Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Peter A. Tasker' 'Robert A. Coxall' 'Leonard F. Lindoy' 'Hamish A. Miller' 'Andrew Parkin' 'Simon Parsons' 'David J. White' _publ_contact_author_name 'Peter A. Tasker' _publ_contact_author_address ; Department of Chemistry The University of Edinburgh The Kings Buildings West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email 'P.A.TASKER@ED.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Solvent extraction of metal sulfates by zwitterionic forms of ditopic ligands ; data_compound1 _database_code_CSD 197885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H50N4 O4' _chemical_formula_sum 'C34 H50 N4 O4' _chemical_formula_weight 578.78 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 32.080(7) _cell_length_b 10.430(2) _cell_length_c 20.871(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.156(4) _cell_angle_gamma 90.00 _cell_volume 6636(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2774 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24 _exptl_crystal_description rod _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type 'Multiscan (Sadabs)' _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART APEX diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18290 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.55 _reflns_number_total 6799 _reflns_number_gt 3546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'riding and rotating' _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 6799 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2176 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 C1A C 0.06919(9) 0.3192(3) -0.09466(13) 0.0294(6) Uani 1 1 d . . . O1A O 0.03038(6) 0.2664(2) -0.09529(10) 0.0368(5) Uani 1 1 d . . . H1A H 0.0236 0.2076 -0.1242 0.055 Uiso 1 1 calc R . . C2A C 0.09161(9) 0.2748(3) -0.13848(13) 0.0305(7) Uani 1 1 d . . . C21A C 0.07412(10) 0.1705(3) -0.18512(13) 0.0328(7) Uani 1 1 d . . . H21A H 0.0899 0.1434 -0.2144 0.039 Uiso 1 1 calc R . . N2A N 0.03829(8) 0.1139(2) -0.18830(11) 0.0325(6) Uani 1 1 d . . . C22A C 0.02450(9) 0.0049(3) -0.23332(14) 0.0361(7) Uani 1 1 d . . . H22A H 0.0333 -0.0755 -0.2074 0.043 Uiso 1 1 calc R . . H22B H 0.0394 0.0081 -0.2683 0.043 Uiso 1 1 calc R . . C3A C 0.13106(9) 0.3332(3) -0.13647(14) 0.0341(7) Uani 1 1 d . . . H3A H 0.1459 0.3044 -0.1667 0.041 Uiso 1 1 calc R . . C4A C 0.14938(9) 0.4314(3) -0.09224(13) 0.0323(7) Uani 1 1 d . . . C41A C 0.19435(9) 0.4884(3) -0.08757(15) 0.0378(7) Uani 1 1 d . . . C42A C 0.22918(12) 0.3886(4) -0.0541(2) 0.0749(12) Uani 1 1 d . . . H42A H 0.2245 0.3113 -0.0822 0.112 Uiso 1 1 calc R . . H42B H 0.2270 0.3668 -0.0096 0.112 Uiso 1 1 calc R . . H42C H 0.2584 0.4236 -0.0492 0.112 Uiso 1 1 calc R . . C43A C 0.20470(13) 0.6128(4) -0.0474(2) 0.0677(11) Uani 1 1 d . . . H43A H 0.2343 0.6414 -0.0445 0.101 Uiso 1 1 calc R . . H43B H 0.2030 0.5983 -0.0018 0.101 Uiso 1 1 calc R . . H43C H 0.1834 0.6788 -0.0699 0.101 Uiso 1 1 calc R . . C44A C 0.19720(11) 0.5156(4) -0.15756(18) 0.0567(10) Uani 1 1 d . . . H44A H 0.1737 0.5747 -0.1812 0.085 Uiso 1 1 calc R . . H44B H 0.1941 0.4352 -0.1829 0.085 Uiso 1 1 calc R . . H44C H 0.2257 0.5543 -0.1538 0.085 Uiso 1 1 calc R . . C5A C 0.12592(9) 0.4714(3) -0.04929(13) 0.0339(7) Uani 1 1 d . . . H5A H 0.1376 0.5391 -0.0185 0.041 Uiso 1 1 calc R . . C6A C 0.08659(9) 0.4169(3) -0.04968(13) 0.0316(7) Uani 1 1 d . . . C61A C 0.06161(9) 0.4625(3) -0.00308(14) 0.0371(7) Uani 1 1 d . . . H61A H 0.0362 0.5144 -0.0294 0.044 Uiso 1 1 calc R . . H61B H 0.0501 0.3870 0.0147 0.044 Uiso 1 1 calc R . . N62A N 0.08814(8) 0.5388(2) 0.05333(11) 0.0344(6) Uani 1 1 d . . . C63A C 0.11968(10) 0.4622(3) 0.10322(15) 0.0464(8) Uani 1 1 d . . . H63A H 0.1395 0.4184 0.0821 0.056 Uiso 1 1 calc R . . H63B H 0.1042 0.3958 0.1210 0.056 Uiso 1 1 calc R . . C64A C 0.14589(11) 0.5451(5) 0.15948(17) 0.0688(12) Uani 1 1 d . . . H64A H 0.1669 0.4912 0.1936 0.083 Uiso 1 1 calc R . . H64B H 0.1629 0.6072 0.1418 0.083 Uiso 1 1 calc R . . O65A O 0.11900(8) 0.6134(3) 0.19087(11) 0.0676(8) Uani 1 1 d . . . C66A C 0.08746(13) 0.6860(4) 0.14221(18) 0.0578(10) Uani 1 1 d . . . H66A H 0.1026 0.7522 0.1235 0.069 Uiso 1 1 calc R . . H66B H 0.0682 0.7304 0.1641 0.069 Uiso 1 1 calc R . . C67A C 0.06003(10) 0.6046(3) 0.08608(15) 0.0409(8) Uani 1 1 d . . . H67A H 0.0437 0.5409 0.1040 0.049 Uiso 1 1 calc R . . H67B H 0.0385 0.6589 0.0528 0.049 Uiso 1 1 calc R . . C1B C 0.06817(8) 0.1830(3) 0.16020(13) 0.0292(6) Uani 1 1 d . . . O1B O 0.02972(6) 0.2374(2) 0.12286(9) 0.0352(5) Uani 1 1 d . . . H1B H 0.0233 0.2979 0.1447 0.053 Uiso 1 1 calc R . . C2B C 0.08983(8) 0.2255(3) 0.22599(13) 0.0279(6) Uani 1 1 d . . . C21B C 0.07263(9) 0.3309(3) 0.25544(14) 0.0316(7) Uani 1 1 d . . . H21B H 0.0881 0.3569 0.3002 0.038 Uiso 1 1 calc R . . N2B N 0.03740(7) 0.3903(2) 0.22353(11) 0.0305(6) Uani 1 1 d . . . C22B C 0.02446(9) 0.4998(3) 0.25601(14) 0.0331(7) Uani 1 1 d . . . H22C H 0.0330 0.5800 0.2380 0.040 Uiso 1 1 calc R . . H22D H 0.0400 0.4969 0.3051 0.040 Uiso 1 1 calc R . . C3B C 0.12885(9) 0.1665(3) 0.26215(14) 0.0317(7) Uani 1 1 d . . . H3B H 0.1433 0.1946 0.3069 0.038 Uiso 1 1 calc R . . C4B C 0.14753(8) 0.0683(3) 0.23569(13) 0.0292(6) Uani 1 1 d . . . C41B C 0.19275(9) 0.0134(3) 0.27439(15) 0.0357(7) Uani 1 1 d . . . C42B C 0.20070(11) -0.1162(3) 0.24586(17) 0.0545(9) Uani 1 1 d . . . H42D H 0.2289 -0.1513 0.2737 0.082 Uiso 1 1 calc R . . H42E H 0.2013 -0.1048 0.1995 0.082 Uiso 1 1 calc R . . H42F H 0.1771 -0.1756 0.2461 0.082 Uiso 1 1 calc R . . C43B C 0.19753(11) -0.0029(4) 0.34888(16) 0.0523(9) Uani 1 1 d . . . H43D H 0.2263 -0.0400 0.3723 0.078 Uiso 1 1 calc R . . H43E H 0.1744 -0.0601 0.3537 0.078 Uiso 1 1 calc R . . H43F H 0.1949 0.0808 0.3685 0.078 Uiso 1 1 calc R . . C44B C 0.22641(11) 0.1095(4) 0.2662(2) 0.0640(11) Uani 1 1 d . . . H44D H 0.2228 0.1909 0.2874 0.096 Uiso 1 1 calc R . . H44E H 0.2221 0.1235 0.2181 0.096 Uiso 1 1 calc R . . H44F H 0.2560 0.0761 0.2879 0.096 Uiso 1 1 calc R . . C5B C 0.12471(9) 0.0299(3) 0.17018(13) 0.0315(7) Uani 1 1 d . . . H5B H 0.1365 -0.0380 0.1509 0.038 Uiso 1 1 calc R . . C6B C 0.08582(9) 0.0854(3) 0.13169(13) 0.0298(6) Uani 1 1 d . . . C61B C 0.06173(9) 0.0420(3) 0.06079(14) 0.0367(7) Uani 1 1 d . . . H61C H 0.0354 -0.0071 0.0613 0.044 Uiso 1 1 calc R . . H61D H 0.0516 0.1186 0.0321 0.044 Uiso 1 1 calc R . . N62B N 0.08825(7) -0.0373(2) 0.03095(11) 0.0323(6) Uani 1 1 d . . . C63B C 0.12140(10) 0.0365(3) 0.01274(15) 0.0438(8) Uani 1 1 d . . . H63C H 0.1410 0.0798 0.0532 0.053 Uiso 1 1 calc R . . H63D H 0.1071 0.1030 -0.0208 0.053 Uiso 1 1 calc R . . C64B C 0.14772(11) -0.0518(4) -0.01643(17) 0.0605(11) Uani 1 1 d . . . H64C H 0.1702 -0.0015 -0.0289 0.073 Uiso 1 1 calc R . . H64D H 0.1631 -0.1151 0.0182 0.073 Uiso 1 1 calc R . . O65B O 0.12099(7) -0.1180(3) -0.07441(10) 0.0577(7) Uani 1 1 d . . . C66B C 0.08769(11) -0.1878(3) -0.05749(16) 0.0488(9) Uani 1 1 d . . . H66C H 0.1015 -0.2546 -0.0238 0.059 Uiso 1 1 calc R . . H66D H 0.0686 -0.2311 -0.0983 0.059 Uiso 1 1 calc R . . C67B C 0.06050(10) -0.1014(3) -0.02936(14) 0.0370(7) Uani 1 1 d . . . H67C H 0.0457 -0.0366 -0.0635 0.044 Uiso 1 1 calc R . . H67D H 0.0377 -0.1521 -0.0180 0.044 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 C1A 0.0363(15) 0.0273(16) 0.0238(14) 0.0010(12) 0.0082(11) 0.0070(13) O1A 0.0407(11) 0.0356(13) 0.0348(12) -0.0105(9) 0.0128(9) 0.0002(10) C2A 0.0398(16) 0.0281(16) 0.0231(14) 0.0018(12) 0.0091(12) 0.0084(13) C21A 0.0467(17) 0.0310(17) 0.0206(14) 0.0014(12) 0.0101(12) 0.0105(15) N2A 0.0448(14) 0.0285(14) 0.0223(12) -0.0013(10) 0.0077(10) 0.0058(12) C22A 0.0569(18) 0.0170(15) 0.0327(16) -0.0019(13) 0.0115(13) 0.0053(13) C3A 0.0432(16) 0.0335(17) 0.0268(15) 0.0023(13) 0.0125(12) 0.0112(14) C4A 0.0393(16) 0.0334(17) 0.0251(14) 0.0033(13) 0.0112(12) 0.0086(13) C41A 0.0342(16) 0.0367(19) 0.0415(17) 0.0012(14) 0.0102(13) 0.0007(13) C42A 0.051(2) 0.066(3) 0.092(3) 0.010(2) 0.000(2) 0.009(2) C43A 0.082(3) 0.056(3) 0.082(3) -0.013(2) 0.050(2) -0.012(2) C44A 0.052(2) 0.064(3) 0.059(2) 0.0027(19) 0.0249(17) -0.0041(18) C5A 0.0436(17) 0.0309(17) 0.0261(15) 0.0036(13) 0.0092(12) 0.0049(14) C6A 0.0426(16) 0.0297(16) 0.0236(14) 0.0007(12) 0.0120(12) 0.0045(14) C61A 0.0404(16) 0.0393(18) 0.0335(16) -0.0110(14) 0.0144(13) -0.0013(14) N62A 0.0442(14) 0.0367(15) 0.0249(12) -0.0071(11) 0.0144(10) -0.0062(12) C63A 0.0482(18) 0.057(2) 0.0360(17) 0.0082(17) 0.0156(14) -0.0055(17) C64A 0.056(2) 0.112(4) 0.0370(19) -0.005(2) 0.0117(17) -0.024(2) O65A 0.0782(17) 0.097(2) 0.0316(13) -0.0215(14) 0.0230(12) -0.0345(17) C66A 0.086(3) 0.054(2) 0.045(2) -0.0243(19) 0.038(2) -0.029(2) C67A 0.0584(19) 0.0358(18) 0.0360(17) -0.0089(14) 0.0257(14) -0.0079(16) C1B 0.0339(15) 0.0278(16) 0.0294(15) -0.0017(13) 0.0147(12) -0.0078(13) O1B 0.0381(11) 0.0344(12) 0.0332(11) -0.0098(9) 0.0110(9) 0.0020(9) C2B 0.0356(15) 0.0274(16) 0.0259(14) -0.0019(12) 0.0170(12) -0.0056(12) C21B 0.0425(16) 0.0320(17) 0.0267(15) -0.0063(13) 0.0200(13) -0.0104(14) N2B 0.0391(13) 0.0260(13) 0.0326(13) -0.0062(11) 0.0205(11) -0.0064(11) C22B 0.0473(17) 0.0190(16) 0.0399(16) -0.0040(13) 0.0235(14) -0.0043(13) C3B 0.0383(15) 0.0324(17) 0.0277(14) -0.0046(13) 0.0150(12) -0.0080(14) C4B 0.0360(15) 0.0301(16) 0.0260(14) -0.0005(12) 0.0161(12) -0.0065(13) C41B 0.0324(15) 0.0370(18) 0.0396(16) -0.0074(14) 0.0138(13) -0.0016(13) C42B 0.058(2) 0.053(2) 0.046(2) -0.0081(18) 0.0057(16) 0.0155(18) C43B 0.0474(19) 0.060(2) 0.0450(19) 0.0029(17) 0.0075(15) 0.0125(17) C44B 0.048(2) 0.062(3) 0.087(3) 0.003(2) 0.0270(19) -0.0065(19) C5B 0.0379(16) 0.0304(16) 0.0323(15) -0.0064(13) 0.0198(12) -0.0041(13) C6B 0.0382(15) 0.0274(16) 0.0274(14) -0.0037(12) 0.0153(12) -0.0030(13) C61B 0.0411(16) 0.0383(18) 0.0293(15) -0.0098(14) 0.0091(13) 0.0032(14) N62B 0.0413(13) 0.0338(14) 0.0235(12) -0.0014(11) 0.0125(10) 0.0039(11) C63B 0.0521(19) 0.050(2) 0.0311(16) 0.0039(15) 0.0160(14) 0.0007(17) C64B 0.054(2) 0.096(3) 0.0377(19) -0.006(2) 0.0233(16) 0.006(2) O65B 0.0653(15) 0.0817(19) 0.0317(12) -0.0074(12) 0.0233(11) 0.0148(14) C66B 0.068(2) 0.047(2) 0.0333(17) -0.0062(16) 0.0179(16) 0.0142(18) C67B 0.0500(17) 0.0359(18) 0.0251(15) -0.0045(13) 0.0117(13) 0.0050(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 C1A O1A 1.358(3) . ? C1A C6A 1.380(4) . ? C1A C2A 1.407(4) . ? O1A H1A 0.8400 . ? C2A C3A 1.393(4) . ? C2A C21A 1.451(4) . ? C21A N2A 1.275(4) . ? C21A H21A 0.9500 . ? N2A C22A 1.453(3) . ? C22A C22A 1.508(6) 2_554 ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C3A C4A 1.381(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.402(4) . ? C4A C41A 1.535(4) . ? C41A C44A 1.519(4) . ? C41A C43A 1.525(5) . ? C41A C42A 1.527(4) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C5A C6A 1.382(4) . ? C5A H5A 0.9500 . ? C6A C61A 1.517(4) . ? C61A N62A 1.455(3) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? N62A C63A 1.446(4) . ? N62A C67A 1.462(4) . ? C63A C64A 1.489(5) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A O65A 1.426(5) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? O65A C66A 1.410(4) . ? C66A C67A 1.491(4) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? C1B O1B 1.360(3) . ? C1B C6B 1.387(4) . ? C1B C2B 1.403(4) . ? O1B H1B 0.8400 . ? C2B C3B 1.388(4) . ? C2B C21B 1.450(4) . ? C21B N2B 1.279(3) . ? C21B H21B 0.9500 . ? N2B C22B 1.453(3) . ? C22B C22B 1.510(5) 2 ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C3B C4B 1.385(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.393(4) . ? C4B C41B 1.535(4) . ? C41B C44B 1.522(4) . ? C41B C43B 1.523(4) . ? C41B C42B 1.530(4) . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C5B C6B 1.383(4) . ? C5B H5B 0.9500 . ? C6B C61B 1.509(4) . ? C61B N62B 1.458(3) . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? N62B C63B 1.456(4) . ? N62B C67B 1.458(3) . ? C63B C64B 1.501(4) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B O65B 1.424(4) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? O65B C66B 1.425(4) . ? C66B C67B 1.496(4) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C6A 118.8(2) . . ? O1A C1A C2A 120.9(2) . . ? C6A C1A C2A 120.3(3) . . ? C1A O1A H1A 109.5 . . ? C3A C2A C1A 118.7(3) . . ? C3A C2A C21A 120.4(3) . . ? C1A C2A C21A 120.9(3) . . ? N2A C21A C2A 122.4(3) . . ? N2A C21A H21A 118.8 . . ? C2A C21A H21A 118.8 . . ? C21A N2A C22A 118.9(2) . . ? N2A C22A C22A 111.2(2) . 