Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Gianfranco Ciani' 'Lucia Carlucci' 'Davide Proserpio' 'Laura Spadacini' _publ_contact_author_name 'Prof Gianfranco Ciani' _publ_contact_author_address ; DCSSI University of Milano Venezian 21 Milano 20133 ITALY ; _publ_contact_author_email GIANFRANCO.CIANI@UNIMI.IT _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Supramolecular isomers in the same crystal: a new case involving two different types of layers polycatenated in the 3D architecture of [Cu(bix)2(SO4)].7.5H2O [bix = 1,4-bis(imidazol-1-ylmethyl)benzene] ; data_1 _database_code_depnum_ccdc_archive 'CCDC 232405' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C14 H22 Cu N4 O8 S' _chemical_formula_weight 469.96 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' 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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.960(5) _cell_length_b 10.122(5) _cell_length_c 12.782(5) _cell_angle_alpha 67.234(5) _cell_angle_beta 84.407(5) _cell_angle_gamma 80.782(5) _cell_volume 936.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description colum _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 1.329 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 9880 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.05 _reflns_number_total 4511 _reflns_number_observed 3930 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.0524P)^2^+0.3186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4511 _refine_ls_number_parameters 253 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_obs 0.0314 _refine_ls_wR_factor_all 0.0915 _refine_ls_wR_factor_obs 0.0884 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.67684(3) 0.34365(3) 0.83929(2) 0.02898(9) Uani 1 1 d . . . S S 0.26293(6) 0.53134(5) 0.84156(4) 0.02650(11) Uani 1 1 d . . . O1W O 0.58767(19) 0.29369(16) 0.99768(12) 0.0332(3) Uani 1 1 d D . . H11W H 0.4812 0.3314 0.9901 0.040 Uiso 1 1 d RD . . H12W H 0.6392 0.3003 1.0496 0.040 Uiso 1 1 d RD . . O2W O 0.7994(2) 0.49027(19) 0.85507(14) 0.0419(4) Uani 1 1 d D . . H21W H 0.7828 0.5074 0.9184 0.050 Uiso 1 1 d RD . . H22W H 0.9111 0.4851 0.8355 0.050 Uiso 1 1 d RD . . N12 N 0.5364(2) -0.00363(19) 0.79066(15) 0.0330(4) Uani 1 1 d . . . O3 O 0.2364(2) 0.67758(17) 0.84522(14) 0.0372(3) Uani 1 1 d . . . N21 N 0.7762(2) 0.38390(19) 0.68299(15) 0.0311(4) Uani 1 1 d . . . O1 O 0.42559(18) 0.50938(17) 0.78254(13) 0.0357(3) Uani 1 1 d . . . O2 O 0.26684(19) 0.42414(17) 0.96192(12) 0.0345(3) Uani 1 1 d . . . O4 O 0.12254(19) 0.51292(19) 0.78445(14) 0.0407(4) Uani 1 1 d . . . C25 C 1.0368(3) 0.1327(2) 0.49397(19) 0.0330(4) Uani 1 1 d . . . N11 N 0.5676(2) 0.1837(2) 0.82995(16) 0.0341(4) Uani 1 1 d . . . N22 N 0.9337(2) 0.34306(19) 0.54503(16) 0.0333(4) Uani 1 1 d . . . C21 C 0.9270(3) 0.3280(2) 0.65412(19) 0.0331(4) Uani 1 1 d . . . H21 H 1.0164 0.2841 0.7031 0.040 Uiso 1 1 calc R . . C15 C 0.5342(3) -0.0516(2) 0.61544(18) 0.0303(4) Uani 1 1 d . . . C17 C 0.5421(3) 0.0925(2) 0.54618(19) 0.0369(5) Uani 1 1 d . . . H17 H 0.5704 0.1553 0.5769 0.044 Uiso 1 1 calc R . . C26 