 -1.3(8) . . . . ? C8 C9 C10 C11 176.4(5) . . . . ? C9 C10 C11 C12 0.5(9) . . . . ? C10 C11 C12 C13 0.8(9) . . . . ? C9 N2 C13 C12 0.6(6) . . . . ? Co1 N2 C13 C12 -177.6(3) . . . . ? C11 C12 C13 N2 -1.4(7) . . . . ? C8 N1 C14 C15 -66.9(4) . . . . ? S1 N1 C14 C15 167.1(2) . . . . ? Co1 N1 C14 C15 49.8(3) . . . . ? C19 N3 C15 C16 1.0(5) . . . . ? Co1 N3 C15 C16 -174.9(3) . . . . ? C19 N3 C15 C14 -178.3(3) . . . . ? Co1 N3 C15 C14 5.8(4) . . . . ? N1 C14 C15 N3 -41.0(4) . . . . ? N1 C14 C15 C16 139.7(4) . . . . ? N3 C15 C16 C17 -0.8(6) . . . . ? C14 C15 C16 C17 178.5(4) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C16 C17 C18 C19 1.3(7) . . . . ? C15 N3 C19 C18 -0.1(6) . . . . ? Co1 N3 C19 C18 175.4(3) . . . . ? C17 C18 C19 N3 -1.0(6) . . . . ? C26 N4 C20 C21 -71.7(3) . . . . ? S2 N4 C20 C21 163.3(2) . . . . ? Co2 N4 C20 C21 44.4(3) . . . . ? C25 N5 C21 C22 1.1(5) . . . . ? Co2 N5 C21 C22 175.1(3) . . . . ? C25 N5 C21 C20 -176.6(3) . . . . ? Co2 N5 C21 C20 -2.6(4) . . . . ? N4 C20 C21 N5 -30.5(4) . . . . ? N4 C20 C21 C22 151.8(3) . . . . ? N5 C21 C22 C23 -0.6(6) . . . . ? C20 C21 C22 C23 177.0(4) . . . . ? C21 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C25 0.6(6) . . . . ? C21 N5 C25 C24 -0.8(5) . . . . ? Co2 N5 C25 C24 -174.2(3) . . . . ? C23 C24 C25 N5 -0.1(6) . . . . ? C20 N4 C26 C27 141.1(3) . . . . ? S2 N4 C26 C27 -95.4(3) . . . . ? Co2 N4 C26 C27 27.5(3) . . . . ? C31 N6 C27 C28 1.9(5) . . . . ? Co2 N6 C27 C28 -168.7(3) . . . . ? C31 N6 C27 C26 -174.8(3) . . . . ? Co2 N6 C27 C26 14.7(4) . . . . ? N4 C26 C27 N6 -29.2(4) . . . . ? N4 C26 C27 C28 154.1(3) . . . . ? N6 C27 C28 C29 -2.3(5) . . . . ? C26 C27 C28 C29 174.2(3) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C28 C29 C30 C31 1.1(5) . . . . ? C27 N6 C31 C30 0.1(5) . . . . ? Co2 N6 C31 C30 169.9(3) . . . . ? C29 C30 C31 N6 -1.5(5) . . . . ? Co1 O2 C32 O3 -20.2(6) . . . . ? Co1 O2 C32 C33 160.5(3) . . . . ? Co2 O3 C32 O2 10.9(5) . . . . ? Co2 O3 C32 C33 -169.8(2) . . . . ? Co2 O5 C34 O4 4.4(6) . . . . ? Co2 O5 C34 C35 -175.7(3) . . . . ? Co1 O4 C34 O5 -12.4(5) . . . . ? Co1 O4 C34 C35 167.7(3) . . . . ? ## NOTE: H atoms are place along O...O vectors then allowed to ## ride on parent O atoms ## It is no coincidence that all of the O-H...O angles are 180 deg.! ## BEWARE: unfeasibly short O2W...O1F separation ## O atom positions in disordered perchlorate anion are approximate 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 O1S H1S O2W 0.84 2.27 3.114(14) 179.3 6_565 O1W H2W O2W 0.84 1.85 2.694(15) 178.7 2 O1W H1W O1C 0.84 2.17 3.007(12) 179.8 . O2W H4W O1F 0.84 1.38 2.223(15) 178.7 . O2W H3W O1W 0.84 2.04 2.880(14) 179.9 6_556