2_554 ? N2A C22A H22A 109.4 . . ? C22A C22A H22A 109.4 2_554 . ? N2A C22A H22B 109.4 . . ? C22A C22A H22B 109.4 2_554 . ? H22A C22A H22B 108.0 . . ? C4A C3A C2A 122.5(3) . . ? C4A C3A H3A 118.7 . . ? C2A C3A H3A 118.7 . . ? C3A C4A C5A 116.5(3) . . ? C3A C4A C41A 121.7(3) . . ? C5A C4A C41A 121.7(3) . . ? C44A C41A C43A 107.6(3) . . ? C44A C41A C42A 108.2(3) . . ? C43A C41A C42A 109.0(3) . . ? C44A C41A C4A 110.4(2) . . ? C43A C41A C4A 113.8(3) . . ? C42A C41A C4A 107.7(3) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C6A C5A C4A 123.0(3) . . ? C6A C5A H5A 118.5 . . ? C4A C5A H5A 118.5 . . ? C1A C6A C5A 118.9(3) . . ? C1A C6A C61A 119.1(2) . . ? C5A C6A C61A 122.1(3) . . ? N62A C61A C6A 113.4(2) . . ? N62A C61A H61A 108.9 . . ? C6A C61A H61A 108.9 . . ? N62A C61A H61B 108.9 . . ? C6A C61A H61B 108.9 . . ? H61A C61A H61B 107.7 . . ? C63A N62A C61A 112.5(2) . . ? C63A N62A C67A 108.6(2) . . ? C61A N62A C67A 110.2(2) . . ? N62A C63A C64A 110.1(3) . . ? N62A C63A H63A 109.6 . . ? C64A C63A H63A 109.6 . . ? N62A C63A H63B 109.6 . . ? C64A C63A H63B 109.6 . . ? H63A C63A H63B 108.2 . . ? O65A C64A C63A 112.2(3) . . ? O65A C64A H64A 109.2 . . ? C63A C64A H64A 109.2 . . ? O65A C64A H64B 109.2 . . ? C63A C64A H64B 109.2 . . ? H64A C64A H64B 107.9 . . ? C66A O65A C64A 109.8(3) . . ? O65A C66A C67A 112.1(3) . . ? O65A C66A H66A 109.2 . . ? C67A C66A H66A 109.2 . . ? O65A C66A H66B 109.2 . . ? C67A C66A H66B 109.2 . . ? H66A C66A H66B 107.9 . . ? N62A C67A C66A 109.6(3) . . ? N62A C67A H67A 109.7 . . ? C66A C67A H67A 109.7 . . ? N62A C67A H67B 109.7 . . ? C66A C67A H67B 109.7 . . ? H67A C67A H67B 108.2 . . ? O1B C1B C6B 118.6(2) . . ? O1B C1B C2B 120.9(2) . . ? C6B C1B C2B 120.5(3) . . ? C1B O1B H1B 109.5 . . ? C3B C2B C1B 118.7(2) . . ? C3B C2B C21B 120.2(2) . . ? C1B C2B C21B 121.1(3) . . ? N2B C21B C2B 122.5(2) . . ? N2B C21B H21B 118.7 . . ? C2B C21B H21B 118.7 . . ? C21B N2B C22B 118.2(2) . . ? N2B C22B C22B 110.8(2) . 2 ? N2B C22B H22C 109.5 . . ? C22B C22B H22C 109.5 2 . ? N2B C22B H22D 109.5 . . ? C22B C22B H22D 109.5 2 . ? H22C C22B H22D 108.1 . . ? C4B C3B C2B 122.7(3) . . ? C4B C3B H3B 118.7 . . ? C2B C3B H3B 118.7 . . ? C3B C4B C5B 116.3(3) . . ? C3B C4B C41B 121.4(2) . . ? C5B C4B C41B 122.1(2) . . ? C44B C41B C43B 109.8(3) . . ? C44B C41B C42B 109.2(3) . . ? C43B C41B C42B 108.8(3) . . ? C44B C41B C4B 106.4(3) . . ? C43B C41B C4B 110.9(2) . . ? C42B C41B C4B 111.7(2) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C6B C5B C4B 123.6(3) . . ? C6B C5B H5B 118.2 . . ? C4B C5B H5B 118.2 . . ? C5B C6B C1B 118.2(2) . . ? C5B C6B C61B 122.6(2) . . ? C1B C6B C61B 119.2(2) . . ? N62B C61B C6B 113.6(2) . . ? N62B C61B H61C 108.9 . . ? C6B C61B H61C 108.9 . . ? N62B C61B H61D 108.9 . . ? C6B C61B H61D 108.9 . . ? H61C C61B H61D 107.7 . . ? C63B N62B C67B 108.4(2) . . ? C63B N62B C61B 112.5(2) . . ? C67B N62B C61B 110.4(2) . . ? N62B C63B C64B 109.3(3) . . ? N62B C63B H63C 109.8 . . ? C64B C63B H63C 109.8 . . ? N62B C63B H63D 109.8 . . ? C64B C63B H63D 109.8 . . ? H63C C63B H63D 108.3 . . ? O65B C64B C63B 112.1(3) . . ? O65B C64B H64C 109.2 . . ? C63B C64B H64C 109.2 . . ? O65B C64B H64D 109.2 . . ? C63B C64B H64D 109.2 . . ? H64C C64B H64D 107.9 . . ? C64B O65B C66B 109.7(2) . . ? O65B C66B C67B 111.3(3) . . ? O65B C66B H66C 109.4 . . ? C67B C66B H66C 109.4 . . ? O65B C66B H66D 109.4 . . ? C67B C66B H66D 109.4 . . ? H66C C66B H66D 108.0 . . ? N62B C67B C66B 110.0(2) . . ? N62B C67B H67C 109.7 . . ? C66B C67B H67C 109.7 . . ? N62B C67B H67D 109.7 . . ? C66B C67B H67D 109.7 . . ? H67C C67B H67D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.781 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.092 #===END data_compound2 _database_code_CSD 197886 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C38H56N4O4].?0.5C6H14' _chemical_formula_sum 'C41 H63 N4 O4' _chemical_formula_weight 675.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 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 24.786(3) _cell_length_b 12.9082(15) _cell_length_c 26.542(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.715(18) _cell_angle_gamma 90.00 _cell_volume 8488(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -3 _diffrn_reflns_number 8611 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 69.73 _reflns_number_total 7339 _reflns_number_gt 3727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'riding and rotating' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7339 _refine_ls_number_parameters 434 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 C1A C 0.12132(12) 0.7384(2) 0.22017(12) 0.0556(8) Uani 1 1 d . . . O1A O 0.16254(8) 0.79106(17) 0.24379(9) 0.0664(6) Uani 1 1 d . . . H1A H 0.1530 0.8516 0.2491 0.100 Uiso 1 1 calc R . . C2A C 0.07234(12) 0.7874(2) 0.20827(12) 0.0513(8) Uani 1 1 d . . . C21A C 0.06345(13) 0.8966(2) 0.21850(12) 0.0540(8) Uani 1 1 d . . . H21A H 0.0296 0.9255 0.2097 0.065 Uiso 1 1 calc R . . N2A N 0.09968(10) 0.9556(2) 0.23902(10) 0.0528(6) Uani 1 1 d . . . C22A C 0.08671(12) 1.0654(2) 0.24365(11) 0.0512(8) Uani 1 1 d . . . H22A H 0.0474 1.0750 0.2380 0.061 Uiso 1 1 calc R . . C23A C 0.11655(14) 1.1263(3) 0.20409(13) 0.0655(9) Uani 1 1 d . . . H23A H 0.1049 1.1023 0.1705 0.079 Uiso 1 1 calc R . . H23B H 0.1554 1.1131 0.2082 0.079 Uiso 1 1 calc R . . C24A C 0.10618(16) 1.2424(3) 0.20816(15) 0.0784(11) Uani 1 1 d . . . H24A H 0.1272 1.2792 0.1831 0.094 Uiso 1 1 calc R . . H24B H 0.0679 1.2566 0.2010 0.094 Uiso 1 1 calc R . . C3A C 0.03063(12) 0.7305(3) 0.18515(12) 0.0563(8) Uani 1 1 d . . . H3A H -0.0023 0.7638 0.1773 0.068 Uiso 1 1 calc R . . C4A C 0.03623(12) 0.6265(2) 0.17337(12) 0.0553(8) Uani 1 1 d . A . C41A C -0.01024(12) 0.5628(3) 0.14967(13) 0.0604(9) Uani 1 1 d D . . C42A C -0.0279(3) 0.4808(5) 0.1863(2) 0.0896(18) Uani 0.70 1 d PD A 1 H42A H -0.0574 0.4410 0.1711 0.134 Uiso 0.70 1 calc PR A 1 H42B H -0.0399 0.5136 0.2169 0.134 Uiso 0.70 1 calc PR A 1 H42C H 0.0022 0.4350 0.1944 0.134 Uiso 0.70 1 calc PR A 1 C43A C 0.0078(3) 0.5146(6) 0.1007(2) 0.099(2) Uani 0.70 1 d PD A 1 H43A H -0.0216 0.4746 0.0857 0.148 Uiso 0.70 1 calc PR A 1 H43B H 0.0385 0.4696 0.1076 0.148 Uiso 0.70 1 calc PR A 1 H43C H 0.0181 0.5690 0.0777 0.148 Uiso 0.70 1 calc PR A 1 C44A C -0.0601(2) 0.6303(5) 0.1370(3) 0.0892(18) Uani 0.70 1 d PD A 1 H44A H -0.0884 0.5874 0.1221 0.134 Uiso 0.70 1 calc PR A 1 H44B H -0.0504 0.6839 0.1133 0.134 Uiso 0.70 1 calc PR A 1 H44C H -0.0727 0.6620 0.1675 0.134 Uiso 0.70 1 calc PR A 1 C45A C -0.0115(7) 0.5679(12) 0.0934(4) 0.0896(18) Uani 0.30 1 d PD A 2 H45A H -0.0415 0.5270 0.0801 0.134 Uiso 0.30 1 calc PR A 2 H45B H 0.0221 0.5406 0.0809 0.134 Uiso 0.30 1 calc PR A 2 H45C H -0.0158 0.6393 0.0827 0.134 Uiso 0.30 1 calc PR A 2 C46A C -0.0639(5) 0.5997(13) 0.1688(6) 0.099(2) Uani 0.30 1 d PD A 2 H46A H -0.0928 0.5589 0.1534 0.148 Uiso 0.30 1 calc PR A 2 H46B H -0.0690 0.6721 0.1601 0.148 Uiso 0.30 1 calc PR A 2 H46C H -0.0642 0.5919 0.2051 0.148 Uiso 0.30 1 calc PR A 2 C47A C -0.0049(6) 0.4468(8) 0.1631(6) 0.0892(18) Uani 0.30 1 d PD A 2 H47A H -0.0349 0.4089 0.1476 0.134 Uiso 0.30 1 calc PR A 2 H47B H -0.0054 0.4386 0.1994 0.134 Uiso 0.30 1 calc PR A 2 H47C H 0.0288 0.4202 0.1508 0.134 Uiso 0.30 1 calc PR A 2 C5A C 0.08604(12) 0.5815(3) 0.18468(13) 0.0602(9) Uani 1 1 d . . . H5A H 0.0911 0.5115 0.1761 0.072 Uiso 1 1 calc R A . C6A C 0.12886(12) 0.6345(3) 0.20801(13) 0.0574(8) Uani 1 1 d . A . C61A C 0.18146(14) 0.5796(3) 0.22033(14) 0.0689(10) Uani 1 1 d . . . H61A H 0.2099 0.6312 0.2263 0.083 Uiso 1 1 calc R A . H61B H 0.1778 0.5396 0.2514 0.083 Uiso 1 1 calc R . . N62A N 0.19708(10) 0.5105(2) 0.18007(11) 0.0614(7) Uani 1 1 d . A . C63A C 0.21593(15) 0.5670(3) 0.13624(15) 0.0779(11) Uani 1 1 d . . . H63A H 0.2475 0.6087 0.1461 0.093 Uiso 1 1 calc R A . H63B H 0.1875 0.6140 0.1238 0.093 Uiso 1 1 calc R . . C64A C 0.23049(17) 0.4936(4) 0.09517(16) 0.0918(13) Uani 1 1 d . A . H64A H 0.1983 0.4549 0.0840 0.110 Uiso 1 1 calc R . . H64B H 0.2433 0.5331 0.0663 0.110 Uiso 1 1 calc R . . O65A O 0.27120(10) 0.4231(3) 0.11162(12) 0.0938(9) Uani 1 1 d . . . C66A C 0.25437(15) 0.3683(3) 0.15452(18) 0.0855(12) Uani 1 1 d . A . H66A H 0.2834 0.3217 0.1661 0.103 Uiso 1 1 calc R . . H66B H 0.2228 0.3258 0.1452 0.103 Uiso 1 1 calc R . . C67A C 0.24017(13) 0.4400(3) 0.19680(15) 0.0698(10) Uani 1 1 d . . . H67A H 0.2283 0.3994 0.2256 0.084 Uiso 1 1 calc R A . H67B H 0.2721 0.4799 0.2076 0.084 Uiso 1 1 calc R . . C1B C 0.01474(12) 0.9501(2) 0.41351(11) 0.0499(7) Uani 1 1 d . . . O1B O -0.01544(8) 1.01531(17) 0.38399(8) 0.0610(6) Uani 1 1 d . . . H1B H 0.0038 1.0412 0.3622 0.092 Uiso 1 1 calc R . . C2B C 0.07011(12) 0.9378(2) 0.40566(11) 0.0506(7) Uani 1 1 d . . . C21B C 0.09689(13) 0.9920(2) 0.36551(12) 0.0530(8) Uani 1 1 d . . . H21B H 0.1343 0.9835 0.3625 0.064 Uiso 1 1 calc R . . N2B N 0.07171(10) 1.0504(2) 0.33429(10) 0.0534(6) Uani 1 1 d . . . C22B C 0.10282(12) 1.1040(2) 0.29639(12) 0.0536(8) Uani 1 1 d . . . H22B H 0.1417 1.0904 0.3029 0.064 Uiso 1 1 calc R . . C23B C 0.09236(15) 1.2206(3) 0.30015(14) 0.0703(10) Uani 1 1 d . . . H23C H 0.0535 1.2335 0.2965 0.084 Uiso 1 1 calc R . . H23D H 0.1045 1.2452 0.3335 0.084 Uiso 1 1 calc R . . C24B C 0.12157(17) 1.2809(3) 0.25985(15) 0.0794(11) Uani 1 1 d . . . H24C H 0.1125 1.3546 0.2624 0.095 Uiso 1 1 calc R . . H24D H 0.1606 1.2738 0.2655 0.095 Uiso 1 1 calc R . . C3B C 0.10046(13) 0.8731(2) 0.43809(12) 0.0537(8) Uani 1 1 d . . . H3B H 0.1375 0.8642 0.4326 0.064 Uiso 1 1 calc R . . C4B C 0.07764(12) 0.8223(2) 0.47766(12) 0.0548(8) Uani 1 1 d . B . C41B C 0.11078(14) 0.7536(3) 0.51420(13) 0.0662(9) Uani 1 1 d D . . C42B C 0.1724(2) 0.7639(6) 0.5068(3) 0.105(2) Uani 0.70 1 d PD B 1 H42D H 0.1916 0.7193 0.5307 0.158 Uiso 0.70 1 calc PR B 1 H42E H 0.1833 0.8352 0.5124 0.158 Uiso 0.70 1 calc PR B 1 H42F H 0.1808 0.7435 0.4728 0.158 Uiso 0.70 1 calc PR B 1 C43B C 0.1005(3) 0.7842(6) 0.5684(2) 0.104(2) Uani 0.70 1 d PD B 1 H43D H 0.1217 0.7404 0.5911 0.157 Uiso 0.70 1 calc PR B 1 H43E H 0.0624 0.7756 0.5750 0.157 Uiso 0.70 1 calc PR B 1 H43F H 0.1106 0.8560 0.5736 0.157 Uiso 0.70 1 calc PR B 1 C44B C 0.0962(3) 0.6407(4) 0.5064(3) 0.102(2) Uani 0.70 1 d PD B 1 H44D H 0.1176 0.5983 0.5296 0.152 Uiso 0.70 1 calc PR B 1 H44E H 0.1035 0.6208 0.4720 0.152 Uiso 0.70 1 calc PR B 1 H44F H 0.0582 0.6308 0.5126 0.152 Uiso 0.70 1 calc PR B 1 C45B C 0.0773(5) 0.6730(12) 0.5402(7) 0.105(2) Uani 0.30 1 d PD B 2 H45D H 0.1005 0.6316 0.5623 0.158 Uiso 0.30 1 calc PR B 2 H45E H 0.0599 0.6285 0.5151 0.158 Uiso 0.30 1 calc PR B 2 H45F H 0.0500 0.7071 0.5597 0.158 Uiso 0.30 1 calc PR B 2 C46B C 0.1550(6) 0.6993(14) 0.4874(5) 0.104(2) Uani 0.30 1 d PD B 2 H46D H 0.1756 0.6568 0.5111 0.157 Uiso 0.30 1 calc PR B 2 H46E H 0.1786 0.7502 0.4726 0.157 Uiso 0.30 1 calc PR B 2 H46F H 0.1394 0.6557 0.4610 0.157 Uiso 0.30 1 calc PR B 2 C47B C 0.1351(7) 0.8263(10) 0.5531(6) 0.102(2) Uani 0.30 1 d PD B 2 H47D H 0.1571 0.7872 0.5772 0.152 Uiso 0.30 1 calc PR B 2 H47E H 0.1064 0.8612 0.5706 0.152 Uiso 0.30 1 calc PR B 2 H47F H 0.1573 0.8772 0.5366 0.152 Uiso 0.30 1 calc PR B 2 C5B C 0.02235(13) 0.8359(2) 0.48384(12) 0.0570(8) Uani 1 1 d . . . H5B H 0.0060 0.8012 0.5105 0.068 Uiso 1 1 calc R B . C6B C -0.00971(12) 0.8986(2) 0.45237(12) 0.0549(8) Uani 1 1 d . B . C61B C -0.06897(13) 0.9145(3) 0.46064(14) 0.0659(9) Uani 1 1 d . . . H61C H -0.0736 0.9775 0.4807 0.079 Uiso 1 1 calc R B . H61D H -0.0875 0.9253 0.4279 0.079 Uiso 1 1 calc R . . N62B N -0.09446(10) 0.8283(2) 0.48613(11) 0.0617(7) Uani 1 1 d . B . C63B C -0.14830(15) 0.8581(3) 0.50223(17) 0.0853(12) Uani 1 1 d . . . H63C H -0.1706 0.8790 0.4728 0.102 Uiso 1 1 calc R B . H63D H -0.1454 0.9172 0.5253 0.102 Uiso 1 1 calc R . . C64B C -0.1742(2) 0.7691(4) 0.5280(2) 0.1231(19) Uani 1 1 d . B . H64C H -0.1529 0.7516 0.5585 