C 1.0577(3) 0.0115(2) 0.5936(2) 0.0394(5) Uani 1 1 d . . . H26 H 1.0969 0.0190 0.6570 0.047 Uiso 1 1 calc R . . C23 C 0.7789(3) 0.4125(2) 0.5007(2) 0.0379(5) Uani 1 1 d . . . H23 H 0.7461 0.4375 0.4269 0.045 Uiso 1 1 calc R . . C13 C 0.3792(3) 0.0452(3) 0.8250(2) 0.0417(5) Uani 1 1 d . . . H13 H 0.2785 0.0069 0.8305 0.050 Uiso 1 1 calc R . . C14 C 0.5758(3) -0.1126(2) 0.73950(19) 0.0366(5) Uani 1 1 d . . . H14 H 0.5112 -0.1923 0.7803 0.044 Uiso 1 1 calc R . . H15 H 0.6959 -0.1503 0.7469 0.044 Uiso 1 1 calc R . . C16 C 0.4916(3) -0.1435(2) 0.56793(19) 0.0351(5) Uani 1 1 d . . . H16 H 0.4857 -0.2402 0.6132 0.042 Uiso 1 1 calc R . . C24 C 1.0732(3) 0.2771(3) 0.4886(2) 0.0430(6) Uani 1 1 d . . . H24 H 1.1790 0.2642 0.5253 0.052 Uiso 1 1 calc R . . H25 H 1.0866 0.3412 0.4099 0.052 Uiso 1 1 calc R . . C22 C 0.6835(3) 0.4373(2) 0.58707(19) 0.0359(5) Uani 1 1 d . . . H22 H 0.5721 0.4836 0.5818 0.043 Uiso 1 1 calc R . . C12 C 0.3992(3) 0.1609(3) 0.8496(2) 0.0436(5) Uani 1 1 d . . . H12 H 0.3131 0.2159 0.8755 0.052 Uiso 1 1 calc R . . C27 C 0.9790(3) 0.1205(2) 0.40007(19) 0.0387(5) Uani 1 1 d . . . H27 H 0.9647 0.2010 0.3327 0.046 Uiso 1 1 calc R . . C11 C 0.6449(3) 0.0821(2) 0.79447(19) 0.0353(5) Uani 1 1 d . . . H11 H 0.7604 0.0716 0.7746 0.042 Uiso 1 1 calc R . . O4W O 0.9359(2) 0.8024(2) 0.92121(19) 0.0598(5) Uani 1 1 d D . . H41W H 1.0276 0.7650 0.8923 0.072 Uiso 1 1 d RD . . H42W H 0.8726 0.7329 0.9631 0.072 Uiso 1 1 d RD . . O3W O 0.9363(3) 0.1457(3) 0.9098(2) 0.0828(7) Uani 1 1 d D . . H31W H 0.9988 0.1672 0.9605 0.099 Uiso 1 1 d RD . . H32W H 1.0087 0.1437 0.8457 0.099 Uiso 1 1 d RD . . 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 Cu 0.02949(14) 0.03565(15) 0.02761(14) -0.01725(11) 0.00385(9) -0.00998(10) S 0.0213(2) 0.0349(2) 0.0257(2) -0.01457(19) 0.00210(17) -0.00424(17) O1W 0.0332(7) 0.0412(8) 0.0273(7) -0.0144(6) -0.0014(6) -0.0065(6) O2W 0.0353(8) 0.0624(10) 0.0452(9) -0.0364(8) 0.0133(7) -0.0225(7) N12 0.0392(9) 0.0320(9) 0.0326(9) -0.0170(7) 0.0037(7) -0.0092(7) O3 0.0399(8) 0.0359(8) 0.0388(8) -0.0184(7) -0.0061(7) -0.0001(6) N21 0.0314(8) 0.0346(9) 0.0321(9) -0.0179(7) 0.0043(7) -0.0071(7) O1 0.0261(7) 0.0430(8) 0.0312(8) -0.0101(6) 0.0070(6) -0.0006(6) O2 0.0350(8) 0.0399(8) 0.0271(7) -0.0123(6) 0.0068(6) -0.0063(6) O4 0.0291(7) 0.0631(11) 0.0407(9) -0.0289(8) 0.0001(6) -0.0129(7) C25 0.0318(10) 0.0321(10) 0.0382(11) -0.0192(9) 0.0098(8) -0.0042(8) N11 0.0369(9) 0.0358(9) 0.0360(9) -0.0200(8) 0.0050(7) -0.0098(7) N22 0.0365(9) 0.0307(8) 0.0381(10) -0.0196(7) 0.0118(7) -0.0106(7) C21 0.0320(10) 0.0338(10) 0.0355(11) -0.0154(9) 0.0032(8) -0.0066(8) C15 0.0324(10) 0.0293(9) 0.0330(10) -0.0160(8) 0.0083(8) -0.0092(8) C17 0.0516(13) 0.0291(10) 0.0370(11) -0.0178(9) 0.0035(10) -0.0143(9) C26 0.0464(13) 0.0403(12) 0.0357(11) -0.0199(10) -0.0026(10) -0.0022(10) C23 0.0441(12) 0.0399(11) 0.0334(11) -0.0186(9) 0.0030(9) -0.0067(9) C13 0.0366(11) 0.0464(13) 0.0506(14) -0.0262(11) 0.0097(10) -0.0163(10) C14 0.0496(13) 0.0285(10) 0.0358(11) -0.0170(9) 0.0033(9) -0.0075(9) C16 0.0470(12) 0.0255(9) 0.0358(11) -0.0132(8) 