0.148 Uiso 1 1 calc R . . H64D H -0.2104 0.7895 0.5381 0.148 Uiso 1 1 calc R . . O65B O -0.17824(13) 0.6805(3) 0.49644(17) 0.1298(13) Uani 1 1 d . . . C66B C -0.12638(19) 0.6524(3) 0.4807(2) 0.1167(18) Uani 1 1 d . B . H66C H -0.1293 0.5916 0.4587 0.140 Uiso 1 1 calc R . . H66D H -0.1038 0.6337 0.5103 0.140 Uiso 1 1 calc R . . C67B C -0.10006(15) 0.7395(3) 0.45287(17) 0.0839(12) Uani 1 1 d . . . H67C H -0.0645 0.7177 0.4418 0.101 Uiso 1 1 calc R B . H67D H -0.1222 0.7581 0.4230 0.101 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 C1A 0.0506(17) 0.052(2) 0.064(2) -0.0012(17) -0.0028(15) -0.0055(15) O1A 0.0585(13) 0.0563(14) 0.0832(17) -0.0139(12) -0.0164(11) -0.0007(11) C2A 0.0494(17) 0.0494(19) 0.0554(19) -0.0003(15) 0.0048(14) -0.0030(14) C21A 0.0545(17) 0.055(2) 0.0525(18) 0.0037(16) 0.0043(14) 0.0032(15) N2A 0.0547(15) 0.0497(16) 0.0540(15) -0.0014(13) 0.0033(12) 0.0012(12) C22A 0.0540(17) 0.0465(18) 0.0533(18) 0.0005(16) 0.0027(14) 0.0046(14) C23A 0.079(2) 0.064(2) 0.054(2) 0.0029(18) 0.0049(17) -0.0013(18) C24A 0.098(3) 0.057(2) 0.081(3) 0.016(2) 0.016(2) 0.004(2) C3A 0.0475(17) 0.062(2) 0.060(2) 0.0062(17) 0.0018(14) -0.0021(15) C4A 0.0551(18) 0.050(2) 0.060(2) 0.0037(16) -0.0009(15) -0.0075(15) C41A 0.0589(19) 0.056(2) 0.065(2) 0.0030(18) -0.0031(16) -0.0120(16) C42A 0.096(4) 0.088(4) 0.085(4) 0.011(3) -0.009(3) -0.039(3) C43A 0.084(4) 0.112(5) 0.100(5) -0.032(4) -0.004(3) -0.018(3) C44A 0.080(4) 0.080(4) 0.105(5) 0.014(3) -0.033(3) -0.024(3) C45A 0.096(4) 0.088(4) 0.085(4) 0.011(3) -0.009(3) -0.039(3) C46A 0.084(4) 0.112(5) 0.100(5) -0.032(4) -0.004(3) -0.018(3) C47A 0.080(4) 0.080(4) 0.105(5) 0.014(3) -0.033(3) -0.024(3) C5A 0.061(2) 0.051(2) 0.069(2) -0.0029(17) -0.0059(16) -0.0005(16) C6A 0.0558(19) 0.0509(19) 0.065(2) 0.0012(17) -0.0094(15) 0.0005(15) C61A 0.069(2) 0.064(2) 0.074(2) -0.005(2) -0.0160(18) 0.0088(18) N62A 0.0571(15) 0.0519(16) 0.0743(19) 0.0007(15) -0.0105(13) 0.0042(13) C63A 0.074(2) 0.076(3) 0.083(3) 0.012(2) -0.009(2) 0.002(2) C64A 0.079(3) 0.116(4) 0.081(3) 0.000(3) -0.002(2) 0.018(3) O65A 0.0622(15) 0.120(2) 0.099(2) -0.012(2) -0.0022(14) 0.0176(16) C66A 0.064(2) 0.076(3) 0.116(4) -0.011(3) -0.006(2) 0.014(2) C67A 0.060(2) 0.060(2) 0.088(3) 0.005(2) -0.0104(18) 0.0050(17) C1B 0.0518(17) 0.0484(18) 0.0490(17) -0.0025(15) -0.0072(14) 0.0040(15) O1B 0.0565(12) 0.0648(14) 0.0615(14) 0.0104(12) -0.0029(10) 0.0063(11) C2B 0.0582(18) 0.0459(18) 0.0475(17) -0.0059(15) -0.0033(14) 0.0016(14) C21B 0.0568(18) 0.0514(19) 0.0507(18) -0.0042(16) -0.0003(14) 0.0050(15) N2B 0.0596(15) 0.0476(15) 0.0530(15) -0.0013(13) 0.0025(12) 0.0054(13) C22B 0.0554(18) 0.0468(18) 0.0588(19) -0.0004(16) 0.0036(15) 0.0030(15) C23B 0.087(3) 0.050(2) 0.074(2) -0.0051(19) 0.007(2) -0.0006(18) C24B 0.103(3) 0.052(2) 0.084(3) -0.002(2) 0.018(2) -0.009(2) C3B 0.0588(18) 0.0463(18) 0.0557(19) -0.0039(16) -0.0029(15) 0.0059(15) C4B 0.0598(19) 0.0491(19) 0.055(2) -0.0017(16) -0.0085(15) 0.0020(15) C41B 0.078(2) 0.064(2) 0.056(2) 0.0069(18) -0.0088(17) 0.0070(18) C42B 0.084(4) 0.123(6) 0.107(5) 0.043(4) -0.026(3) 0.006(4) C43B 0.130(5) 0.126(6) 0.058(3) 0.015(4) -0.008(3) 0.052(4) C44B 0.143(6) 0.059(3) 0.099(5) 0.004(3) -0.059(4) 0.009(3) C45B 0.084(4) 0.123(6) 0.107(5) 0.043(4) -0.026(3) 0.006(4) C46B 0.130(5) 0.126(6) 0.058(3) 0.015(4) -0.008(3) 0.052(4) C47B 0.143(6) 0.059(3) 0.099(5) 0.004(3) -0.059(4) 0.009(3) C5B 0.066(2) 0.0503(19) 0.0545(19) 0.0045(16) 0.0015(15) -0.0062(16) C6B 0.0546(18) 0.0526(19) 0.057(2) -0.0037(16) -0.0007(15) -0.0023(15) C61B 0.066(2) 0.059(2) 0.073(2) -0.0001(19) 0.0044(17) -0.0023(17) N62B 0.0555(16) 0.0615(17) 0.0684(18) -0.0104(15) 0.0060(13) -0.0117(14) C63B 0.071(2) 0.084(3) 0.102(3) -0.018(2) 0.020(2) -0.017(2) C64B 0.097(3) 0.125(5) 0.149(5) -0.018(4) 0.041(3) -0.040(3) O65B 0.086(2) 0.098(2) 0.206(4) 0.001(3) 0.013(2) -0.0341(19) C66B 0.088(3) 0.073(3) 0.188(6) -0.004(3) -0.020(3) -0.015(3) C67B 0.069(2) 0.069(3) 0.113(3) -0.028(2) -0.001(2) -0.004(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 C1A O1A 1.364(4) . ? C1A C6A 1.394(4) . ? C1A C2A 1.396(4) . ? O1A H1A 0.8300 . ? C2A C3A 1.395(4) . ? C2A C21A 1.454(4) . ? C21A N2A 1.286(4) . ? C21A H21A 0.9400 . ? N2A C22A 1.460(4) . ? C22A C23A 1.521(4) . ? C22A C22B 1.528(4) . ? C22A H22A 0.9900 . ? C23A C24A 1.525(5) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C24A C24B 1.498(5) . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C3A C4A 1.387(4) . ? C3A H3A 0.9400 . ? C4A C5A 1.389(4) . ? C4A C41A 1.535(4) . ? C41A C45A 1.494(11) . ? C41A C42A 1.511(6) . ? C41A C46A 1.514(10) . ? C41A C43A 1.519(6) . ? C41A C44A 1.541(6) . ? C41A C47A 1.543(10) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C42A H42C 0.9700 . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C43A H43C 0.9700 . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C44A H44C 0.9700 . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C45A H45C 0.9700 . ? C46A H46A 0.9700 . ? C46A H46B 0.9700 . ? C46A H46C 0.9700 . ? C47A H47A 0.9700 . ? C47A H47B 0.9700 . ? C47A H47C 0.9700 . ? C5A C6A 1.392(4) . ? C5A H5A 0.9400 . ? C6A C61A 1.511(4) . ? C61A N62A 1.453(4) . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? N62A C63A 1.461(4) . ? N62A C67A 1.463(4) . ? C63A C64A 1.496(5) . ? C63A H63A 0.9800 . ? C63A H63B 0.9800 . ? C64A O65A 1.418(5) . ? C64A H64A 0.9800 . ? C64A H64B 0.9800 . ? O65A C66A 1.414(5) . ? C66A C67A 1.504(5) . ? C66A H66A 0.9800 . ? C66A H66B 0.9800 . ? C67A H67A 0.9800 . ? C67A H67B 0.9800 . ? C1B O1B 1.359(3) . ? C1B C6B 1.382(4) . ? C1B C2B 1.403(4) . ? O1B H1B 0.8300 . ? C2B C3B 1.402(4) . ? C2B C21B 1.452(4) . ? C21B N2B 1.271(4) . ? C21B H21B 0.9400 . ? N2B C22B 1.460(4) . ? C22B C23B 1.531(4) . ? C22B H22B 0.9900 . ? C23B C24B 1.524(5) . ? C23B H23C 0.9800 . ? C23B H23D 0.9800 . ? C24B H24C 0.9800 . ? C24B H24D 0.9800 . ? C3B C4B 1.374(4) . ? C3B H3B 0.9400 . ? C4B C5B 1.396(4) . ? C4B C41B 1.534(4) . ? C41B C46B 1.498(11) . ? C41B C47B 1.508(10) . ? C41B C45B 1.509(11) . ? C41B C44B 1.513(6) . ? C41B C43B 1.520(6) . ? C41B C42B 1.552(6) . ? C42B H42D 0.9700 . ? C42B H42E 0.9700 . ? C42B H42F 0.9700 . ? C43B H43D 0.9700 . ? C43B H43E 0.9700 . ? C43B H43F 0.9700 . ? C44B H44D 0.9700 . ? C44B H44E 0.9700 . ? C44B H44F 0.9700 . ? C45B H45D 0.9700 . ? C45B H45E 0.9700 . ? C45B H45F 0.9700 . ? C46B H46D 0.9700 . ? C46B H46E 0.9700 . ? C46B H46F 0.9700 . ? C47B H47D 0.9700 . ? C47B H47E 0.9700 . ? C47B H47F 0.9700 . ? C5B C6B 1.394(4) . ? C5B H5B 0.9400 . ? C6B C61B 1.506(4) . ? C61B N62B 1.456(4) . ? C61B H61C 0.9800 . ? C61B H61D 0.9800 . ? N62B C67B 1.451(4) . ? N62B C63B 1.465(4) . ? C63B C64B 1.492(6) . ? C63B H63C 0.9800 . ? C63B H63D 0.9800 . ? C64B O65B 1.420(6) . ? C64B H64C 0.9800 . ? C64B H64D 0.9800 . ? O65B C66B 1.410(5) . ? C66B C67B 1.505(6) . ? C66B H66C 0.9800 . ? C66B H66D 0.9800 . ? C67B H67C 0.9800 . ? C67B H67D 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 O1A C1A C6A 118.8(3) . . ? O1A C1A C2A 120.8(3) . . ? C6A C1A C2A 120.4(3) . . ? C1A O1A H1A 109.5 . . ? C3A C2A C1A 119.3(3) . . ? C3A C2A C21A 118.5(3) . . ? C1A C2A C21A 122.2(3) . . ? N2A C21A C2A 123.0(3) . . ? N2A C21A H21A 118.5 . . ? C2A C21A H21A 118.5 . . ? C21A N2A C22A 117.2(3) . . ? N2A C22A C23A 109.3(2) . . ? N2A C22A C22B 110.0(3) . . ? C23A C22A C22B 110.2(3) . . ? N2A C22A H22A 109.1 . . ? C23A C22A H22A 109.1 . . ? C22B C22A H22A 109.1 . . ? C22A C23A C24A 111.8(3) . . ? C22A C23A H23A 109.2 . . ? C24A C23A H23A 109.2 . . ? C22A C23A H23B 109.2 . . ? C24A C23A H23B 109.2 . . ? H23A C23A H23B 107.9 . . ? C24B C24A C23A 110.6(3) . . ? C24B C24A H24A 109.5 . . ? C23A C24A H24A 109.5 . . ? C24B C24A H24B 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 108.1 . . ? C4A C3A C2A 122.1(3) . . ? C4A C3A H3A 119.0 . . ? C2A C3A H3A 119.0 . . ? C3A C4A C5A 116.8(3) . . ? C3A C4A C41A 122.1(3) . . ? C5A C4A C41A 121.1(3) . . ? C45A C41A C42A 132.6(7) . . ? C45A C41A C46A 109.2(9) . . ? C42A C41A C46A 74.4(7) . . ? C45A C41A C43A 33.0(6) . . ? C42A C41A C43A 111.2(4) . . ? C46A C41A C43A 134.4(7) . . ? C45A C41A C4A 112.2(6) . . ? C42A C41A C4A 109.9(3) . . ? C46A C41A C4A 110.5(6) . . ? C43A C41A C4A 109.5(3) . . ? C45A C41A C44A 76.3(7) . . ? C42A C41A C44A 106.9(4) . . ? C46A C41A C44A 35.8(6) . . ? C43A C41A C44A 107.4(4) . . ? C4A C41A C44A 111.9(3) . . ? C45A C41A C47A 105.9(9) . . ? C42A C41A C47A 36.5(6) . . ? C46A C41A C47A 107.3(8) . . ? C43A C41A C47A 77.1(7) . . ? C4A C41A C47A 111.5(6) . . ? C44A C41A C47A 131.4(6) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C41A C45A H45A 109.5 . . ? C41A C45A H45B 109.5 . . ? H45A C45A H45B 109.5 . . ? C41A C45A H45C 109.5 . . ? H45A C45A H45C 109.5 . . ? H45B C45A H45C 109.5 . . ? C41A C46A H46A 109.5 . . ? C41A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C41A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C41A C47A H47A 109.5 . . ? C41A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C41A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C4A C5A C6A 123.5(3) . . ? C4A C5A H5A 118.3 . . ? C6A C5A H5A 118.3 . . ? C5A C6A C1A 118.1(3) . . ? C5A C6A C61A 120.5(3) . . ? C1A C6A C61A 121.5(3) . . ? N62A C61A C6A 112.1(3) . . ? N62A C61A H61A 109.2 . . ? C6A C61A H61A 109.2 . . ? N62A C61A H61B 109.2 . . ? C6A C61A H61B 109.2 . . ? H61A C61A H61B 107.9 . . ? C61A N62A C63A 112.2(3) . . ? C61A N62A C67A 111.5(3) . . ? C63A N62A C67A 107.7(3) . . ? N62A C63A C64A 110.8(3) . . ? N62A C63A H63A 109.5 . . ? C64A C63A H63A 109.5 . . ? N62A C63A H63B 109.5 . . ? C64A C63A H63B 109.5 . . ? H63A C63A H63B 108.1 . . ? O65A C64A C63A 111.5(3) . . ? O65A C64A H64A 109.3 . . ? C63A C64A H64A 109.3 . . ? O65A C64A H64B 109.3 . . ? C63A C64A H64B 109.3 . . ? H64A C64A H64B 108.0 . . ? C66A O65A C64A 110.2(3) . . ? O65A C66A C67A 112.0(3) . . ? O65A C66A H66A 109.2 . . ? C67A C66A H66A 109.2 . . ? O65A C66A H66B 109.2 . . ? C67A C66A H66B 109.2 . . ? H66A C66A H66B 107.9 . . ? N62A C67A C66A 110.0(3) . . ? N62A C67A H67A 109.7 . . ? C66A C67A H67A 109.7 . . ? N62A C67A H67B 109.7 . . ? C66A C67A H67B 109.7 . . ? H67A C67A H67B 108.2 . . ? O1B C1B C6B 118.8(3) . . ? O1B C1B C2B 120.6(3) . . ? C6B C1B C2B 120.6(3) . . ? C1B O1B H1B 109.5 . . ? C3B C2B C1B 119.0(3) . . ? C3B C2B C21B 119.3(3) . . ? C1B C2B C21B 121.7(3) . . ? N2B C21B C2B 122.6(3) . . ? N2B C21B H21B 118.7 . . ? C2B C21B H21B 118.7 . . ? C21B N2B C22B 118.1(3) . . ? N2B C22B C22A 110.4(2) . . ? N2B C22B C23B 109.1(2) . . ? C22A C22B C23B 109.9(3) . . ? N2B C22B H22B 109.2 . . ? C22A C22B H22B 109.2 . . ? C23B C22B H22B 109.2 . . ? C24B C23B C22B 111.8(3) . . ? C24B C23B H23C 109.2 . . ? C22B C23B H23C 109.2 . . ? C24B C23B H23D 109.2 . . ? C22B C23B H23D 109.2 . . ? H23C C23B H23D 107.9 . . ? C24A C24B C23B 111.1(3) . . ? C24A C24B H24C 109.4 . . ? C23B C24B H24C 109.4 . . ? C24A C24B H24D 109.4 . . ? C23B C24B H24D 109.4 . . ? H24C C24B H24D 108.0 . . ? C4B C3B C2B 121.9(3) . . ? C4B C3B H3B 119.1 . . ? C2B C3B H3B 119.1 . . ? C3B C4B C5B 117.2(3) . . ? C3B C4B C41B 122.3(3) . . ? C5B C4B C41B 120.5(3) . . ? C46B C41B C47B 109.5(10) . . ? C46B C41B C45B 108.3(9) . . ? C47B C41B C45B 109.3(9) . . ? C46B C41B C44B 70.1(8) . . ? C47B C41B C44B 141.4(7) . . ? C45B C41B C44B 42.9(7) . . ? C46B C41B C43B 135.8(7) . . ? C47B C41B C43B 42.7(7) . . ? C45B C41B C43B 68.7(8) . . ? C44B C41B C43B 109.5(5) . . ? C46B C41B C4B 110.8(6) . . ? C47B C41B C4B 105.6(6) . . ? C45B C41B C4B 113.3(6) . . ? C44B C41B C4B 110.4(3) . . ? C43B C41B C4B 110.2(3) . . ? C46B C41B C42B 40.8(7) . . ? C47B C41B C42B 70.0(8) . . ? C45B C41B C42B 132.3(7) . . ? C44B C41B C42B 107.3(5) . . ? C43B C41B C42B 106.9(4) . . ? C4B C41B C42B 112.4(3) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C41B C45B H45D 109.5 . . ? C41B C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C41B C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? C41B C46B H46D 109.5 . . ? C41B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C41B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C41B C47B H47D 109.5 . . ? C41B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C41B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C6B C5B C4B 123.1(3) . . ? C6B C5B H5B 118.4 . . ? C4B C5B H5B 118.4 . . ? C1B C6B C5B 118.1(3) . . ? C1B C6B C61B 119.6(3) . . ? C5B C6B C61B 122.2(3) . . ? N62B C61B C6B 113.7(3) . . ? N62B C61B H61C 108.8 . . ? C6B C61B H61C 108.8 . . ? N62B C61B H61D 108.8 . . ? C6B C61B H61D 108.8 . . ? H61C C61B H61D 107.7 . . ? C67B N62B C61B 110.8(3) . . ? C67B N62B C63B 108.3(3) . . ? C61B N62B C63B 110.3(3) . . ? N62B C63B C64B 109.8(4) . . ? N62B C63B H63C 109.7 . . ? C64B C63B H63C 109.7 . . ? N62B C63B H63D 109.7 . . ? C64B C63B H63D 109.7 . . ? H63C C63B H63D 108.2 . . ? O65B C64B C63B 112.0(4) . . ? O65B C64B H64C 109.2 . . ? C63B C64B H64C 109.2 . . ? O65B C64B H64D 109.2 . . ? C63B C64B H64D 109.2 . . ? H64C C64B H64D 107.9 . . ? C66B O65B C64B 109.4(3) . . ? O65B C66B C67B 111.4(4) . . ? O65B C66B H66C 109.3 . . ? C67B C66B H66C 109.3 . . ? O65B C66B H66D 109.3 . . ? C67B C66B H66D 109.3 . . ? H66C C66B H66D 108.0 . . ? N62B C67B C66B 109.1(4) . . ? N62B C67B H67C 109.9 . . ? C66B C67B H67C 109.9 . . ? N62B C67B H67D 109.9 . . ? C66B C67B H67D 109.9 . . ? H67C C67B H67D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 69.73 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.237 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.047 #===END data_compound5 _database_code_CSD 197887 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5H10N CH2 C6H2(tBu)(OH) CHN C6H4)2' _chemical_formula_sum 'C46 H58 N4 O2' _chemical_formula_weight 698.96 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0272(5) _cell_length_b 11.5800(8) _cell_length_c 20.5591(13) _cell_angle_alpha 74.237(3) _cell_angle_beta 78.507(4) _cell_angle_gamma 85.200(3) _cell_volume 2025.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.006 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20863 _diffrn_reflns_av_R_equivalents 0.1327 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5300 _reflns_number_gt 2847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric and difmap' _refine_ls_hydrogen_treatment 'riding, rotating and refined freely' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0091(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5300 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 C1A C 0.0720(4) 0.9136(3) -0.20217(17) 0.0343(9) Uani 1 1 d . . . O1A O 0.1864(3) 0.9408(2) -0.17512(13) 0.0436(7) Uani 1 1 d . . . H1A H 0.214(4) 0.862(4) -0.139(2) 0.086(14) Uiso 1 1 d . . . C2A C 0.0019(4) 0.8034(3) -0.17614(16) 0.0334(9) Uani 1 1 d . . . C21A C 0.0542(4) 0.7095(3) -0.12216(17) 0.0381(10) Uani 1 1 d . . . H21A H 0.0038 0.6354 -0.1062 0.046 Uiso 1 1 calc R . . N2A N 0.1656(3) 0.7229(3) -0.09534(14) 0.0394(8) Uani 1 1 d . . . C22A C 0.2182(4) 0.6264(4) -0.04571(18) 0.0387(10) Uani 1 1 d . . . C23A C 0.2264(4) 0.5084(4) -0.0500(2) 0.0488(11) Uani 1 1 d . . . H23A H 0.1919 0.4899 -0.0866 0.059 Uiso 1 1 calc R . . C24A C 0.2834(4) 0.4180(4) -0.0021(2) 0.0559(12) Uani 1 1 d . . . H24A H 0.2889 0.3376 -0.0057 0.067 Uiso 1 1 calc R . . C25A C 0.3326(4) 0.4446(4) 0.0514(2) 0.0536(12) Uani 1 1 d . . . H25A H 0.3715 0.3823 0.0849 0.064 Uiso 1 1 calc R . . C26A C 0.3255(4) 0.5617(4) 0.05642(19) 0.0490(11) Uani 1 1 d . . . H26A H 0.3592 0.5787 0.0937 0.059 Uiso 1 1 calc R . . C27A C 0.2697(4) 0.6553(3) 0.00775(18) 0.0397(10) Uani 1 1 d . . . C3A C -0.1173(4) 0.7814(3) -0.20492(17) 0.0361(9) Uani 1 1 d . . . H3A H -0.1645 0.7061 -0.1871 0.043 Uiso 1 1 calc R . . C4A C -0.1693(4) 0.8647(3) -0.25829(17) 0.0338(9) Uani 1 1 d . . . C41A C -0.2976(4) 0.8373(3) -0.28944(18) 0.0400(10) Uani 1 1 d . . . C42A C -0.4355(5) 0.7995(5) -0.2338(2) 0.109(2) Uani 1 1 d . . . H42A H -0.5172 0.7820 -0.2544 0.163 Uiso 1 1 calc R . . H42B H -0.4686 0.8645 -0.2116 0.163 Uiso 1 1 calc R . . H42C H -0.4097 0.7274 -0.1995 0.163 Uiso 1 1 calc R . . C43A C -0.2450(5) 0.7359(4) -0.3236(2) 0.0772(15) Uani 1 1 d . . . H43A H -0.3263 0.7177 -0.3442 0.116 Uiso 1 1 calc R . . H43B H -0.2188 0.6643 -0.2891 0.116 Uiso 1 1 calc R . . H43C H -0.1559 0.7604 -0.3595 0.116 Uiso 1 1 calc R . . C44A C -0.3422(5) 0.9432(4) -0.3448(2) 0.0732(15) Uani 1 1 d . . . H44A H -0.4242 0.9206 -0.3633 0.110 Uiso 1 1 calc R . . H44B H -0.2547 0.9665 -0.3818 0.110 Uiso 1 1 calc R . . H44C H -0.3765 1.0110 -0.3250 0.110 Uiso 1 1 calc R . . C5A C -0.0927(4) 0.9730(3) -0.28352(17) 0.0362(9) Uani 1 1 d . . . H5A H -0.1251 1.0320 -0.3205 0.043 Uiso 1 1 calc R . . C6A C 0.0273(4) 0.9987(3) -0.25757(17) 0.0356(9) Uani 1 1 d . . . C61A C 0.1058(4) 1.1170(3) -0.28552(18) 0.0452(10) Uani 1 1 d . . . H61A H 0.0699 1.1683 -0.2537 0.054 Uiso 1 1 calc R . . H61B H 0.2160 1.1021 -0.2873 0.054 Uiso 1 1 calc R . . N62A N 0.0789(3) 1.1812(3) -0.35416(14) 0.0385(8) Uani 1 1 d . . . C63A C 0.1620(4) 1.1229(3) -0.40574(19) 0.0462(10) Uani 1 1 d . . . H63A H 0.1371 1.0370 -0.3922 0.055 Uiso 1 1 calc R . . H63B H 0.2720 1.1279 -0.4082 0.055 Uiso 1 1 calc R . . C64A C 0.1226(4) 1.1821(3) -0.47591(19) 0.0536(11) Uani 1 1 d . . . H64A H 0.1838 1.1437 -0.5104 0.064 Uiso 1 1 calc R . . H64B H 0.0146 1.1704 -0.4746 0.064 Uiso 1 1 calc R . . C65A C 0.1524(4) 1.3154(3) -0.49687(19) 0.0534(11) Uani 1 1 d . . . H65A H 0.2628 1.3273 -0.5064 0.064 Uiso 1 1 calc R . . H65B H 0.1130 1.3542 -0.5395 0.064 Uiso 1 1 calc R . . C66A C 0.0776(4) 1.3732(3) -0.44078(18) 0.0459(11) Uani 1 1 d . . . H66A H -0.0336 1.3735 -0.4367 0.055 Uiso 1 1 calc R . . H66B H 0.1086 1.4575 -0.4529 0.055 Uiso 1 1 calc R . . C67A C 0.1208(4) 1.3060(3) -0.37226(18) 0.0444(10) Uani 1 1 d . . . H67A H 0.2312 1.3101 -0.3754 0.053 Uiso 1 1 calc R . . H67B H 0.0687 1.3444 -0.3360 0.053 Uiso 1 1 calc R . . C1B C -0.1510(4) 0.5688(3) 0.20522(17) 0.0333(9) Uani 1 1 d . . . O1B O -0.0086(3) 0.5236(2) 0.18909(13) 0.0418(7) Uani 1 1 d . . . H1B H 0.049(4) 0.588(3) 0.1548(18) 0.066(13) Uiso 1 1 d . . . C2B C -0.1921(4) 0.6874(3) 0.17418(16) 0.0332(9) Uani 1 1 d . . . C21B C -0.0843(4) 0.7690(3) 0.12528(17) 0.0380(10) Uani 1 1 d . . . H21B H -0.1163 0.8493 0.1065 0.046 Uiso 1 1 calc R . . N2B N 0.0535(3) 0.7358(3) 0.10666(14) 0.0374(8) Uani 1 1 d . . . C22B C 0.1548(4) 0.8215(3) 0.05998(18) 0.0371(10) Uani 1 1 d . . . C23B C 0.1494(4) 0.9403(4) 0.06275(19) 0.0468(11) Uani 1 1 d . . . H23B H 0.0761 0.9660 0.0964 0.056 Uiso 1 1 calc R . . C24B C 0.2495(5) 1.0213(4) 0.0170(2) 0.0551(12) Uani 1 1 d . . . H24B H 0.2449 1.1026 0.0189 0.066 Uiso 1 1 calc R . . C25B C 0.3568(5) 0.9828(4) -0.0317(2) 0.0562(13) Uani 1 1 d . . . H25B H 0.4257 1.0382 -0.0635 0.067 Uiso 1 1 calc R . . C26B C 0.3641(4) 0.8647(4) -0.03412(18) 0.0487(11) Uani 1 1 d . . . H26B H 0.4382 0.8397 -0.0678 0.058 Uiso 1 1 calc R . . C27B C 0.2649(4) 0.7814(3) 0.01186(17) 0.0382(10) Uani 1 1 d . . . C3B C -0.3405(4) 0.7288(3) 0.19119(16) 0.0363(9) Uani 1 1 d . . . H3B H -0.3670 0.8096 0.1704 0.044 Uiso 1 1 calc R . . C4B C -0.4508(4) 0.6565(3) 0.23725(17) 0.0351(9) Uani 1 1 d . . . C41B C -0.6122(4) 0.7016(3) 0.25744(18) 0.0398(10) Uani 1 1 d . . . C42B C -0.7253(4) 0.6117(4) 0.2559(2) 0.0711(14) Uani 1 1 d . . . H42D H -0.8285 0.6422 0.2688 0.107 Uiso 1 1 calc R . . H42E H -0.7086 0.5346 0.2884 0.107 Uiso 1 1 calc R . . H42F H -0.7113 0.6007 0.2094 0.107 Uiso 1 1 calc R . . C43B C -0.6339(4) 0.7151(4) 0.33069(18) 0.0572(12) Uani 1 1 d . . . H43D H -0.7373 0.7444 0.3443 0.086 Uiso 1 1 calc R . . H43E H -0.5620 0.7724 0.3326 0.086 Uiso 1 1 calc R . . H43F H -0.6162 0.6370 0.3622 0.086 Uiso 1 1 calc R . . C44B C -0.6464(4) 0.8221(4) 0.20988(19) 0.0630(13) Uani 1 1 d . . . H44D H -0.7510 0.8479 0.2246 0.094 Uiso 1 1 calc R . . H44E H -0.6329 0.8145 0.1627 0.094 Uiso 1 1 calc R . . H44F H -0.5774 0.8817 0.2117 0.094 Uiso 1 1 calc R . . C5B C -0.4029(4) 0.5395(3) 0.26756(17) 0.0367(10) Uani 1 1 d . . . H5B H -0.4754 0.4881 0.3000 0.044 Uiso 1 1 calc R . . C6B C -0.2583(4) 0.4942(3) 0.25342(17) 0.0325(9) Uani 1 1 d . . . C61B C -0.2145(4) 0.3671(3) 0.28829(17) 0.0416(10) Uani 1 1 d . . . H61C H -0.2275 0.3135 0.2598 0.050 Uiso 1 1 calc R . . H61D H -0.1063 0.3632 0.2918 0.050 Uiso 1 1 calc R . . N62B N -0.3053(3) 0.3245(2) 0.35710(14) 0.0369(8) Uani 1 1 d . . . C63B C -0.2650(4) 0.3862(3) 0.40450(18) 0.0472(11) Uani 1 1 d . . . H63C H -0.2750 0.4741 0.3854 0.057 Uiso 1 1 calc R . . H63D H -0.1584 0.3661 0.4094 0.057 Uiso 1 1 calc R . . C64B C -0.3666(4) 0.3494(3) 0.47432(18) 0.0531(11) Uani 1 1 d . . . H64C H -0.4723 0.3751 0.4699 0.064 Uiso 1 1 calc R . . H64D H -0.3358 0.3901 0.5059 0.064 Uiso 1 1 calc R . . C65B C -0.3578(4) 0.2145(3) 0.50425(19) 0.0529(12) Uani 1 1 d . . . H65C H -0.2566 0.1902 0.5159 0.063 Uiso 1 1 calc R . . H65D H -0.4342 0.1913 0.5470 0.063 Uiso 1 1 calc R . . C66B C -0.3860(4) 0.1510(3) 0.45308(18) 0.0473(11) Uani 1 1 d . . . H66C H -0.4929 0.1649 0.4473 0.057 Uiso 1 1 calc R . . H66D H -0.3683 0.0635 0.4709 0.057 Uiso 1 1 calc R . . C67B C -0.2832(4) 0.1952(3) 0.38363(17) 0.0420(10) Uani 1 1 d . . . H67C H -0.1763 0.1764 0.3886 0.050 Uiso 1 1 calc R . . H67D H -0.3060 0.1535 0.3508 0.050 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 C1A 0.035(2) 0.038(3) 0.034(2) -0.0146(19) -0.0084(18) -0.0023(18) O1A 0.0443(16) 0.0416(18) 0.0475(17) -0.0055(14) -0.0213(13) -0.0048(13) C2A 0.038(2) 0.033(2) 0.028(2) -0.0049(18) -0.0089(18) 0.0027(18) C21A 0.041(2) 0.039(3) 0.034(2) -0.0099(19) -0.0048(19) -0.0011(19) N2A 0.0404(19) 0.041(2) 0.0360(19) -0.0068(16) -0.0118(16) 0.0010(15) C22A 0.033(2) 0.042(3) 0.033(2) 0.002(2) -0.0046(18) 0.0014(19) C23A 0.055(3) 0.043(3) 0.049(3) -0.009(2) -0.019(2) 0.006(2) C24A 0.055(3) 0.047(3) 0.056(3) -0.004(3) -0.001(2) 0.000(2) C25A 0.041(2) 0.060(3) 0.043(3) 0.008(2) 0.001(2) 0.005(2) C26A 0.045(2) 0.060(3) 0.034(2) -0.002(2) -0.0035(19) 0.003(2) C27A 0.030(2) 0.049(3) 0.033(2) 0.001(2) -0.0024(18) -0.0017(19) C3A 0.037(2) 0.035(2) 0.037(2) -0.0080(19) -0.0070(18) -0.0033(18) C4A 0.034(2) 0.036(2) 0.035(2) -0.0141(19) -0.0102(18) 0.0028(18) C41A 0.047(2) 0.037(3) 0.036(2) -0.0020(19) -0.0156(19) -0.0055(19) C42A 0.050(3) 0.206(6) 0.062(3) -0.003(4) -0.018(2) -0.048(4) C43A 0.095(4) 0.061(3) 0.100(4) -0.037(3) -0.056(3) 0.002(3) C44A 0.087(3) 0.055(3) 0.095(4) -0.017(3) -0.062(3) -0.002(3) C5A 0.041(2) 0.035(2) 0.032(2) -0.0077(18) -0.0123(18) 0.0065(19) C6A 0.040(2) 0.032(2) 0.037(2) -0.0101(19) -0.0129(19) 0.0015(18) C61A 0.053(2) 0.037(3) 0.047(3) -0.007(2) -0.016(2) -0.005(2) N62A 0.0485(19) 0.0277(19) 0.0383(19) -0.0053(16) -0.0095(16) -0.0028(15) C63A 0.042(2) 0.036(2) 0.058(3) -0.011(2) -0.008(2) 0.0060(19) C64A 0.065(3) 0.049(3) 0.045(3) -0.014(2) -0.006(2) 0.004(2) C65A 0.056(3) 0.052(3) 0.048(3) -0.009(2) -0.005(2) 0.003(2) C66A 0.051(2) 0.035(2) 0.049(3) -0.003(2) -0.015(2) -0.003(2) C67A 0.047(2) 0.036(3) 0.049(3) -0.007(2) -0.013(2) -0.0032(19) C1B 0.031(2) 0.033(2) 0.037(2) -0.0099(19) -0.0098(18) 0.0062(19) O1B 0.0337(15) 0.0354(16) 0.0507(17) -0.0067(14) -0.0015(13) -0.0008(13) C2B 0.036(2) 0.038(3) 0.027(2) -0.0100(19) -0.0059(17) 0.0015(19) C21B 0.046(2) 0.033(2) 0.033(2) -0.0056(18) -0.0087(19) 0.001(2) N2B 0.0395(19) 0.040(2) 0.0314(18) -0.0073(15) -0.0062(15) -0.0026(16) C22B 0.037(2) 0.037(3) 0.036(2) -0.0010(19) -0.0141(19) -0.0059(19) C23B 0.051(2) 0.044(3) 0.045(3) -0.009(2) -0.012(2) -0.007(2) C24B 0.060(3) 0.047(3) 0.057(3) 0.000(2) -0.024(2) -0.013(2) C25B 0.052(3) 0.062(4) 0.045(3) 0.013(2) -0.017(2) -0.023(3) C26B 0.039(2) 0.065(3) 0.034(2) 0.004(2) -0.0079(19) -0.010(2) C27B 0.034(2) 0.049(3) 0.029(2) -0.004(2) -0.0092(19) -0.004(2) C3B 0.046(2) 0.031(2) 0.032(2) -0.0066(18) -0.0115(19) 0.0048(19) C4B 0.037(2) 0.038(3) 0.030(2) -0.0069(19) -0.0068(18) 0.0020(19) C41B 0.039(2) 0.039(3) 0.041(2) -0.012(2) -0.0067(19) 0.0061(19) C42B 0.044(3) 0.084(4) 0.097(4) -0.045(3) -0.013(2) 0.005(2) C43B 0.050(3) 0.065(3) 0.054(3) -0.020(2) -0.002(2) 0.012(2) C44B 0.051(3) 0.072(3) 0.052(3) -0.006(2) -0.007(2) 0.031(2) C5B 0.036(2) 0.036(3) 0.034(2) -0.0071(19) 0.0003(18) -0.0013(19) C6B 0.032(2) 0.027(2) 0.037(2) -0.0090(18) -0.0036(17) 0.0003(18) C61B 0.040(2) 0.035(2) 0.045(2) -0.009(2) -0.0010(19) -0.0007(19) N62B 0.0429(18) 