0.0055(9) -0.0133(9) C24 0.0412(12) 0.0401(12) 0.0552(15) -0.0284(11) 0.0223(11) -0.0145(10) C22 0.0340(11) 0.0408(11) 0.0365(11) -0.0196(9) 0.0005(9) -0.0031(9) C12 0.0385(12) 0.0456(13) 0.0562(15) -0.0303(11) 0.0150(10) -0.0133(10) C27 0.0482(13) 0.0329(10) 0.0308(11) -0.0108(9) 0.0014(9) 0.0013(9) C11 0.0331(10) 0.0385(11) 0.0412(12) -0.0226(10) 0.0031(9) -0.0073(8) O4W 0.0453(10) 0.0568(12) 0.0705(14) -0.0208(10) 0.0063(9) -0.0007(9) O3W 0.0769(17) 0.0934(18) 0.0792(17) -0.0307(15) -0.0148(14) -0.0126(14) _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 Cu O1W 1.9750(16) . ? Cu O2W 1.9821(17) . ? Cu N21 1.9870(19) . ? Cu N11 2.0029(19) . ? Cu O1 2.3678(18) . ? Cu O3W 2.594(3) . ? S O1 1.4636(16) . ? S O4 1.4655(16) . ? S O3 1.4796(17) . ? S O2 1.5006(16) . ? O1W H11W 0.8703 . ? O1W H12W 0.8420 . ? O2W H21W 0.8853 . ? O2W H22W 0.8988 . ? N12 C11 1.335(3) . ? N12 C13 1.366(3) . ? N12 C14 1.467(3) . ? N21 C21 1.325(3) . ? N21 C22 1.370(3) . ? C25 C27 1.381(3) . ? C25 C26 1.386(3) . ? C25 C24 1.510(3) . ? N11 C11 1.321(3) . ? N11 C12 1.379(3) . ? N22 C21 1.339(3) . ? N22 C23 1.372(3) . ? N22 C24 1.476(3) . ? C21 H21 0.9300 . ? C15 C16 1.388(3) . ? C15 C17 1.391(3) . ? C15 C14 1.511(3) . ? C17 C16 1.384(3) 2_656 ? C17 H17 0.9300 . ? C26 C27 1.383(3) 2_756 ? C26 H26 0.9300 . ? C23 C22 1.359(3) . ? C23 H23 0.9300 . ? C13 C12 1.360(3) . ? C13 H13 0.9300 . ? C14 H14 0.9700 . ? C14 H15 0.9700 . ? C16 C17 1.384(3) 2_656 ? C16 H16 0.9300 . ? C24 H24 0.9700 . ? C24 H25 0.9700 . ? C22 H22 0.9300 . ? C12 H12 0.9300 . ? C27 C26 1.383(3) 2_756 ? C27 H27 0.9300 . ? C11 H11 0.9300 . ? O4W H41W 0.8834 . ? O4W H42W 0.8966 . ? O3W H31W 0.9600 . ? O3W H32W 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cu O2W 89.72(7) . . ? O1W Cu N21 176.75(7) . . ? O2W Cu N21 90.94(7) . . ? O1W Cu N11 89.41(7) . . ? O2W Cu N11 175.52(8) . . ? N21 Cu N11 89.68(7) . . ? O1W Cu O1 87.72(6) . . ? O2W Cu O1 92.63(8) . . ? N21 Cu O1 95.43(7) . . ? N11 Cu O1 91.73(8) . . ? O1W Cu O3W 89.65(8) . . ? O2W Cu O3W 91.24(9) . . ? N21 Cu O3W 87.15(9) . . ? N11 Cu O3W 84.35(9) . . ? O1 Cu O3W 175.31(7) . . ? O1 S O4 110.36(10) . . ? O1 S O3 109.94(10) . . ? O4 S O3 110.07(10) . . ? O1 S O2 109.38(9) . . ? O4 S O2 109.56(10) . . ? O3 S O2 107.47(9) . . ? Cu O1W H11W 103.3 . . ? Cu O1W H12W 124.2 . . ? H11W O1W H12W 117.1 . . ? Cu O2W H21W 118.6 . . ? Cu O2W H22W 116.2 . . ? H21W O2W H22W 109.3 . . ? C11 N12 C13 107.49(18) . . ? C11 N12 C14 124.98(19) . . ? C13 N12 C14 126.71(18) . . ? C21 N21 C22 105.80(18) . . ? C21 N21 Cu 126.88(15) . . ? C22 N21 Cu 124.58(15) . . ? S O1 Cu 133.10(9) . . ? C27 C25 C26 119.2(2) . . ? C27 C25 C24 120.2(2) . . ? C26 C25 C24 120.5(2) . . ? C11 N11 C12 105.53(18) . . ? C11 N11 Cu 125.34(16) . . ? C12 N11 Cu 128.96(15) . . ? C21 N22 C23 107.71(18) . . ? C21 N22 C24 125.5(2) . . ? C23 N22 C24 126.2(2) . . ? N21 C21 N22 111.0(2) . . ? N21 C21 H21 124.5 . . ? N22 C21 H21 124.5 . . ? C16 C15 C17 118.7(2) . . ? C16 C15 C14 118.90(18) . . ? C17 C15 C14 122.35(18) . . ? C16 C17 C15 120.74(19) 2_656 . ? C16 C17 H17 119.6 2_656 . ? C15 C17 H17 119.6 . . ? C27 C26 C25 120.9(2) 2_756 . ? C27 C26 H26 119.6 2_756 . ? C25 C26 H26 119.6 . . ? C22 C23 N22 105.8(2) . . ? C22 C23 H23 127.1 . . ? N22 C23 H23 127.1 . . ? C12 C13 N12 106.3(2) . . ? C12 C13 H13 126.8 . . ? N12 C13 H13 126.8 . . ? N12 C14 C15 112.13(18) . . ? N12 C14 H14 109.2 . . ? C15 C14 H14 109.2 . . ? N12 C14 H15 109.2 . . ? C15 C14 H15 109.2 . . ? H14 C14 H15 107.9 . . ? C17 C16 C15 120.54(19) 2_656 . ? C17 C16 H16 119.7 2_656 . ? C15 C16 H16 119.7 . . ? N22 C24 C25 110.84(17) . . ? N22 C24 H24 109.5 . . ? C25 C24 H24 109.5 . . ? N22 C24 H25 109.5 . . ? C25 C24 H25 109.5 . . ? H24 C24 H25 108.1 . . ? C23 C22 N21 109.7(2) . . ? C23 C22 H22 125.1 . . ? N21 C22 H22 125.1 . . ? C13 C12 N11 109.1(2) . . ? C13 C12 H12 125.5 . . ? N11 C12 H12 125.5 . . ? C25 C27 C26 119.9(2) . 2_756 ? C25 C27 H27 120.1 . . ? C26 C27 H27 120.1 2_756 . ? N11 C11 N12 111.5(2) . . ? N11 C11 H11 124.2 . . ? N12 C11 H11 124.2 . . ? H41W O4W H42W 110.2 . . ? Cu O3W H31W 109.6 . . ? Cu O3W H32W 109.1 . . ? H31W O3W H32W 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.496 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.070 data_2 _database_code_depnum_ccdc_archive 'CCDC 232406' _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 43 _chemical_formula_sum 'C28 H43 Cu N8 O11.50 S' _chemical_formula_weight 771.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 C2/c _symmetry_Int_Tables_number 15 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 23.548(11) _cell_length_b 18.524(8) _cell_length_c 16.469(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.008(17) _cell_angle_gamma 90.00 _cell_volume 7027(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 726 _cell_measurement_theta_min 3 _cell_measurement_theta_max 16 _exptl_crystal_description block _exptl_crystal_colour darkblue _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 24638 _diffrn_reflns_av_R_equivalents 0.1433 _diffrn_reflns_av_sigmaI/netI 0.1385 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5061 _reflns_number_observed 2481 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.1435P)^2^+49.0031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5061 _refine_ls_number_parameters 440 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_obs 0.0884 _refine_ls_wR_factor_all 0.2967 _refine_ls_wR_factor_obs 0.2300 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 0.23705(9) 0.2500 0.0487(7) Uani 1 2 d S . . N11 N 0.0486(3) 0.3148(4) 0.2167(6) 0.039(2) Uani 1 1 d . . . N12 N 0.0989(4) 0.4157(5) 0.2201(6) 0.044(2) Uani 1 1 d . . . N13 N 0.4493(3) 0.6584(4) 0.2802(6) 0.041(2) Uani 1 1 d . . . N14 N 0.3989(4) 0.5579(5) 0.2640(6) 0.050(2) Uani 1 1 d . . . C11 C 0.0737(4) 0.3684(6) 0.2626(7) 0.039(3) Uani 1 1 d . . . H11 H 0.0740 0.3729 0.3190 0.03(3) Uiso 1 1 d R . . C12 C 0.0894(6) 0.3910(7) 0.1404(8) 0.070(4) Uani 1 1 d . . . H12 H 0.1016 0.4122 0.0958 0.02(2) Uiso 1 1 d R . . C13 C 0.0592(5) 0.3293(7) 0.1404(8) 0.059(3) Uani 1 1 d . . . H13 H 0.0469 0.3002 0.0941 0.04(3) Uiso 1 1 d R . . C14 C 0.4224(4) 0.6109(6) 0.2258(8) 