0.0281(19) 0.0374(19) -0.0052(15) -0.0043(15) -0.0059(15) C63B 0.052(2) 0.040(3) 0.049(3) -0.007(2) -0.011(2) -0.008(2) C64B 0.062(3) 0.053(3) 0.047(3) -0.013(2) -0.013(2) -0.008(2) C65B 0.059(3) 0.050(3) 0.046(3) -0.002(2) -0.013(2) -0.010(2) C66B 0.048(2) 0.038(3) 0.051(3) -0.003(2) -0.007(2) -0.0059(19) C67B 0.043(2) 0.030(2) 0.048(3) -0.0033(19) -0.0065(19) -0.0040(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 C1A O1A 1.362(4) . ? C1A C6A 1.392(4) . ? C1A C2A 1.395(4) . ? O1A H1A 1.06(4) . ? C2A C3A 1.398(4) . ? C2A C21A 1.451(5) . ? C21A N2A 1.278(4) . ? C21A H21A 0.9500 . ? N2A C22A 1.414(4) . ? C22A C23A 1.387(5) . ? C22A C27A 1.403(5) . ? C23A C24A 1.372(5) . ? C23A H23A 0.9500 . ? C24A C25A 1.381(5) . ? C24A H24A 0.9500 . ? C25A C26A 1.382(5) . ? C25A H25A 0.9500 . ? C26A C27A 1.397(5) . ? C26A H26A 0.9500 . ? C27A C27B 1.482(5) . ? C3A C4A 1.382(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.403(4) . ? C4A C41A 1.523(4) . ? C41A C42A 1.517(5) . ? C41A C44A 1.518(5) . ? C41A C43A 1.524(5) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C5A C6A 1.385(4) . ? C5A H5A 0.9500 . ? C6A C61A 1.511(4) . ? C61A N62A 1.463(4) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? N62A C67A 1.454(4) . ? N62A C63A 1.459(4) . ? C63A C64A 1.518(5) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.518(5) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.505(5) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A C67A 1.521(4) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? C1B O1B 1.359(4) . ? C1B C6B 1.400(4) . ? C1B C2B 1.401(5) . ? O1B H1B 0.98(3) . ? C2B C3B 1.394(4) . ? C2B C21B 1.449(4) . ? C21B N2B 1.285(4) . ? C21B H21B 0.9500 . ? N2B C22B 1.424(4) . ? C22B C23B 1.388(5) . ? C22B C27B 1.401(5) . ? C23B C24B 1.380(4) . ? C23B H23B 0.9500 . ? C24B C25B 1.387(5) . ? C24B H24B 0.9500 . ? C25B C26B 1.378(5) . ? C25B H25B 0.9500 . ? C26B C27B 1.393(4) . ? C26B H26B 0.9500 . ? C3B C4B 1.386(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.401(4) . ? C4B C41B 1.522(5) . ? C41B C44B 1.518(5) . ? C41B C43B 1.528(5) . ? C41B C42B 1.528(5) . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C5B C6B 1.372(4) . ? C5B H5B 0.9500 . ? C6B C61B 1.509(4) . ? C61B N62B 1.464(4) . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? N62B C67B 1.459(4) . ? N62B C63B 1.468(4) . ? C63B C64B 1.514(4) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B C65B 1.518(5) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? C65B C66B 1.507(5) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66B C67B 1.522(4) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A C1A C6A 118.1(3) . . ? O1A C1A C2A 121.5(3) . . ? C6A C1A C2A 120.4(3) . . ? C1A O1A H1A 107(2) . . ? C1A C2A C3A 119.0(3) . . ? C1A C2A C21A 121.5(3) . . ? C3A C2A C21A 119.4(3) . . ? N2A C21A C2A 122.3(3) . . ? N2A C21A H21A 118.8 . . ? C2A C21A H21A 118.8 . . ? C21A N2A C22A 120.3(3) . . ? C23A C22A C27A 120.2(4) . . ? C23A C22A N2A 122.9(4) . . ? C27A C22A N2A 116.8(4) . . ? C24A C23A C22A 121.0(4) . . ? C24A C23A H23A 119.5 . . ? C22A C23A H23A 119.5 . . ? C23A C24A C25A 119.5(4) . . ? C23A C24A H24A 120.2 . . ? C25A C24A H24A 120.2 . . ? C24A C25A C26A 120.2(4) . . ? C24A C25A H25A 119.9 . . ? C26A C25A H25A 119.9 . . ? C25A C26A C27A 121.2(4) . . ? C25A C26A H26A 119.4 . . ? C27A C26A H26A 119.4 . . ? C26A C27A C22A 117.8(4) . . ? C26A C27A C27B 121.6(4) . . ? C22A C27A C27B 120.7(3) . . ? C4A C3A C2A 122.7(3) . . ? C4A C3A H3A 118.6 . . ? C2A C3A H3A 118.6 . . ? C3A C4A C5A 116.0(3) . . ? C3A C4A C41A 121.5(3) . . ? C5A C4A C41A 122.5(3) . . ? C42A C41A C44A 108.9(3) . . ? C42A C41A C4A 110.2(3) . . ? C44A C41A C4A 112.8(3) . . ? C42A C41A C43A 109.6(4) . . ? C44A C41A C43A 106.7(3) . . ? C4A C41A C43A 108.6(3) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C6A C5A C4A 123.7(3) . . ? C6A C5A H5A 118.2 . . ? C4A C5A H5A 118.2 . . ? C5A C6A C1A 118.2(3) . . ? C5A C6A C61A 122.2(3) . . ? C1A C6A C61A 119.6(3) . . ? N62A C61A C6A 112.9(3) . . ? N62A C61A H61A 109.0 . . ? C6A C61A H61A 109.0 . . ? N62A C61A H61B 109.0 . . ? C6A C61A H61B 109.0 . . ? H61A C61A H61B 107.8 . . ? C67A N62A C63A 109.6(3) . . ? C67A N62A C61A 111.6(3) . . ? C63A N62A C61A 110.8(3) . . ? N62A C63A C64A 110.9(3) . . ? N62A C63A H63A 109.5 . . ? C64A C63A H63A 109.5 . . ? N62A C63A H63B 109.5 . . ? C64A C63A H63B 109.5 . . ? H63A C63A H63B 108.1 . . ? C65A C64A C63A 110.9(3) . . ? C65A C64A H64A 109.5 . . ? C63A C64A H64A 109.5 . . ? C65A C64A H64B 109.5 . . ? C63A C64A H64B 109.5 . . ? H64A C64A H64B 108.1 . . ? C66A C65A C64A 110.7(3) . . ? C66A C65A H65A 109.5 . . ? C64A C65A H65A 109.5 . . ? C66A C65A H65B 109.5 . . ? C64A C65A H65B 109.5 . . ? H65A C65A H65B 108.1 . . ? C65A C66A C67A 111.0(3) . . ? C65A C66A H66A 109.4 . . ? C67A C66A H66A 109.4 . . ? C65A C66A H66B 109.4 . . ? C67A C66A H66B 109.4 . . ? H66A C66A H66B 108.0 . . ? N62A C67A C66A 110.3(3) . . ? N62A C67A H67A 109.6 . . ? C66A C67A H67A 109.6 . . ? N62A C67A H67B 109.6 . . ? C66A C67A H67B 109.6 . . ? H67A C67A H67B 108.1 . . ? O1B C1B C6B 118.8(3) . . ? O1B C1B C2B 121.4(3) . . ? C6B C1B C2B 119.8(3) . . ? C1B O1B H1B 107(2) . . ? C3B C2B C1B 119.3(3) . . ? C3B C2B C21B 118.8(3) . . ? C1B C2B C21B 121.9(3) . . ? N2B C21B C2B 121.8(3) . . ? N2B C21B H21B 119.1 . . ? C2B C21B H21B 119.1 . . ? C21B N2B C22B 119.0(3) . . ? C23B C22B C27B 120.4(3) . . ? C23B C22B N2B 121.9(3) . . ? C27B C22B N2B 117.7(3) . . ? C24B C23B C22B 120.6(4) . . ? C24B C23B H23B 119.7 . . ? C22B C23B H23B 119.7 . . ? C23B C24B C25B 119.3(4) . . ? C23B C24B H24B 120.3 . . ? C25B C24B H24B 120.3 . . ? C26B C25B C24B 120.3(4) . . ? C26B C25B H25B 119.8 . . ? C24B C25B H25B 119.8 . . ? C25B C26B C27B 121.2(4) . . ? C25B C26B H26B 119.4 . . ? C27B C26B H26B 119.4 . . ? C26B C27B C22B 118.1(4) . . ? C26B C27B C27A 121.1(4) . . ? C22B C27B C27A 120.7(3) . . ? C4B C3B C2B 122.5(3) . . ? C4B C3B H3B 118.7 . . ? C2B C3B H3B 118.7 . . ? C3B C4B C5B 115.8(3) . . ? C3B C4B C41B 123.0(3) . . ? C5B C4B C41B 121.2(3) . . ? C44B C41B C4B 112.0(3) . . ? C44B C41B C43B 108.8(3) . . ? C4B C41B C43B 108.6(3) . . ? C44B C41B C42B 108.4(3) . . ? C4B C41B C42B 110.5(3) . . ? C43B C41B C42B 108.5(3) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C6B C5B C4B 124.3(3) . . ? C6B C5B H5B 117.9 . . ? C4B C5B H5B 117.9 . . ? C5B C6B C1B 118.3(3) . . ? C5B C6B C61B 121.4(3) . . ? C1B C6B C61B 120.3(3) . . ? N62B C61B C6B 112.2(3) . . ? N62B C61B H61C 109.2 . . ? C6B C61B H61C 109.2 . . ? N62B C61B H61D 109.2 . . ? C6B C61B H61D 109.2 . . ? H61C C61B H61D 107.9 . . ? C67B N62B C61B 110.8(3) . . ? C67B N62B C63B 109.4(3) . . ? C61B N62B C63B 110.4(3) . . ? N62B C63B C64B 110.7(3) . . ? N62B C63B H63C 109.5 . . ? C64B C63B H63C 109.5 . . ? N62B C63B H63D 109.5 . . ? C64B C63B H63D 109.5 . . ? H63C C63B H63D 108.1 . . ? C63B C64B C65B 111.0(3) . . ? C63B C64B H64C 109.4 . . ? C65B C64B H64C 109.4 . . ? C63B C64B H64D 109.4 . . ? C65B C64B H64D 109.4 . . ? H64C C64B H64D 108.0 . . ? C66B C65B C64B 110.1(3) . . ? C66B C65B H65C 109.6 . . ? C64B C65B H65C 109.6 . . ? C66B C65B H65D 109.6 . . ? C64B C65B H65D 109.6 . . ? H65C C65B H65D 108.2 . . ? C65B C66B C67B 111.4(3) . . ? C65B C66B H66C 109.3 . . ? C67B C66B H66C 109.3 . . ? C65B C66B H66D 109.3 . . ? C67B C66B H66D 109.3 . . ? H66C C66B H66D 108.0 . . ? N62B C67B C66B 110.2(3) . . ? N62B C67B H67C 109.6 . . ? C66B C67B H67C 109.6 . . ? N62B C67B H67D 109.6 . . ? C66B C67B H67D 109.6 . . ? H67C C67B H67D 108.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.240 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.045 #===END data_compoundCu4-2h _database_code_CSD 197888 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu(L)] _chemical_formula_sum 'C36 H52 Cu N4 O2' _chemical_formula_weight 636.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.934(8) _cell_length_b 17.260(7) _cell_length_c 12.692(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.63(4) _cell_angle_gamma 90.00 _cell_volume 3430(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 26 _cell_measurement_theta_max 30 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6216 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 60.13 _reflns_number_total 4973 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1521P)^2^+1.2154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment 'riding and rotating groups' _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 4973 _refine_ls_number_parameters 395 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2613 _refine_ls_wR_factor_gt 0.2096 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.045 _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 0.53393(6) 0.91000(6) 0.05030(8) 0.0351(4) Uani 1 1 d . . . C1A C 0.3530(5) 0.9058(4) 0.0558(6) 0.0487(19) Uani 1 1 d . . . O1A O 0.4175(3) 0.8861(3) 0.0072(4) 0.0397(12) Uani 1 1 d . . . C2A C 0.3605(4) 0.9583(4) 0.1431(5) 0.0351(16) Uani 1 1 d . . . C21A C 0.4412(4) 0.9949(4) 0.1886(5) 0.0389(17) Uani 1 1 d . . . H21A H 0.4415 1.0312 0.2439 0.047 Uiso 1 1 calc R . . N2A N 0.5125(3) 0.9808(3) 0.1578(4) 0.0349(13) Uani 1 1 d . . . C22A C 0.5886(5) 1.0235(4) 0.2101(6) 0.0446(18) Uani 1 1 d . . . H22A H 0.5823 1.0397 0.2822 0.054 Uiso 1 1 calc R . . H22B H 0.5968 1.0698 0.1685 0.054 Uiso 1 1 calc R . . C3A C 0.2913(4) 0.9740(4) 0.1911(6) 0.0441(18) Uani 1 1 d . . . H3AA H 0.2984 1.0094 0.2483 0.053 Uiso 1 1 calc R . . C4A C 0.2130(4) 0.9405(4) 0.1592(6) 0.0434(18) Uani 1 1 d . . . C41A C 0.1358(6) 0.9579(6) 0.2146(8) 0.065(2) Uani 1 1 d U . . C42A C 0.1582(7) 1.0180(8) 0.3048(10) 0.105(4) Uani 1 1 d U . . H42A H 0.1084 1.0279 0.3367 0.157 Uiso 1 1 calc R . . H42B H 0.1762 1.0659 0.2755 0.157 Uiso 1 1 calc R . . H42C H 0.2042 0.9983 0.3591 0.157 Uiso 1 1 calc R . . C43A C 0.1085(8) 0.8848(7) 0.2617(11) 0.114(4) Uani 1 1 d U . . H43A H 0.0580 0.8947 0.2922 0.171 Uiso 1 1 calc R . . H43B H 0.1541 0.8664 0.3174 0.171 Uiso 1 1 calc R . . H43C H 0.0955 0.8457 0.2061 0.171 Uiso 1 1 calc R . . C44A C 0.0640(7) 0.9894(10) 0.1334(10) 0.125(4) Uani 1 1 d U . . H44A H 0.0174 1.0045 0.1686 0.187 Uiso 1 1 calc R . . H44B H 0.0444 0.9500 0.0800 0.187 Uiso 1 1 calc R . . H44C H 0.0837 1.0343 0.0988 0.187 Uiso 1 1 calc R . . C5A C 0.2063(4) 0.8882(5) 0.0753(7) 0.047(2) Uani 1 1 d . . . H5AA H 0.1541 0.8619 0.0551 0.056 Uiso 1 1 calc R . . C6A C 0.2704(5) 0.8719(4) 0.0194(6) 0.0429(18) Uani 1 1 d . . . C61A C 0.2602(5) 0.8173(5) -0.0738(7) 0.055(2) Uani 1 1 d . . . H61A H 0.3141 0.7896 -0.0723 0.066 Uiso 1 1 calc R . . H61B H 0.2163 0.7789 -0.0665 0.066 Uiso 1 1 calc R . . N62A N 0.2365(4) 0.8564(4) -0.1767(5) 0.0557(18) Uani 1 1 d . . . C63A C 0.2587(7) 0.8079(6) -0.2642(8) 0.085(3) Uani 1 1 d . . . H63A H 0.2288 0.7581 -0.2668 0.102 Uiso 1 1 calc R . . H63B H 0.3203 0.7976 -0.2503 0.102 Uiso 1 1 calc R . . C64A C 0.2340(8) 0.8486(8) -0.3693(8) 0.101(4) Uani 1 1 d . . . H64A H 0.2657 0.8974 -0.3671 0.121 Uiso 1 1 calc R . . H64B H 0.2499 0.8163 -0.4262 0.121 Uiso 1 1 calc R . . C65A C 0.1408(8) 0.8652(9) -0.3951(9) 0.111(5) Uani 1 1 d . . . H65A H 0.1088 0.8164 -0.4027 0.133 Uiso 1 1 calc R . . H65B H 0.1273 0.8932 -0.4633 0.133 Uiso 1 1 calc R . . C66A C 0.1147(6) 0.9136(8) -0.3065(8) 0.090(4) Uani 1 1 d . . . H66A H 0.0525 0.9199 -0.3198 0.107 Uiso 1 1 calc R . . H66B H 0.1407 0.9651 -0.3050 0.107 Uiso 1 1 calc R . . C67A C 0.1442(6) 0.8730(7) -0.1991(8) 0.079(3) Uani 1 1 d . . . H67A H 0.1302 0.9056 -0.1416 0.095 Uiso 1 1 calc R . . H67B H 0.1128 0.8242 -0.1988 0.095 Uiso 1 1 calc R . . C1B C 0.6391(4) 0.8334(4) -0.0828(6) 0.0381(16) Uani 1 1 d . . . O1B O 0.5619(3) 0.8551(3) -0.0680(4) 0.0382(11) Uani 1 1 d . . . C2B C 0.7162(4) 0.8534(4) -0.0147(5) 0.0360(16) Uani 1 1 d . . . C21B C 0.7175(5) 0.9003(4) 0.0809(5) 0.0415(18) Uani 1 1 d . . . H21B H 0.7712 0.9132 0.1213 0.050 Uiso 1 1 calc R . . N2B N 0.6517(4) 0.9255(3) 0.1144(4) 0.0372(14) Uani 1 1 d . . . C22B C 0.6642(5) 0.9694(4) 0.2161(6) 0.0434(18) Uani 1 1 d . . . H22C H 0.7175 0.9991 0.2253 0.052 Uiso 1 1 calc R . . H22D H 0.6672 0.9339 0.2770 0.052 Uiso 1 1 calc R . . C3B