0.047(3) Uani 1 1 d . . . H14 H 0.4203 0.6135 0.1688 0.04(3) Uiso 1 1 d R . . C15 C 0.4124(5) 0.5718(7) 0.3472(8) 0.060(3) Uani 1 1 d . . . H15 H 0.4023 0.5443 0.3893 0.06(4) Uiso 1 1 d R . . C16 C 0.4428(5) 0.6337(6) 0.3551(7) 0.049(3) Uani 1 1 d . . . H16 H 0.4578 0.6564 0.4053 0.05(3) Uiso 1 1 d R . . C17 C 0.1285(5) 0.4832(6) 0.2509(9) 0.057(3) Uani 1 1 d . . . H17A H 0.1269 0.4890 0.3089 0.08(4) Uiso 1 1 d R . . H17B H 0.1081 0.5237 0.2206 0.08(4) Uiso 1 1 d R . . C18 C 0.3684(5) 0.4943(7) 0.2249(10) 0.067(4) Uani 1 1 d . . . H18A H 0.3699 0.4938 0.1665 0.13(7) Uiso 1 1 d R . . H18B H 0.3880 0.4513 0.2503 0.03(3) Uiso 1 1 d R . . C19 C 0.1904(5) 0.4848(6) 0.2428(6) 0.042(3) Uani 1 1 d . . . C110 C 0.2116(5) 0.5433(6) 0.2049(7) 0.046(3) Uani 1 1 d . . . H110 H 0.1868 0.5810 0.1837 0.03(3) Uiso 1 1 d R . . C111 C 0.2285(5) 0.4300(6) 0.2760(7) 0.050(3) Uani 1 1 d . . . H111 H 0.2152 0.3902 0.3012 0.06(3) Uiso 1 1 d R . . C112 C 0.3059(5) 0.4925(6) 0.2325(7) 0.051(3) Uani 1 1 d . . . C113 C 0.2674(5) 0.5461(6) 0.1990(7) 0.051(3) Uani 1 1 d . . . H113 H 0.2807 0.5846 0.1719 0.08(4) Uiso 1 1 d R . . C114 C 0.2844(5) 0.4344(6) 0.2710(8) 0.051(3) Uani 1 1 d . . . H114 H 0.3096 0.3976 0.2938 0.07(4) Uiso 1 1 d R . . Cu2 Cu 0.2500 0.7500 0.0000 0.0382(6) Uani 1 2 d S . . N21 N 0.2351(4) 0.6430(4) -0.0072(5) 0.042(2) Uani 1 1 d . . . N22 N 0.2445(4) 0.5267(4) -0.0265(5) 0.048(3) Uani 1 1 d . . . N23 N 0.2347(3) 0.2452(4) 0.3775(4) 0.0291(18) Uani 1 1 d . . . N24 N 0.2457(4) 0.2315(4) 0.2492(5) 0.035(2) Uani 1 1 d . . . C21 C 0.2719(6) 0.5915(5) -0.0156(6) 0.046(3) Uani 1 1 d . . . H21 H 0.3110 0.5987 -0.0149 0.04(3) Uiso 1 1 d R . . C22 C 0.1890(6) 0.5380(6) -0.0223(8) 0.057(3) Uani 1 1 d . . . H22 H 0.1599 0.5033 -0.0270 0.02(2) Uiso 1 1 d R . . C23 C 0.1830(5) 0.6096(6) -0.0107(7) 0.052(3) Uani 1 1 d . . . H23 H 0.1490 0.6328 -0.0052 0.03(3) Uiso 1 1 d R . . C24 C 0.2734(4) 0.2386(5) 0.3303(6) 0.033(2) Uani 1 1 d . . . H24 H 0.3134 0.2391 0.3493 0.02(2) Uiso 1 1 d R . . C25 C 0.1818(5) 0.2415(5) 0.3280(6) 0.041(3) Uani 1 1 d . . . H25 H 0.1468 0.2453 0.3453 0.03(2) Uiso 1 1 d R . . C26 C 0.1872(5) 0.2312(5) 0.2469(6) 0.042(3) Uani 1 1 d . . . H26 H 0.1575 0.2254 0.2003 0.02(2) Uiso 1 1 d R . . C27 C 0.2710(7) 0.4583(6) -0.0481(8) 0.069(4) Uani 1 1 d . . . H27A H 0.3111 0.4678 -0.0507 0.04(3) Uiso 1 1 d R . . H27B H 0.2509 0.4429 -0.1029 0.04(3) Uiso 1 1 d R . . C28 C 0.2734(6) 0.2172(6) 0.1776(7) 0.052(3) Uani 1 1 d . . . H28A H 0.3136 0.2033 0.1980 0.08(5) Uiso 1 1 d R . . H28B H 0.2537 0.1772 0.1455 0.08(4) Uiso 1 1 d R . . C29 C 0.2713(6) 0.3978(5) 0.0126(7) 0.050(3) Uani 1 1 d . . . C210 C 0.2196(6) 0.3619(6) 0.0169(7) 0.052(3) Uani 1 1 d . . . H210 H 0.1845 0.3769 -0.0159 0.03(3) Uiso 1 1 d R . . C211 C 0.2210(6) 0.3033(6) 0.0726(7) 0.050(3) Uani 1 1 d . . . H211 H 0.1868 0.2789 0.0740 0.06(4) Uiso 1 1 d R . . C212 C 0.2715(5) 0.2822(6) 0.1223(6) 0.039(3) Uani 1 1 d . . . C213 C 0.3215(6) 0.3164(6) 0.1166(7) 0.052(3) Uani 1 1 d . . . H213 H 0.3567 0.3009 0.1488 0.08(4) Uiso 1 1 d R . . C214 C 0.3210(6) 0.3746(6) 0.0617(8) 