C 0.7943(5) 0.8236(4) -0.0315(6) 0.0435(18) Uani 1 1 d . . . H3BA H 0.8445 0.8381 0.0157 0.052 Uiso 1 1 calc R . . C4B C 0.8006(5) 0.7740(4) -0.1141(6) 0.0426(18) Uani 1 1 d . . . C41B C 0.8843(5) 0.7351(5) -0.1295(7) 0.052(2) Uani 1 1 d . . . C42B C 0.8767(6) 0.6480(6) -0.1129(10) 0.086(3) Uani 1 1 d . . . H42D H 0.9273 0.6223 -0.1278 0.129 Uiso 1 1 calc R . . H42E H 0.8267 0.6284 -0.1610 0.129 Uiso 1 1 calc R . . H42F H 0.8711 0.6379 -0.0393 0.129 Uiso 1 1 calc R . . C43B C 0.9611(5) 0.7667(6) -0.0507(7) 0.069(3) Uani 1 1 d . . . H43D H 1.0130 0.7432 -0.0654 0.104 Uiso 1 1 calc R . . H43E H 0.9548 0.7545 0.0220 0.104 Uiso 1 1 calc R . . H43F H 0.9641 0.8225 -0.0589 0.104 Uiso 1 1 calc R . . C44B C 0.8999(6) 0.7501(6) -0.2425(7) 0.074(3) Uani 1 1 d . . . H44D H 0.9528 0.7255 -0.2515 0.112 Uiso 1 1 calc R . . H44E H 0.9038 0.8055 -0.2538 0.112 Uiso 1 1 calc R . . H44F H 0.8530 0.7289 -0.2941 0.112 Uiso 1 1 calc R . . C5B C 0.7240(5) 0.7578(4) -0.1834(6) 0.0419(18) Uani 1 1 d . . . H5BA H 0.7262 0.7240 -0.2410 0.050 Uiso 1 1 calc R . . C6B C 0.6456(4) 0.7872(4) -0.1740(5) 0.0354(16) Uani 1 1 d . . . C61B C 0.5685(5) 0.7712(4) -0.2576(6) 0.0429(18) Uani 1 1 d . . . H61C H 0.5763 0.7218 -0.2925 0.051 Uiso 1 1 calc R . . H61D H 0.5188 0.7659 -0.2227 0.051 Uiso 1 1 calc R . . N62B N 0.5508(4) 0.8321(3) -0.3402(5) 0.0429(15) Uani 1 1 d . . . C63B C 0.6211(6) 0.8358(5) -0.4018(6) 0.058(2) Uani 1 1 d . . . H63C H 0.6260 0.7858 -0.4369 0.070 Uiso 1 1 calc R . . H63D H 0.6751 0.8458 -0.3527 0.070 Uiso 1 1 calc R . . C64B C 0.6054(7) 0.8987(7) -0.4852(7) 0.079(3) Uani 1 1 d . . . H64C H 0.6521 0.8993 -0.5257 0.094 Uiso 1 1 calc R . . H64D H 0.6043 0.9491 -0.4498 0.094 Uiso 1 1 calc R . . C65B C 0.5208(8) 0.8858(6) -0.5619(7) 0.084(3) Uani 1 1 d . . . H65C H 0.5245 0.8391 -0.6048 0.101 Uiso 1 1 calc R . . H65D H 0.5087 0.9299 -0.6109 0.101 Uiso 1 1 calc R . . C66B C 0.4484(7) 0.8767(6) -0.4970(8) 0.076(3) Uani 1 1 d . . . H66C H 0.4385 0.9265 -0.4643 0.091 Uiso 1 1 calc R . . H66D H 0.3956 0.8619 -0.5455 0.091 Uiso 1 1 calc R . . C67B C 0.4700(6) 0.8158(5) -0.4096(7) 0.061(2) Uani 1 1 d . . . H67C H 0.4247 0.8142 -0.3669 0.073 Uiso 1 1 calc R . . H67D H 0.4728 0.7647 -0.4427 0.073 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 Cu1 0.0362(6) 0.0329(6) 0.0371(6) -0.0020(5) 0.0092(4) 0.0013(5) C1A 0.059(5) 0.030(4) 0.058(5) -0.006(4) 0.014(4) 0.011(4) O1A 0.042(3) 0.043(3) 0.038(3) -0.007(2) 0.017(2) -0.002(2) C2A 0.037(4) 0.036(4) 0.036(4) -0.001(3) 0.018(3) 0.011(3) C21A 0.045(4) 0.037(4) 0.034(4) 0.005(3) 0.004(3) 0.000(3) N2A 0.030(3) 0.038(3) 0.037(3) 0.007(3) 0.009(2) 0.000(3) C22A 0.049(5) 0.043(4) 0.041(4) -0.003(3) 0.004(3) -0.007(4) C3A 0.039(4) 0.039(4) 0.056(5) 0.001(4) 0.016(4) 0.009(3) C4A 0.034(4) 0.043(4) 0.056(5) -0.004(4) 0.016(3) 0.010(3) C41A 0.051(5) 0.075(6) 0.081(6) -0.006(4) 0.042(4) -0.001(4) C42A 0.092(7) 0.115(8) 0.125(8) -0.043(7) 0.066(6) -0.006(7) C43A 0.111(8) 0.094(7) 0.167(10) 0.004(6) 0.107(8) -0.006(6) C44A 0.085(7) 0.174(11) 0.120(8) -0.004(7) 0.032(6) 0.061(8) C5A 0.017(3) 0.049(5) 0.079(6) 0.001(4) 0.020(3) 0.001(3) C6A 0.038(4) 0.044(4) 0.046(4) -0.003(4) 0.006(3) -0.003(3) C61A 0.052(5) 0.047(5) 0.068(5) -0.012(4) 0.014(4) -0.010(4) N62A 0.047(4) 0.067(5) 0.054(4) -0.008(4) 0.013(3) -0.020(4) C63A 0.104(8) 0.079(7) 0.075(7) -0.033(6) 0.027(6) -0.025(6) C64A 0.109(10) 0.129(11) 0.062(7) -0.045(7) 0.013(6) -0.025(8) C65A 0.087(9) 0.167(14) 0.075(7) -0.020(9) 0.003(6) -0.041(9) C66A 0.054(6) 0.140(11) 0.070(7) -0.001(7) -0.002(5) -0.016(7) C67A 0.047(5) 0.107(9) 0.084(7) -0.003(6) 0.015(5) -0.007(5) C1B 0.036(4) 0.031(4) 0.046(4) 0.011(3) 0.006(3) 0.006(3) O1B 0.034(3) 0.033(3) 0.049(3) 0.001(2) 0.012(2) 0.001(2) C2B 0.032(4) 0.042(4) 0.038(4) -0.001(3) 0.017(3) 0.015(3) C21B 0.054(5) 0.042(4) 0.026(3) -0.001(3) 0.002(3) 0.002(4) N2B 0.042(3) 0.038(3) 0.034(3) -0.002(3) 0.016(3) 0.008(3) C22B 0.043(4) 0.047(5) 0.038(4) -0.011(3) 0.003(3) 0.005(4) C3B 0.041(4) 0.051(5) 0.040(4) 0.005(4) 0.010(3) 0.003(4) C4B 0.042(4) 0.044(4) 0.043(4) -0.003(4) 0.009(3) 0.010(4) C41B 0.034(4) 0.066(6) 0.059(5) -0.005(4) 0.015(4) 0.016(4) C42B 0.070(7) 0.059(6) 0.135(10) 0.011(6) 0.036(7) 0.023(5) C43B 0.040(4) 0.089(7) 0.079(6) 0.001(6) 0.009(4) 0.016(5) C44B 0.061(6) 0.099(8) 0.072(6) -0.009(6) 0.034(5) 0.027(5) C5B 0.057(5) 0.034(4) 0.039(4) -0.001(3) 0.020(4) 0.014(4) C6B 0.041(4) 0.031(4) 0.038(4) 0.000(3) 0.015(3) 0.004(3) C61B 0.048(4) 0.035(4) 0.043(4) -0.001(3) 0.001(3) 0.007(3) N62B 0.053(4) 0.034(3) 0.039(3) -0.003(3) 0.004(3) 0.006(3) C63B 0.067(6) 0.062(6) 0.048(5) 0.003(4) 0.017(4) 0.010(5) C64B 0.093(8) 0.096(8) 0.052(5) 0.020(5) 0.026(5) 0.013(6) C65B 0.137(10) 0.071(7) 0.044(5) 0.003(5) 0.019(6) 0.023(7) C66B 0.087(7) 0.065(6) 0.066(6) 0.002(5) -0.011(5) 0.016(6) C67B 0.066(6) 0.050(5) 0.061(5) -0.002(4) -0.003(4) 0.006(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 O1A 1.881(5) . ? Cu1 O1B 1.896(5) . ? Cu1 N2A 1.909(6) . ? Cu1 N2B 1.921(6) . ? C1A O1A 1.336(9) . ? C1A C2A 1.419(10) . ? C1A C6A 1.437(11) . ? C2A C3A 1.381(9) . ? C2A C21A 1.454(10) . ? C21A N2A 1.291(9) . ? N2A C22A 1.469(9) . ? C22A C22B 1.515(10) . ? C3A C4A 1.368(10) . ? C4A C5A 1.385(11) . ? C4A C41A 1.554(10) . ? C41A C44A 1.493(14) . ? C41A C43A 1.496(14) . ? C41A C42A 1.538(14) . ? C5A C6A 1.376(10) . ? C6A C61A 1.497(11) . ? C61A N62A 1.456(11) . ? N62A C67A 1.473(11) . ? N62A C63A 1.485(11) . ? C63A C64A 1.494(15) . ? C64A C65A 1.489(15) . ? C65A C66A 1.520(16) . ? C66A C67A 1.528(14) . ? C1B O1B 1.331(8) . ? C1B C2B 1.409(10) . ? C1B C6B 1.426(10) . ? C2B C3B 1.399(9) . ? C2B C21B 1.456(9) . ? C21B N2B 1.278(9) . ? N2B C22B 1.479(9) . ? C3B C4B 1.371(10) . ? C4B C5B 1.395(10) . ? C4B C41B 1.537(9) . ? C41B C44B 1.522(12) . ? C41B C42B 1.526(13) . ? C41B C43B 1.531(11) . ? C5B C6B 1.374(9) . ? C6B C61B 1.494(10) . ? C61B N62B 1.474(9) . ? N62B C67B 1.446(9) . ? N62B C63B 1.482(10) . ? C63B C64B 1.505(12) . ? C64B C65B 1.527(14) . ? C65B C66B 1.545(15) . ? C66B C67B 1.521(12) . ? 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 O1A Cu1 O1B 91.37(19) . . ? O1A Cu1 N2A 92.9(2) . . ? O1B Cu1 N2A 170.0(2) . . ? O1A Cu1 N2B 171.0(2) . . ? O1B Cu1 N2B 92.9(2) . . ? N2A Cu1 N2B 84.1(2) . . ? O1A C1A C2A 124.2(7) . . ? O1A C1A C6A 119.0(7) . . ? C2A C1A C6A 116.8(7) . . ? C1A O1A Cu1 127.7(5) . . ? C3A C2A C1A 120.7(7) . . ? C3A C2A C21A 117.4(6) . . ? C1A C2A C21A 121.9(6) . . ? N2A C21A C2A 124.1(7) . . ? C21A N2A C22A 117.9(6) . . ? C21A N2A Cu1 128.4(5) . . ? C22A N2A Cu1 113.7(4) . . ? N2A C22A C22B 107.2(6) . . ? C4A C3A C2A 123.1(7) . . ? C3A C4A C5A 116.1(7) . . ? C3A C4A C41A 122.6(7) . . ? C5A C4A C41A 121.2(7) . . ? C44A C41A C43A 110.0(10) . . ? C44A C41A C42A 108.1(10) . . ? C43A C41A C42A 108.5(9) . . ? C44A C41A C4A 109.1(8) . . ? C43A C41A C4A 109.3(8) . . ? C42A C41A C4A 111.9(8) . . ? C6A C5A C4A 124.8(7) . . ? C5A C6A C1A 118.3(7) . . ? C5A C6A C61A 123.6(7) . . ? C1A C6A C61A 118.0(7) . . ? N62A C61A C6A 112.9(7) . . ? C61A N62A C67A 110.4(7) . . ? C61A N62A C63A 110.6(7) . . ? C67A N62A C63A 109.4(7) . . ? N62A C63A C64A 110.1(9) . . ? C65A C64A C63A 112.0(11) . . ? C64A C65A C66A 110.0(9) . . ? C65A C66A C67A 109.0(11) . . ? N62A C67A C66A 113.2(8) . . ? O1B C1B C2B 124.7(6) . . ? O1B C1B C6B 118.7(6) . . ? C2B C1B C6B 116.6(6) . . ? C1B O1B Cu1 127.6(4) . . ? C3B C2B C1B 121.2(7) . . ? C3B C2B C21B 117.1(7) . . ? C1B C2B C21B 121.6(6) . . ? N2B C21B C2B 125.5(7) . . ? C21B N2B C22B 118.5(6) . . ? C21B N2B Cu1 127.5(5) . . ? C22B N2B Cu1 113.9(4) . . ? N2B C22B C22A 107.1(6) . . ? C4B C3B C2B 122.6(7) . . ? C3B C4B C5B 115.4(6) . . ? C3B C4B C41B 123.9(7) . . ? C5B C4B C41B 120.7(7) . . ? C44B C41B C42B 109.2(8) . . ? C44B C41B C43B 107.7(7) . . ? C42B C41B C43B 109.6(8) . . ? C44B C41B C4B 110.0(7) . . ? C42B C41B C4B 108.7(7) . . ? C43B C41B C4B 111.6(7) . . ? C6B C5B C4B 125.1(7) . . ? C5B C6B C1B 118.8(6) . . ? C5B C6B C61B 120.9(6) . . ? C1B C6B C61B 120.4(6) . . ? N62B C61B C6B 113.5(6) . . ? C67B N62B C61B 109.0(6) . . ? C67B N62B C63B 111.2(6) . . ? C61B N62B C63B 110.0(6) . . ? N62B C63B C64B 111.0(7) . . ? C63B C64B C65B 110.9(9) . . ? C64B C65B C66B 109.4(8) . . ? C67B C66B C65B 111.6(8) . . ? N62B C67B C66B 111.4(8) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 60.13 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.785 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.098 #===END data_compoundCu1SO4 _database_code_CSD 197889 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H50 Cu N4 O4.SO4.2C2H5OH.1/2H2O' _chemical_formula_sum 'C38 H63 Cu N4 O10.50 S' _chemical_formula_weight 839.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.2663(7) _cell_length_b 14.7419(11) _cell_length_c 17.4166(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.663(4) _cell_angle_gamma 90.00 _cell_volume 4148.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.2399 _exptl_absorpt_correction_T_max 0.3336 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 8344 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 60.09 _reflns_number_total 6083 _reflns_number_gt 4819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'sir92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+3.3932P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric and difmap' _refine_ls_hydrogen_treatment 'riding and freely refined' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6083 _refine_ls_number_parameters 506 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.019 _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 Cu1 Cu 0.49203(3) -0.61026(3) 1.40906(2) 0.03328(16) Uani 1 1 d . . . C1A C 0.65966(19) -0.5481(2) 1.45106(18) 0.0339(7) Uani 1 1 d . . . O1A O 0.59436(13) -0.55198(15) 1.39980(12) 0.0374(5) Uani 1 1 d . . . C2A C 0.6610(2) -0.5740(2) 1.52954(18) 0.0365(7) Uani 1 1 d . . . C21A C 0.5896(2) -0.6111(2) 1.55949(19) 0.0391(8) Uani 1 1 d . . . H21A H 0.5943 -0.6235 1.6128 0.047 Uiso 1 1 calc R . . N2A N 0.51969(16) -0.62908(18) 1.51989(15) 0.0369(6) Uani 1 1 d . . . C22A C 0.4500(2) -0.6627(3) 1.55887(19) 0.0429(8) Uani 1 1 d . . . H22A H 0.4237 -0.6120 1.5829 0.052 Uiso 1 1 calc R . . H22B H 0.4705 -0.7057 1.5996 0.052 Uiso 1 1 calc R . . C3A C 0.7342(2) -0.5633(2) 1.58087(19) 0.0404(8) Uani 1 1 d . . . H3A H 0.7337 -0.5810 1.6327 0.048 Uiso 1 1 calc R . . C4A C 0.8060(2) -0.5284(2) 1.55870(18) 0.0383(8) Uani 1 1 d . . . C41A C 0.8860(2) -0.5165(3) 1.6136(2) 0.0439(8) Uani 1 1 d . . . C42A C 0.8726(3) -0.5390(3) 1.6973(2) 0.0570(10) Uani 1 1 d . . . H42A H 0.8544 -0.6015 1.7002 0.086 Uiso 1 1 calc R . . H42B H 0.8308 -0.4990 1.7139 0.086 Uiso 1 1 calc R . . H42C H 0.9242 -0.5309 1.7306 0.086 Uiso 1 1 calc R . . C43A C 0.9149(2) -0.4175(3) 1.6109(2) 0.0507(9) Uani 1 1 d . . . H43A H 0.9656 -0.4098 1.6455 0.076 Uiso 1 1 calc R . . H43B H 0.8725 -0.3778 1.6268 0.076 Uiso 1 1 calc R . . H43C H 0.9249 -0.4024 1.5585 0.076 Uiso 1 1 calc R . . C44A C 0.9538(2) -0.5791(3) 1.5889(3) 0.0637(11) Uani 1 1 d . . . H44A H 0.9355 -0.6417 1.5903 0.095 Uiso 1 1 calc R . . H44B H 1.0041 -0.5714 1.6240 0.095 Uiso 1 1 calc R . . H44C H 0.9644 -0.5638 1.5368 0.095 Uiso 1 1 calc R . . C5A C 0.8041(2) -0.5050(2) 1.48010(18) 0.0383(8) Uani 1 1 d . . . H5A H 0.8525 -0.4817 1.4629 0.046 Uiso 1 1 calc R . . C6A C 0.7346(2) -0.5147(2) 1.42699(18) 0.0354(7) Uani 1 1 d . . . C61A C 0.7343(2) -0.4875(2) 1.34386(18) 0.0370(7) Uani 1 1 d . . . H61A H 0.7754 -0.4395 1.3408 0.044 Uiso 1 1 calc R . . H61B H 0.6799 -0.4620 1.3255 0.044 Uiso 1 1 calc R . . N62A N 0.75265(17) -0.5639(2) 1.29013(16) 0.0400(7) Uani 1 1 d . . . H62A H 0.734(2) -0.537(3) 1.242(2) 0.061(12) Uiso 1 1 d . . . C63A C 0.8428(2) -0.5884(3) 1.2983(2) 0.0559(10) Uani 1 1 d . . . H63A H 0.8758 -0.5347 1.2891 0.067 Uiso 1 1 calc R . . H63B H 0.8601 -0.6100 1.3509 0.067 Uiso 1 1 calc R . . C64A C 0.8572(3) -0.6609(4) 1.2413(3) 0.0775(14) Uani 1 1 d . . . H64A H 0.8431 -0.6374 1.1888 0.093 Uiso 1 1 calc R . . H64B H 0.9159 -0.6774 1.2474 0.093 Uiso 1 1 calc R . . O65A O 0.8090(3) -0.7392(2) 1.2514(2) 0.0986(12) Uani 1 1 d . . . C66A