0.057(3) Uani 1 1 d . . . H211' H 0.3555 0.3981 0.0592 0.08(4) Uiso 1 1 d R . . O11 O 0.1454(3) 0.7729(4) 0.0040(5) 0.062(2) Uani 1 1 d D . . O12 O 0.0627(4) 0.8437(5) 0.0129(6) 0.111(4) Uani 1 1 d D . . O13 O 0.0598(3) 0.7614(5) -0.0989(4) 0.071(3) Uani 1 1 d D . . O14 O 0.0627(4) 0.7184(5) 0.0376(6) 0.103(4) Uani 1 1 d D . . S S 0.08307(13) 0.77521(16) -0.01192(18) 0.0498(8) Uani 1 1 d D . . O1W O 0.0511(7) 0.5722(9) 0.0280(11) 0.193(7) Uiso 1 1 d . . . O2W O 0.0867(5) 0.9790(7) 0.9691(8) 0.129(4) Uiso 1 1 d . . . O3W O 0.0547(6) 0.7411(7) 0.4442(9) 0.143(5) Uiso 1 1 d . . . O4W O 0.0177(6) 0.8999(8) 0.4105(9) 0.158(5) Uiso 1 1 d . . . O5W O 0.0761(10) 0.7236(12) 0.2063(14) 0.243(9) Uiso 1 1 d . . . O6W O 0.0903(11) 0.6366(13) 0.3547(14) 0.273(10) Uiso 1 1 d . . . O7W O 0.0000 0.8391(16) 0.2500 0.240(13) Uiso 1 2 d S . . O8W O 0.4706(11) 0.0280(14) 0.1190(15) 0.294(12) Uiso 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 Cu1 0.0341(11) 0.0336(11) 0.0839(16) 0.000 0.0245(10) 0.000 N11 0.027(5) 0.041(5) 0.048(6) -0.008(5) 0.004(5) -0.005(4) N12 0.040(5) 0.044(5) 0.053(6) -0.008(5) 0.022(5) -0.018(4) N13 0.030(5) 0.040(5) 0.053(6) -0.005(5) 0.008(5) -0.003(4) N14 0.043(6) 0.042(6) 0.068(7) -0.005(5) 0.020(5) -0.016(5) C11 0.031(6) 0.046(7) 0.041(7) -0.002(6) 0.015(5) 0.005(5) C12 0.079(10) 0.073(9) 0.061(9) 0.001(8) 0.019(8) -0.034(8) C13 0.055(8) 0.059(8) 0.059(9) -0.007(7) 0.003(7) -0.015(7) C14 0.037(7) 0.043(7) 0.068(9) -0.004(7) 0.027(6) -0.002(6) C15 0.060(9) 0.075(9) 0.044(8) 0.001(7) 0.010(7) -0.018(7) C16 0.039(7) 0.065(8) 0.045(8) 0.005(7) 0.009(6) -0.005(6) C17 0.059(8) 0.041(7) 0.074(10) -0.004(7) 0.020(7) -0.012(6) C18 0.056(9) 0.045(8) 0.108(12) -0.022(8) 0.036(8) -0.025(7) C19 0.049(7) 0.039(6) 0.042(7) -0.007(5) 0.017(6) -0.018(6) C110 0.058(8) 0.033(6) 0.045(7) 0.002(5) 0.004(6) -0.010(6) C111 0.061(8) 0.038(7) 0.058(8) 0.005(6) 0.027(7) -0.008(6) C112 0.056(8) 0.046(7) 0.057(8) -0.021(6) 0.027(6) -0.018(6) C113 0.062(9) 0.047(7) 0.047(7) 0.000(6) 0.016(7) -0.025(7) C114 0.057(8) 0.029(6) 0.072(9) -0.005(6) 0.021(7) -0.009(6) Cu2 0.0650(13) 0.0253(10) 0.0240(9) -0.0009(8) 0.0086(9) 0.0004(9) N21 0.066(7) 0.024(5) 0.039(5) 0.003(4) 0.014(5) 0.000(5) N22 0.074(7) 0.024(5) 0.051(6) 0.001(4) 0.027(6) -0.001(5) N23 0.032(5) 0.025(4) 0.029(4) 0.002(4) 0.003(4) 0.002(4) N24 0.039(5) 0.042(5) 0.024(4) 0.003(4) 0.008(4) 0.000(4) C21 0.065(9) 0.033(6) 0.042(7) 0.006(5) 0.014(6) 0.006(6) C22 0.055(9) 0.038(7) 0.078(9) -0.005(6) 0.014(7) -0.011(6) C23 0.055(8) 0.039(7) 0.067(8) -0.001(6) 0.024(7) 0.001(6) C24 0.031(6) 0.032(6) 0.033(5) 0.000(5) 0.002(5) 0.002(5) C25 0.043(7) 0.041(6) 0.040(6) -0.002(5) 0.009(5) 0.001(5) C26 0.044(7) 0.044(7) 0.032(6) 0.001(5) -0.006(5) -0.007(5) C27 0.124(13) 0.032(7) 0.067(10) 0.004(6) 0.054(9) 0.021(7) C28 0.079(10) 0.049(7) 0.031(6) 0.003(6) 0.021(6) 0.006(7) C29 0.093(10) 0.027(6) 0.040(7) -0.005(5) 0.037(8) 0.001(7) C210 0.063(8) 0.045(7) 0.045(7) 0.008(6) 0.006(7) 0.010(6) C211 0.060(9) 0.043(7) 0.052(8) 0.005(6) 0.025(7) 0.002(6) C212 0.062(8) 0.037(6) 0.022(5) -0.001(5) 