C 0.7240(3) -0.7174(4) 1.2395(3) 0.0830(16) Uani 1 1 d . . . H66A H 0.6912 -0.7723 1.2447 0.100 Uiso 1 1 calc R . . H66B H 0.7102 -0.6940 1.1869 0.100 Uiso 1 1 calc R . . C67A C 0.7018(3) -0.6469(3) 1.2971(2) 0.0536(10) Uani 1 1 d . . . H67A H 0.6428 -0.6317 1.2869 0.064 Uiso 1 1 calc R . . H67B H 0.7122 -0.6712 1.3497 0.064 Uiso 1 1 calc R . . C1B C 0.38961(19) -0.6084(2) 1.26255(18) 0.0351(7) Uani 1 1 d . . . O1B O 0.46013(13) -0.58770(16) 1.30261(12) 0.0396(5) Uani 1 1 d . . . C2B C 0.32128(19) -0.6483(2) 1.29404(18) 0.0359(7) Uani 1 1 d . . . C21B C 0.3255(2) -0.6758(2) 1.37368(19) 0.0372(8) Uani 1 1 d . . . H21B H 0.2777 -0.7018 1.3900 0.045 Uiso 1 1 calc R . . N2B N 0.38892(16) -0.66783(18) 1.42442(14) 0.0348(6) Uani 1 1 d . . . C22B C 0.3876(2) -0.7090(3) 1.50121(18) 0.0433(8) Uani 1 1 d . . . H22C H 0.4006 -0.7738 1.4988 0.052 Uiso 1 1 calc R . . H22D H 0.3322 -0.7030 1.5175 0.052 Uiso 1 1 calc R . . C3B C 0.24748(19) -0.6658(2) 1.24622(19) 0.0376(8) Uani 1 1 d . . . H3B H 0.2034 -0.6928 1.2684 0.045 Uiso 1 1 calc R . . C4B C 0.2363(2) -0.6455(2) 1.16851(19) 0.0379(8) Uani 1 1 d . . . C41B C 0.1539(2) -0.6585(3) 1.1171(2) 0.0430(8) Uani 1 1 d . . . C42B C 0.0865(2) -0.6943(3) 1.1633(2) 0.0622(11) Uani 1 1 d . . . H42D H 0.0787 -0.6522 1.2046 0.093 Uiso 1 1 calc R . . H42E H 0.1029 -0.7530 1.1852 0.093 Uiso 1 1 calc R . . H42F H 0.0351 -0.7005 1.1295 0.093 Uiso 1 1 calc R . . C43B C 0.1654(2) -0.7252(3) 1.0515(2) 0.0644(12) Uani 1 1 d . . . H43D H 0.1836 -0.7833 1.0733 0.097 Uiso 1 1 calc R . . H43E H 0.2067 -0.7016 1.0208 0.097 Uiso 1 1 calc R . . H43F H 0.1133 -0.7327 1.0190 0.097 Uiso 1 1 calc R . . C44B C 0.1263(2) -0.5666(3) 1.0822(2) 0.0568(10) Uani 1 1 d . . . H44D H 0.1190 -0.5241 1.1233 0.085 Uiso 1 1 calc R . . H44E H 0.0743 -0.5737 1.0493 0.085 Uiso 1 1 calc R . . H44F H 0.1681 -0.5437 1.0517 0.085 Uiso 1 1 calc R . . C5B C 0.30559(19) -0.6098(2) 1.13716(18) 0.0348(7) Uani 1 1 d . . . H5B H 0.3008 -0.5971 1.0839 0.042 Uiso 1 1 calc R . . C6B C 0.38003(19) -0.5925(2) 1.18113(18) 0.0337(7) Uani 1 1 d . . . C61B C 0.45377(19) -0.5624(2) 1.14315(18) 0.0332(7) Uani 1 1 d . . . H61C H 0.4484 -0.5871 1.0906 0.040 Uiso 1 1 calc R . . H61D H 0.5035 -0.5892 1.1715 0.040 Uiso 1 1 calc R . . N62B N 0.46685(16) -0.46164(18) 1.13834(15) 0.0325(6) Uani 1 1 d . . . H62B H 0.512(2) -0.456(3) 1.113(2) 0.056(11) Uiso 1 1 d . . . C63B C 0.4873(2) -0.4150(2) 1.21401(19) 0.0410(8) Uani 1 1 d . . . H63C H 0.5354 -0.4440 1.2432 0.049 Uiso 1 1 calc R . . H63D H 0.4405 -0.4193 1.2445 0.049 Uiso 1 1 calc R . . C64B C 0.5063(2) -0.3165(2) 1.1992(2) 0.0517(9) Uani 1 1 d . . . H64C H 0.5193 -0.2852 1.2487 0.062 Uiso 1 1 calc R . . H64D H 0.5552 -0.3129 1.1712 0.062 Uiso 1 1 calc R . . O65B O 0.43903(17) -0.27198(17) 1.15550(17) 0.0593(7) Uani 1 1 d . . . C66B C 0.4192(2) -0.3162(2) 1.0832(2) 0.0524(10) Uani 1 1 d . . . H66C H 0.4669 -0.3129 1.0537 0.063 Uiso 1 1 calc R . . H66D H 0.3729 -0.2845 1.0536 0.063 Uiso 1 1 calc R . . C67B C 0.3962(2) -0.4141(2) 1.0930(2) 0.0416(8) Uani 1 1 d . . . H67C H 0.3468 -0.4181 1.1202 0.050 Uiso 1 1 calc R . . H67D H 0.3837 -0.4429 1.0423 0.050 Uiso 1 1 calc R . . S2 S 0.67602(5) -0.45352(6) 1.09901(5) 0.0381(2) Uani 1 1 d . . . O1S O 0.59360(14) -0.43594(18) 1.05506(13) 0.0467(6) Uani 1 1 d . A . O2S O 0.6631(2) -0.5206(3) 1.1608(2) 0.0479(9) Uani 0.75 1 d P A 1 O3S O 0.7313(2) -0.4921(3) 1.0477(2) 0.0509(10) Uani 0.75 1 d P A 1 O4S O 0.7107(3) -0.3692(3) 1.1347(3) 0.0663(12) Uani 0.75 1 d P A 1 O2SA O 0.7233(10) -0.3752(12) 1.0967(9) 0.073(5) Uiso 0.25 1 d P A 2 O3SA O 0.6619(8) -0.4776(9) 1.1731(8) 0.051(4) Uiso 0.25 1 d P A 2 O4SA O 0.7187(11) -0.5276(12) 1.0654(11) 0.080(6) Uiso 0.25 1 d P A 2 O1C O 0.8607(11) -0.7261(12) 0.9553(9) 0.217(6) Uiso 0.50 1 d PD B 1 C2C C 0.8490(9) -0.6812(11) 1.0279(8) 0.112(4) Uiso 0.50 1 d PD B 1 H2C1 H 0.8700 -0.7206 1.0711 0.134 Uiso 0.50 1 calc PR B 1 H2C2 H 0.8813 -0.6249 1.0322 0.134 Uiso 0.50 1 calc PR B 1 C3C C 0.7646(10) -0.6606(12) 1.0334(11) 0.109(6) Uiso 0.50 1 d PD B 1 H3C1 H 0.7606 -0.6230 1.0785 0.163 Uiso 0.50 1 calc PR B 1 H3C2 H 0.7340 -0.7164 1.0381 0.163 Uiso 0.50 1 calc PR B 1 H3C3 H 0.7415 -0.6283 0.9874 0.163 Uiso 0.50 1 calc PR B 1 O1D O 0.7502(5) -0.6818(6) 1.0466(5) 0.078(3) Uiso 0.50 1 d PD C 2 C2D C 0.7959(8) -0.7035(11) 0.9874(8) 0.121(5) Uiso 0.50 1 d PD C 2 H2D1 H 0.7671 -0.6798 0.9389 0.145 Uiso 0.50 1 calc PR C 2 H2D2 H 0.7977 -0.7697 0.9828 0.145 Uiso 0.50 1 calc PR C 2 C3D C 0.8810(9) -0.6690(12) 0.9959(11) 0.134(5) Uiso 0.50 1 d PD C 2 H3D1 H 0.9118 -0.6984 0.9585 0.201 Uiso 0.50 1 calc PR C 2 H3D2 H 0.9070 -0.6819 1.0477 0.201 Uiso 0.50 1 calc PR C 2 H3D3 H 0.8803 -0.6040 0.9872 0.201 Uiso 0.50 1 calc PR C 2 O1E O 0.8537(3) -0.3783(4) 1.2221(3) 0.0445(16) Uiso 0.50 1 d PD D 1 C2E C 0.9163(6) -0.3610(7) 1.1782(5) 0.068(2) Uiso 0.50 1 d PD D 1 H2E1 H 0.9657 -0.3424 1.2121 0.082 Uiso 0.50 1 calc PR D 1 H2E2 H 0.9001 -0.3105 1.1431 0.082 Uiso 0.50 1 calc PR D 1 C3E C 0.9374(6) -0.4422(6) 1.1313(6) 0.067(2) Uiso 0.50 1 d PD D 1 H3E1 H 0.9806 -0.4259 1.0999 0.100 Uiso 0.50 1 calc PR D 1 H3E2 H 0.8886 -0.4615 1.0980 0.100 Uiso 0.50 1 calc PR D 1 H3E3 H 0.9565 -0.4914 1.1659 0.100 Uiso 0.50 1 calc PR D 1 O1F O 0.9666(8) -0.3466(8) 1.1501(7) 0.165(4) Uiso 0.50 1 d PD E 2 C2F C 0.9137(6) -0.4240(8) 1.1607(6) 0.078(3) Uiso 0.50 1 d PD E 2 H2F1 H 0.8821 -0.4387 1.1109 0.093 Uiso 0.50 1 calc PR E 2 H2F2 H 0.9489 -0.4763 1.1763 0.093 Uiso 0.50 1 calc PR E 2 C3F C 0.8570(5) -0.4108(7) 1.2167(5) 0.048(2) Uiso 0.50 1 d PD E 2 H3F1 H 0.8228 -0.4644 1.2189 0.072 Uiso 0.50 1 calc PR E 2 H3F2 H 0.8220 -0.3588 1.2022 0.072 Uiso 0.50 1 calc PR E 2 H3F3 H 0.8876 -0.4002 1.2671 0.072 Uiso 0.50 1 calc PR E 2 O1W O 0.6069(9) -0.6935(11) 1.0992(9) 0.213(6) Uiso 0.50 1 d P . . 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 0.0325(3) 0.0375(3) 0.0297(3) 0.0047(2) 0.00289(18) -0.0028(2) C1A 0.0345(17) 0.0344(18) 0.0319(17) -0.0028(14) 0.0008(14) -0.0014(14) O1A 0.0349(12) 0.0469(14) 0.0297(11) 0.0031(10) 0.0010(9) -0.0054(10) C2A 0.0402(18) 0.0376(18) 0.0318(17) 0.0004(14) 0.0047(14) -0.0021(14) C21A 0.046(2) 0.0416(19) 0.0304(17) -0.0002(15) 0.0054(15) 0.0002(16) N2A 0.0384(15) 0.0405(16) 0.0328(14) 0.0006(12) 0.0083(12) -0.0038(12) C22A 0.0432(19) 0.051(2) 0.0353(18) 0.0052(16) 0.0080(15) -0.0035(16) C3A 0.045(2) 0.045(2) 0.0299(17) -0.0011(15) -0.0015(15) -0.0008(16) C4A 0.0401(19) 0.0403(19) 0.0332(17) -0.0048(15) -0.0010(14) -0.0026(15) C41A 0.0398(19) 0.052(2) 0.0376(19) -0.0015(16) -0.0051(15) -0.0012(16) C42A 0.059(2) 0.066(3) 0.041(2) 0.0050(19) -0.0125(18) -0.009(2) C43A 0.047(2) 0.054(2) 0.048(2) -0.0058(18) -0.0078(17) -0.0086(18) C44A 0.052(2) 0.065(3) 0.070(3) -0.009(2) -0.011(2) 0.011(2) C5A 0.0369(18) 0.041(2) 0.0369(18) -0.0034(15) 0.0027(14) -0.0053(15) C6A 0.0358(17) 0.0371(18) 0.0328(17) -0.0017(14) 0.0018(14) -0.0033(14) C61A 0.0356(18) 0.0424(19) 0.0328(17) 0.0016(15) 0.0032(14) -0.0058(14) N62A 0.0387(15) 0.0494(18) 0.0323(15) 0.0012(14) 0.0052(12) -0.0043(13) C63A 0.044(2) 0.074(3) 0.051(2) -0.003(2) 0.0078(17) 0.0064(19) C64A 0.068(3) 0.092(4) 0.077(3) -0.014(3) 0.027(3) 0.013(3) O65A 0.124(3) 0.071(2) 0.109(3) -0.024(2) 0.050(3) 0.013(2) C66A 0.104(4) 0.072(3) 0.080(3) -0.034(3) 0.042(3) -0.027(3) C67A 0.064(2) 0.051(2) 0.048(2) -0.0097(18) 0.0169(18) -0.0143(19) C1B 0.0332(17) 0.0333(18) 0.0380(18) 0.0052(14) 0.0007(14) 0.0006(14) O1B 0.0334(12) 0.0494(14) 0.0345(12) 0.0112(10) -0.0020(9) -0.0081(10) C2B 0.0320(17) 0.0387(18) 0.0371(18) 0.0050(15) 0.0051(14) 0.0011(14) C21B 0.0327(17) 0.0379(19) 0.0417(19) 0.0033(15) 0.0082(15) -0.0035(14) N2B 0.0348(15) 0.0375(16) 0.0324(14) 0.0063(12) 0.0050(12) -0.0010(12) C22B 0.0433(19) 0.053(2) 0.0345(18) 0.0099(16) 0.0089(15) -0.0062(16) C3B 0.0326(17) 0.0414(19) 0.0396(18) 0.0033(15) 0.0071(14) -0.0031(14) C4B 0.0334(17) 0.0408(19) 0.0396(18) -0.0026(15) 0.0042(14) -0.0018(14) C41B 0.0313(17) 0.056(2) 0.0412(19) -0.0011(17) 0.0003(14) -0.0046(16) C42B 0.039(2) 0.089(3) 0.057(2) 0.007(2) -0.0026(18) -0.016(2) C43B 0.047(2) 0.081(3) 0.063(3) -0.023(2) -0.0044(19) -0.005(2) C44B 0.043(2) 0.072(3) 0.053(2) 0.008(2) -0.0019(17) 0.0061(19) C5B 0.0372(17) 0.0347(18) 0.0320(16) 0.0006(14) 0.0021(13) 0.0012(14) C6B 0.0310(17) 0.0332(18) 0.0372(18) 0.0013(14) 0.0054(14) -0.0001(13) C61B 0.0342(17) 0.0317(18) 0.0339(17) -0.0002(14) 0.0045(13) 0.0000(13) N62B 0.0328(14) 0.0334(15) 0.0324(14) 0.0015(11) 0.0076(12) -0.0010(11) C63B 0.050(2) 0.0410(19) 0.0328(17) -0.0050(15) 0.0062(15) -0.0055(16) C64B 0.064(2) 0.043(2) 0.048(2) -0.0081(17) 0.0060(18) -0.0074(18) O65B 0.0635(17) 0.0354(14) 0.0786(19) -0.0041(14) 0.0062(14) 0.0070(13) C66B 0.052(2) 0.040(2) 0.064(3) 0.0120(19) 0.0010(19) 0.0049(17) C67B 0.0374(18) 0.043(2) 0.0435(19) 0.0069(16) 0.0002(15) 0.0007(15) S2 0.0326(4) 0.0455(5) 0.0360(4) 0.0016(4) 0.0032(3) 0.0007(4) O1S 0.0343(12) 0.0654(17) 0.0401(13) 0.0104(12) 0.0033(10) 0.0044(11) O2S 0.047(2) 0.055(3) 0.040(2) 0.009(2) -0.0016(15) -0.0048(19) O3S 0.0347(19) 0.081(3) 0.038(2) 0.001(2) 0.0124(15) 0.0062(19) O4S 0.051(2) 0.049(2) 0.094(4) -0.024(2) -0.008(2) -0.0010(17) _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 O1B 1.896(2) . ? Cu1 O1A 1.897(2) . ? Cu1 N2B 1.926(3) . ? Cu1 N2A 1.950(3) . ? C1A O1A 1.307(4) . ? C1A C2A 1.417(4) . ? C1A C6A 1.422(4) . ? C2A C3A 1.412(5) . ? C2A C21A 1.436(5) . ? C21A N2A 1.287(4) . ? N2A C22A 1.473(4) . ? C22A C22B 1.507(5) . ? C3A C4A 1.373(5) . ? C4A C5A 1.408(5) . ? C4A C41A 1.532(5) . ? C41A C43A 1.535(5) . ? C41A C42A 1.535(5) . ? C41A C44A 1.538(5) . ? C5A C6A 1.383(4) . ? C6A C61A 1.502(4) . ? C61A N62A 1.515(4) . ? N62A C67A 1.490(5) . ? N62A C63A 1.501(5) . ? C63A C64A 1.496(6) . ? C64A O65A 1.418(6) . ? O65A C66A 1.411(6) . ? C66A C67A 1.517(6) . ? C1B O1B 1.308(4) . ? C1B C2B 1.423(4) . ? C1B C6B 1.428(4) . ? C2B C3B 1.403(5) . ? C2B C21B 1.439(4) . ? C21B N2B 1.283(4) . ? N2B C22B 1.471(4) . ? C3B C4B 1.377(5) . ? C4B C5B 1.410(4) . ? C4B C41B 1.536(5) . ? C41B C42B 1.527(5) . ? C41B C44B 1.531(5) . ? C41B C43B 1.534(5) . ? C5B C6B 1.379(4) . ? C6B C61B 1.503(4) . ? C61B N62B 1.504(4) . ? N62B C63B 1.489(4) . ? N62B C67B 1.492(4) . ? C63B C64B 1.514(5) . ? C64B O65B 1.419(5) . ? O65B C66B 1.422(5) . ? C66B C67B 1.506(5) . ? S2 O3SA 1.383(13) . ? S2 O2SA 1.391(17) . ? S2 O4SA 1.453(19) . ? S2 O3S 1.455(4) . ? S2 O4S 1.472(4) . ? S2 O1S 1.487(2) . ? S2 O2S 1.494(4) . ? O1C C2C 1.459(15) . ? C2C C3C 1.421(15) . ? O1D C2D 1.378(14) . ? C2D C3D 1.465(15) . ? O1E C2E 1.367(10) . ? C2E C3E 1.511(11) . ? O1F C2F 1.453(13) . ? C2F C3F 1.433(12) . ? 