0.015(6) 0.011(6) C213 0.060(9) 0.053(8) 0.044(7) 0.006(6) 0.012(7) -0.002(7) C214 0.064(9) 0.044(7) 0.063(9) -0.004(7) 0.018(8) -0.008(7) O11 0.041(5) 0.081(6) 0.062(5) 0.002(5) 0.007(4) 0.004(4) O12 0.119(9) 0.100(8) 0.113(9) -0.029(7) 0.019(7) 0.045(7) O13 0.045(5) 0.113(8) 0.055(5) -0.008(5) 0.007(4) -0.007(5) O14 0.125(9) 0.115(8) 0.078(7) 0.032(6) 0.041(7) -0.016(7) S 0.0475(18) 0.0560(19) 0.0474(18) 0.0034(15) 0.0134(15) 0.0054(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 1.987(8) . ? Cu1 N11 1.987(8) 2 ? Cu1 N13 2.011(8) 4_545 ? Cu1 N13 2.011(8) 3_445 ? N11 C11 1.311(12) . ? N11 C13 1.359(14) . ? N12 C11 1.335(12) . ? N12 C12 1.364(14) . ? N12 C17 1.471(13) . ? N13 C14 1.320(13) . ? N13 C16 1.353(13) . ? N13 Cu1 2.011(8) 3 ? N14 C14 1.344(13) . ? N14 C15 1.365(14) . ? N14 C18 1.460(14) . ? C11 H11 0.9311 . ? C12 C13 1.347(16) . ? C12 H12 0.9295 . ? C13 H13 0.9295 . ? C14 H14 0.9309 . ? C15 C16 1.343(16) . ? C15 H15 0.9303 . ? C16 H16 0.9293 . ? C17 C19 1.491(15) . ? C17 H17A 0.9697 . ? C17 H17B 0.9710 . ? C18 C112 1.504(15) . ? C18 H18A 0.9698 . ? C18 H18B 0.9706 . ? C19 C111 1.390(15) . ? C19 C110 1.394(14) . ? C110 C113 1.338(15) . ? C110 H110 0.9305 . ? C111 C114 1.338(15) . ? C111 H111 0.9316 . ? C112 C113 1.380(16) . ? C112 C114 1.396(15) . ? C113 H113 0.9295 . ? C114 H114 0.9301 . ? Cu2 N23 1.976(7) 6_565 ? Cu2 N23 1.976(7) 4 ? Cu2 N21 2.012(8) 7_565 ? Cu2 N21 2.012(8) . ? N21 C21 1.315(13) . ? N21 C23 1.365(13) . ? N22 C22 1.341(14) . ? N22 C21 1.357(13) . ? N22 C27 1.489(13) . ? N23 C24 1.321(12) . ? N23 C25 1.342(12) . ? N23 Cu2 1.976(7) 4_545 ? N24 C24 1.364(12) . ? N24 C26 1.371(13) . ? N24 C28 1.485(12) . ? C21 H21 0.9280 . ? C22 C23 1.351(15) . ? C22 H22 0.9309 . ? C23 H23 0.9295 . ? C24 H24 0.9287 . ? C25 C26 1.380(14) . ? C25 H25 0.9290 . ? C26 H26 0.9307 . ? C27 C29 1.501(15) . ? C27 H27A 0.9702 . ? C27 H27B 0.9706 . ? C28 C212 1.504(15) . ? C28 H28A 0.9710 . ? C28 H28B 0.9704 . ? C29 C214 1.347(16) . ? C29 C210 1.401(16) . ? C210 C211 1.417(15) . ? C210 H210 0.9308 . ? C211 C212 1.353(15) . ? C211 H211 0.9280 . ? C212 C213 1.358(15) . ? C213 C214 1.407(15) . ? C213 H213 0.9316 . ? C214 H211 0.9301 . ? O11 S 1.438(7) . ? O12 S 1.445(8) . ? O13 S 1.446(7) . ? O14 S 1.471(8) . ? 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 N11 Cu1 N11 87.1(5) . 2 ? N11 Cu1 N13 92.9(3) . 4_545 ? N11 Cu1 N13 178.3(4) 2 4_545 ? N11 Cu1 N13 178.3(4) . 3_445 ? N11 Cu1 N13 92.9(3) 2 3_445 ? N13 Cu1 N13 87.1(5) 4_545 3_445 ? C11 N11 C13 103.7(9) . . ? C11 N11 Cu1 127.3(8) . . ? C13 N11 Cu1 128.7(8) . . ? C11 N12 C12 106.5(9) . . ? C11 N12 C17 127.4(10) . . ? C12 N12 C17 126.0(10) . . ? C14 N13 C16 105.3(10) . . ? C14 N13 Cu1 122.8(8) . 3 ? C16 N13 Cu1 130.9(8) . 3 ? C14 N14 C15 107.4(10) . . ? C14 N14 C18 126.5(11) . . ? C15 N14 C18 125.9(11) . . ? N11 C11 N12 113.0(10) . . ? N11 C11 H11 123.5 . . ? N12 C11 H11 123.6 . . ? C13 C12 N12 105.4(11) . . ? C13 C12 H12 127.5 . . ? N12 C12 H12 127.1 . . ? C12 C13 N11 111.5(11) . . ? C12 C13 H13 124.5 . . ? N11 C13 H13 124.0 . . ? N13 C14 N14 110.8(11) . . ? N13 C14 H14 124.5 . . ? N14 C14 H14 124.7 . . ? C16 C15 N14 105.4(11) . . ? C16 C15 H15 127.5 . . ? N14 C15 H15 127.0 . . ? C15 C16 N13 111.0(11) . . ? C15 C16 H16 124.6 . . ? N13 C16 H16 124.3 . . ? N12 C17 C19 112.8(9) . . ? N12 C17 H17A 108.8 . . ? C19 C17 H17A 109.0 . . ? N12 C17 H17B 109.3 . . ? C19 C17 H17B 109.1 . . ? H17A C17 H17B 107.7 . . ? N14 C18 C112 112.4(10) . . ? N14 C18 H18A 109.2 . . ? C112 C18 H18A 108.8 . . ? N14 C18 H18B 109.1 . . ? C112 C18 H18B 109.4 . . ? H18A C18 H18B 107.9 . . ? C111 C19 C110 118.8(11) . . ? C111 C19 C17 120.9(10) . . ? C110 C19 C17 120.2(11) . . ? C113 C110 C19 120.7(11) . . ? C113 C110 H110 119.5 . . ? C19 C110 H110 119.8 . . ? C114 C111 C19 119.6(11) . . ? C114 C111 H111 120.2 . . ? C19 C111 H111 120.3 . . ? C113 C112 C114 117.8(11) . . ? C113 C112 C18 121.6(11) . . ? C114 C112 C18 120.5(12) . . ? C110 C113 C112 121.1(11) . . ? C110 C113 H113 119.9 . . ? C112 C113 H113 119.0 . . ? C111 C114 C112 122.0(12) . . ? C111 C114 H114 118.9 . . ? C112 C114 H114 119.2 . . ? N23 Cu2 N23 180.0(4) 6_565 4 ? N23 Cu2 N21 90.5(3) 6_565 7_565 ? N23 Cu2 N21 89.5(3) 4 7_565 ? N23 Cu2 N21 89.5(3) 6_565 . ? N23 Cu2 N21 90.5(3) 4 . ? N21 Cu2 N21 180.000(1) 7_565 . ? C21 N21 C23 105.8(9) . . ? C21 N21 Cu2 127.6(8) . . ? C23 N21 Cu2 126.4(7) . . ? C22 N22 C21 107.3(9) . . ? C22 N22 C27 127.4(10) . . ? C21 N22 C27 125.0(11) . . ? C24 N23 C25 107.7(8) . . ? C24 N23 Cu2 127.1(6) . 4_545 ? C25 N23 Cu2 124.9(7) . 4_545 ? C24 N24 C26 107.5(8) . . ? C24 N24 C28 126.6(9) . . ? C26 N24 C28 125.5(9) . . ? N21 C21 N22 110.5(11) . . ? N21 C21 H21 124.6 . . ? N22 C21 H21 124.9 . . ? N22 C22 C23 106.9(10) . . ? N22 C22 H22 126.7 . . ? C23 C22 H22 126.4 . . ? C22 C23 N21 109.4(11) . . ? C22 C23 H23 125.8 . . ? N21 C23 H23 124.8 . . ? N23 C24 N24 109.7(8) . . ? N23 C24 H24 125.2 . . ? N24 C24 H24 125.1 . . ? N23 C25 C26 109.5(9) . . ? N23 C25 H25 125.5 . . ? C26 C25 H25 125.0 . . ? N24 C26 C25 105.5(9) . . ? N24 C26 H26 127.0 . . ? C25 C26 H26 127.5 . . ? N22 C27 C29 114.8(9) . . ? N22 C27 H27A 108.5 . . ? C29 C27 H27A 107.2 . . ? N22 C27 H27B 109.0 . . ? C29 C27 H27B 109.5 . . ? H27A C27 H27B 107.6 . . ? N24 C28 C212 112.1(9) . . ? N24 C28 H28A 109.2 . . ? C212 C28 H28A 109.0 . . ? N24 C28 H28B 109.3 . . ? C212 C28 H28B 109.4 . . ? H28A C28 H28B 107.9 . . ? C214 C29 C210 118.3(11) . . ? C214 C29 C27 121.3(12) . . ? C210 C29 C27 120.3(13) . . ? C29 C210 C211 119.6(12) . . ? C29 C210 H210 120.3 . . ? C211 C210 H210 120.1 . . ? C212 C211 C210 120.7(12) . . ? C212 C211 H211 120.1 . . ? C210 C211 H211 119.1 . . ? C211 C212 C213 119.3(10) . . ? C211 C212 C28 120.6(11) . . ? C213 C212 C28 119.9(11) . . ? C212 C213 C214 120.7(12) . . ? C212 C213 H213 119.9 . . ? C214 C213 H213 119.4 . . ? C29 C214 C213 121.4(12) . . ? C29 C214 H211 118.8 . . ? C213 C214 H211 119.8 . . ? O11 S O12 111.1(5) . . ? O11 S O13 109.8(4) . . ? O12 S O13 110.9(5) . . ? O11 S O14 108.4(5) . . ? O12 S O14 107.8(6) . . ? O13 S O14 108.8(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.079 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.124 # * END