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 O1B Cu1 O1A 88.90(9) . . ? O1B Cu1 N2B 93.97(10) . . ? O1A Cu1 N2B 176.85(10) . . ? O1B Cu1 N2A 176.76(11) . . ? O1A Cu1 N2A 92.56(10) . . ? N2B Cu1 N2A 84.51(11) . . ? O1A C1A C2A 124.6(3) . . ? O1A C1A C6A 118.1(3) . . ? C2A C1A C6A 117.4(3) . . ? C1A O1A Cu1 127.8(2) . . ? C3A C2A C1A 119.9(3) . . ? C3A C2A C21A 118.1(3) . . ? C1A C2A C21A 122.1(3) . . ? N2A C21A C2A 125.8(3) . . ? C21A N2A C22A 120.1(3) . . ? C21A N2A Cu1 126.1(2) . . ? C22A N2A Cu1 113.7(2) . . ? N2A C22A C22B 109.9(3) . . ? C4A C3A C2A 123.1(3) . . ? C3A C4A C5A 116.2(3) . . ? C3A C4A C41A 123.8(3) . . ? C5A C4A C41A 120.0(3) . . ? C4A C41A C43A 109.3(3) . . ? C4A C41A C42A 111.4(3) . . ? C43A C41A C42A 108.2(3) . . ? C4A C41A C44A 109.9(3) . . ? C43A C41A C44A 109.3(3) . . ? C42A C41A C44A 108.7(3) . . ? C6A C5A C4A 123.3(3) . . ? C5A C6A C1A 120.1(3) . . ? C5A C6A C61A 121.9(3) . . ? C1A C6A C61A 118.0(3) . . ? C6A C61A N62A 114.7(3) . . ? C67A N62A C63A 109.9(3) . . ? C67A N62A C61A 114.1(3) . . ? C63A N62A C61A 112.3(3) . . ? C64A C63A N62A 109.6(3) . . ? O65A C64A C63A 111.6(4) . . ? C66A O65A C64A 110.0(4) . . ? O65A C66A C67A 111.4(4) . . ? N62A C67A C66A 109.3(3) . . ? O1B C1B C2B 124.5(3) . . ? O1B C1B C6B 118.7(3) . . ? C2B C1B C6B 116.8(3) . . ? C1B O1B Cu1 127.2(2) . . ? C3B C2B C1B 120.0(3) . . ? C3B C2B C21B 117.5(3) . . ? C1B C2B C21B 122.4(3) . . ? N2B C21B C2B 125.7(3) . . ? C21B N2B C22B 119.5(3) . . ? C21B N2B Cu1 126.0(2) . . ? C22B N2B Cu1 114.4(2) . . ? N2B C22B C22A 109.8(3) . . ? C4B C3B C2B 123.3(3) . . ? C3B C4B C5B 116.2(3) . . ? C3B C4B C41B 123.6(3) . . ? C5B C4B C41B 120.2(3) . . ? C42B C41B C44B 108.7(3) . . ? C42B C41B C43B 109.2(3) . . ? C44B C41B C43B 109.1(3) . . ? C42B C41B C4B 111.5(3) . . ? C44B C41B C4B 108.5(3) . . ? C43B C41B C4B 109.9(3) . . ? C6B C5B C4B 122.9(3) . . ? C5B C6B C1B 120.6(3) . . ? C5B C6B C61B 120.3(3) . . ? C1B C6B C61B 119.0(3) . . ? C6B C61B N62B 116.2(3) . . ? C63B N62B C67B 109.3(3) . . ? C63B N62B C61B 115.1(2) . . ? C67B N62B C61B 112.8(3) . . ? N62B C63B C64B 108.7(3) . . ? O65B C64B C63B 112.0(3) . . ? C64B O65B C66B 110.2(3) . . ? O65B C66B C67B 111.9(3) . . ? N62B C67B C66B 108.9(3) . . ? O3SA S2 O2SA 113.1(8) . . ? O3SA S2 O4SA 108.8(9) . . ? O2SA S2 O4SA 108.7(9) . . ? O3SA S2 O3S 130.9(6) . . ? O2SA S2 O3S 85.6(7) . . ? O4SA S2 O3S 25.9(6) . . ? O3SA S2 O4S 85.4(6) . . ? O2SA S2 O4S 28.9(6) . . ? O4SA S2 O4S 128.8(7) . . ? O3S S2 O4S 110.8(3) . . ? O3SA S2 O1S 106.7(6) . . ? O2SA S2 O1S 108.0(7) . . ? O4SA S2 O1S 111.6(7) . . ? O3S S2 O1S 109.64(18) . . ? O4S S2 O1S 110.4(2) . . ? O3SA S2 O2S 26.6(5) . . ? O2SA S2 O2S 134.1(7) . . ? O4SA S2 O2S 84.6(7) . . ? O3S S2 O2S 109.4(3) . . ? O4S S2 O2S 109.6(3) . . ? O1S S2 O2S 106.98(17) . . ? C3C C2C O1C 112.4(15) . . ? O1D C2D C3D 115.4(14) . . ? O1E C2E C3E 112.7(9) . . ? C3F C2F O1F 114.6(11) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 60.09 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.463 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.053 #===END data_compoundNi5SO4 _database_code_CSD 197890 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [NiL(SO4)].4CH2Cl2 _chemical_formula_sum 'C50 H66 Cl8 N4 Ni O6 S' _chemical_formula_weight 1193.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'y, x, -z' 'x+1/2, -y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 18.1205(16) _cell_length_b 18.1205(16) _cell_length_c 35.052(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11510(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4976 _exptl_absorpt_coefficient_mu 4.636 _exptl_absorpt_correction_type 'Gaussian integration' _exptl_absorpt_correction_T_min 0.397 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 8454 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.2284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 60.00 _reflns_number_total 8317 _reflns_number_gt 3283 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four molecules of CH2Cl2 were clearly visible in difference maps, although they were badly disordered. This region was therefore treated in the manner descibed by van der Sluis and Spek (1346 e/cell). ; _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^)+(0.1326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(7) _refine_ls_number_reflns 8317 _refine_ls_number_parameters 523 _refine_ls_number_restraints 555 _refine_ls_R_factor_all 0.1955 _refine_ls_R_factor_gt 0.1069 _refine_ls_wR_factor_ref 0.2957 _refine_ls_wR_factor_gt 0.2389 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.906 _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 Ni1 Ni 0.13987(10) 0.49865(11) 0.03967(5) 0.0318(5) Uani 1 1 d U . . S1S S 0.04416(18) 0.60877(17) 0.05470(10) 0.0402(8) Uani 1 1 d U . . O1S O 0.0742(4) 0.5830(4) 0.01591(19) 0.0360(18) Uani 1 1 d U . . O2S O 0.0861(4) 0.5592(4) 0.0820(2) 0.0357(17) Uani 1 1 d U . . O3S O -0.0347(5) 0.5932(5) 0.0581(2) 0.053(2) Uani 1 1 d U . . O4S O 0.0572(5) 0.6860(4) 0.0605(2) 0.048(2) Uani 1 1 d U . . C1A C 0.2053(7) 0.5095(7) -0.0369(4) 0.041(3) Uani 1 1 d U . . O1A O 0.1720(4) 0.4653(4) -0.01103(18) 0.0314(17) Uani 1 1 d U . . C2A C 0.2505(7) 0.5670(7) -0.0276(4) 0.047(3) Uani 1 1 d U . . C21A C 0.2697(7) 0.5909(7) 0.0131(4) 0.049(3) Uani 1 1 d U . . H21A H 0.3108 0.6225 0.0174 0.059 Uiso 1 1 calc R . . N2A N 0.2307(5) 0.5687(5) 0.0416(3) 0.034(2) Uani 1 1 d U . . C22A C 0.2530(6) 0.5865(7) 0.0797(4) 0.039(3) Uani 1 1 d U . . C23A C 0.2330(6) 0.6556(6) 0.0927(4) 0.036(3) Uani 1 1 d U . . H23A H 0.2038 0.6884 0.0779 0.043 Uiso 1 1 calc R . . C24A C 0.2597(7) 0.6745(7) 0.1306(4) 0.041(3) Uani 1 1 d U . . H24A H 0.2437 0.7191 0.1422 0.049 Uiso 1 1 calc R . . C25A C 0.3062(7) 0.6304(8) 0.1495(4) 0.056(3) Uani 1 1 d U . . H25A H 0.3254 0.6462 0.1734 0.067 Uiso 1 1 calc R . . C26A C 0.3283(7) 0.5585(7) 0.1344(4) 0.048(3) Uani 1 1 d U . . H26A H 0.3589 0.5261 0.1487 0.058 Uiso 1 1 calc R . . C27A C 0.3017(6) 0.5389(7) 0.0969(4) 0.038(3) Uani 1 1 d U . . C3A C 0.2875(8) 0.6106(7) -0.0557(4) 0.049(3) Uani 1 1 d U . . H3A H 0.3208 0.6485 -0.0483 0.059 Uiso 1 1 calc R . . C4A C 0.2738(7) 0.5962(8) -0.0940(4) 0.049(3) Uani 1 1 d U . . C41A C 0.3132(9) 0.6433(9) -0.1231(4) 0.062(4) Uani 1 1 d U . . C42A C 0.2947(11) 0.7321(9) -0.1128(5) 0.091(5) Uani 1 1 d U . . H42A H 0.2414 0.7404 -0.1141 0.136 Uiso 1 1 calc R . . H42B H 0.3197 0.7640 -0.1313 0.136 Uiso 1 1 calc R . . H42C H 0.3125 0.7435 -0.0871 0.136 Uiso 1 1 calc R . . C43A C 0.2841(9) 0.6327(8) -0.1627(3) 0.068(4) Uani 1 1 d U . . H43A H 0.2301 0.6352 -0.1623 0.103 Uiso 1 1 calc R . . H43B H 0.2997 0.5844 -0.1723 0.103 Uiso 1 1 calc R . . H43C H 0.3036 0.6715 -0.1793 0.103 Uiso 1 1 calc R . . C44A C 0.3930(9) 0.6425(11) -0.1215(5) 0.096(6) Uani 1 1 d U . . H44A H 0.4092 0.6512 -0.0952 0.144 Uiso 1 1 calc R . . H44B H 0.4127 0.6813 -0.1381 0.144 Uiso 1 1 calc R . . H44C H 0.4112 0.5944 -0.1301 0.144 Uiso 1 1 calc R . . C5A C 0.2300(7) 0.5393(7) -0.1027(4) 0.044(3) Uani 1 1 d U . . H5A H 0.2212 0.5293 -0.1289 0.053 Uiso 1 1 calc R . . C6A C 0.1961(7) 0.4933(8) -0.0755(4) 0.045(3) Uani 1 1 d U . . C61A C 0.1507(7) 0.4276(7) -0.0876(4) 0.042(3) Uani 1 1 d U . . H61A H 0.1782 0.3816 -0.0820 0.051 Uiso 1 1 calc R . . H61B H 0.1416 0.4299 -0.1154 0.051 Uiso 1 1 calc R . . N62A N 0.0781(6) 0.4269(5) -0.0666(3) 0.045(2) Uani 1 1 d U . . H62A H 0.0889 0.4298 -0.0407 0.053 Uiso 1 1 calc R . . C63A C 0.0321(7) 0.4906(8) -0.0759(4) 0.054(3) Uani 1 1 d U . . H63A H 0.0187 0.4894 -0.1033 0.065 Uiso 1 1 calc R . . H63B H 0.0597 0.5368 -0.0709 0.065 Uiso 1 1 calc R . . C64A C -0.0387(8) 0.4886(8) -0.0511(4) 0.062(4) Uani 1 1 d U . . H64A H -0.0252 0.4941 -0.0239 0.074 Uiso 1 1 calc R . . H64B H -0.0711 0.5304 -0.0581 0.074 Uiso 1 1 calc R . . C65A C -0.0799(8) 0.4169(9) -0.0567(4) 0.061(4) Uani 1 1 d U . . H65A H -0.1224 0.4153 -0.0389 0.074 Uiso 1 1 calc R . . H65B H -0.0994 0.4149 -0.0830 0.074 Uiso 1 1 calc R . . C66A C -0.0333(8) 0.3532(8) -0.0500(4) 0.060(4) Uani 1 1 d U . . H66A H -0.0607 0.3081 -0.0574 0.072 Uiso 1 1 calc R . . H66B H -0.0222 0.3498 -0.0224 0.072 Uiso 1 1 calc R . . C67A C 0.0409(7) 0.3560(7) -0.0728(4) 0.050(3) Uani 1 1 d U . . H67A H 0.0734 0.3152 -0.0644 0.060 Uiso 1 1 calc R . . H67B H 0.0308 0.3495 -0.1004 0.060 Uiso 1 1 calc R . . C1B C 0.0336(7) 0.3857(7) 0.0694(4) 0.039(3) Uani 1 1 d U . . O1B O 0.0480(4) 0.4316(4) 0.0401(2) 0.0380(19) Uani 1 1 d U . . C2B C 0.0909(7) 0.3550(7) 0.0903(3) 0.039(3) Uani 1 1 d U . . C21B C 0.1662(6) 0.3668(6) 0.0876(3) 0.030(3) Uani 1 1 d U . . H21B H 0.1978 0.3323 0.0998 0.036 Uiso 1 1 calc R . . N2B N 0.1972(5) 0.4219(5) 0.0696(2) 0.030(2) Uani 1 1 d U . . C22B C 0.2762(7) 0.4160(7) 0.0683(4) 0.040(3) Uani 1 1 d U . . C23B C 0.3092(7) 0.3513(7) 0.0501(4) 0.045(3) Uani 1 1 d U . . H23B H 0.2774 0.3153 0.0392 0.054 Uiso 1 1 calc R . . C24B C 0.3785(8) 0.3411(8) 0.0482(4) 0.052(3) Uani 1 1 d U . . H24B H 0.3957 0.2973 0.0362 0.063 Uiso 1 1 calc R . . C25B C 0.4305(7) 0.3893(7) 0.0624(4) 0.042(3) Uani 1 1 d U . . H25B H 0.4820 0.3796 0.0617 0.050 Uiso 1 1 calc R . . C26B C 0.4001(6) 0.4556(7) 0.0784(4) 0.040(3) Uani 1 1 d U . . H26B H 0.4328 0.4928 0.0874 0.048 Uiso 1 1 calc R . . C27B C 0.3269(6) 0.4671(7) 0.0813(4) 0.038(3) Uani 1 1 d U . . C3B C 0.0641(7) 0.2976(7) 0.1175(3) 0.037(3) Uani 1 1 d U . . H3B H 0.1004 0.2750 0.1331 0.044 Uiso 1 1 calc R . . C4B C -0.0014(7) 0.2757(6) 0.1219(4) 0.039(3) Uani 1 1 d U . . C41B C -0.0220(8) 0.2136(7) 0.1527(5) 0.056(3) Uani 1 1 d U . . C42B C -0.0856(9) 0.2407(10) 0.1784(5) 0.094(6) Uani 1 1 d U . . H42D H -0.1263 0.2585 0.1625 0.141 Uiso 1 1 calc R . . H42E H -0.0679 0.2809 0.1948 0.141 Uiso 1 1 calc R . . H42F H -0.1029 0.1998 0.1944 0.141 Uiso 1 1 calc R . . C43B C -0.0521(9) 0.1473(8) 0.1276(5) 0.077(5) Uani 1 1 d U . . H43D H -0.0941 0.1642 0.1124 0.116 Uiso 1 1 calc R . . H43E H -0.0679 0.1070 0.1444 0.116 Uiso 1 1 calc R . . H43F H -0.0129 0.1296 0.1107 0.116 Uiso 1 1 calc R . . C44B C 0.0414(9) 0.1875(8) 0.1743(4) 0.068(4) Uani 1 1 d U . . H44D H 0.0255 0.1491 0.1922 0.102 Uiso 1 1 calc R . . H44E H 0.0631 0.2287 0.1885 0.102 Uiso 1 1 calc R . . H44F H 0.0782 0.1670 0.1568 0.102 Uiso 1 1 calc R . . C5B C -0.0564(7) 0.3130(7) 0.1001(4) 0.048(3) Uani 1 1 d U . . H5B H -0.1069 0.3007 0.1037 0.057 Uiso 1 1 calc R . . C6B C -0.0373(7) 0.3678(7) 0.0733(4) 0.039(3) Uani 1 1 d U . . C61B C -0.0982(7) 0.4018(7) 0.0515(4) 0.042(3) Uani 1 1 d U . . H61C H -0.0831 0.4050 0.0244 0.050 Uiso 1 1 calc R . . H61D H -0.1415 0.3685 0.0528 0.050 Uiso 1 1 calc R . . N62B N -0.1214(5) 0.4759(5) 0.0642(3) 0.036(2) Uani 1 1 d U . . H62B H -0.0806 0.5069 0.0621 0.044 Uiso 1 1 calc R . . C63B C -0.1477(7) 0.4787(7) 0.1057(3) 0.051(3) Uani 1 1 d U . . H63C H -0.1889 0.4435 0.1091 0.061 Uiso 1 1 calc R . . H63D H -0.1069 0.4630 0.1227 0.061 Uiso 1 1 calc R . . C64B C -0.1721(7) 0.5525(8) 0.1168(4) 0.056(3) Uani 1 1 d U . . H64C H -0.1301 0.5871 0.1147 0.067 Uiso 1 1 calc R . . H64D H -0.1881 0.5516 0.1438 0.067 Uiso 1 1 calc R . . C65B C -0.2368(8) 0.5809(9) 0.0917(4) 0.067(4) Uani 1 1 d U . . H65C H -0.2509 0.6314 0.0995 0.081 Uiso 1 1 calc R . . H65D H -0.2803 0.5483 0.0946 0.081 Uiso 1 1 calc R . . C66B C -0.2093(9) 0.5808(8) 0.0487(4) 0.071(4) Uani 1 1 d U . . H66C H -0.2506 0.5950 0.0317 0.086 Uiso 1 1 calc R . . H66D H -0.1694 0.6175 0.0455 0.086 Uiso 1 1 calc R . . C67B C -0.1816(7) 0.5063(8) 0.0376(4) 0.052(3) Uani 1 1 d U . . H67C H -0.1617 0.5088 0.0113 0.062 Uiso 1 1 calc R . . H67D H -0.2236 0.4713 0.0374 0.062 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 Ni1 0.0388(12) 0.0282(11) 0.0283(9) -0.0007(9) 0.0008(10) -0.0006(9) S1S 0.042(2) 0.0331(18) 0.045(2) 0.0013(16) -0.0027(16) -0.0009(15) O1S 0.059(5) 0.035(4) 0.014(3) 0.009(3) -0.014(4) 0.003(3) O2S 0.043(5) 0.039(4) 0.026(4) -0.002(3) 0.001(3) 0.001(3) O3S 0.055(5) 0.053(6) 0.049(6) 0.001(5) -0.014(4) 0.004(4) O4S 0.058(6) 0.040(4) 0.047(5) 0.014(4) 0.004(5) 0.005(4) C1A 0.040(7) 0.047(7) 0.036(5) 0.013(5) 0.005(5) -0.004(5) O1A 0.038(5) 0.045(5) 0.011(3) -0.005(3) 0.003(3) -0.005(3) C2A 0.046(8) 0.040(7) 0.053(5) 0.013(5) 0.007(6) -0.001(5) C21A 0.052(8) 0.039(8) 0.057(6) -0.001(6) 0.023(6) -0.015(6) N2A 0.031(4) 0.027(5) 0.044(5) -0.003(4) -0.001(4) -0.005(4) C22A 0.031(7) 0.039(6) 0.047(6) -0.010(5) -0.006(5) -0.002(5) C23A 0.033(7) 0.029(6) 0.045(7) 0.001(5) -0.002(6) -0.016(5) C24A 0.041(8) 0.038(7) 0.045(7) -0.007(6) 0.002(6) -0.008(5) C25A 0.039(8) 0.075(9) 0.053(8) -0.006(7) 0.006(6) 0.002(7) C26A 0.039(8) 0.043(7) 0.062(8) 0.014(6) -0.010(6) -0.010(6) C27A 0.024(6) 0.051(6) 0.039(7) 0.008(5) 0.006(5) 0.007(5) C3A 0.067(9) 0.038(7) 0.042(5) 0.019(6) -0.009(6) -0.010(6) C4A 0.045(7) 0.067(8) 0.034(5) 0.013(6) 0.004(6) -0.018(6) C41A 0.072(8) 0.091(8) 0.023(6) -0.005(7) 0.020(7) -0.034(8) C42A 0.128(15) 0.075(8) 0.069(11) 0.016(8) -0.004(11) -0.038(9) C43A 0.105(12) 0.066(10) 0.035(6) 0.018(7) -0.007(8) -0.031(9) C44A 0.070(8) 0.137(15) 0.081(12) 0.036(13) 0.006(8) -0.042(9) C5A 0.045(8) 0.058(8) 0.028(6) 0.008(6) 0.005(6) -0.007(5) C6A 0.048(7) 0.046(7) 0.041(5) 0.021(6) 0.005(6) -0.006(5) C61A 0.043(6) 0.043(7) 0.040(8) 0.002(6) -0.005(6) -0.001(5) N62A 0.047(6) 0.033(5) 0.054(7) -0.004(5) 0.004(5) -0.001(4) C63A 0.052(7) 0.049(7) 0.061(9) -0.006(7) 0.001(6) 0.009(6) C64A 0.067(8) 0.060(7) 0.058(9) -0.007(8) 0.006(7) 0.029(7) C65A 0.061(8) 0.093(10) 0.029(7) 0.011(8) -0.010(7) -0.002(6) C66A 0.077(8) 0.057(7) 0.046(8) 0.011(7) 0.010(7) -0.022(6) C67A 0.056(7) 0.051(6) 0.043(8) 0.011(7) -0.009(6) -0.012(6) C1B 0.033(5) 0.042(7) 0.042(7) -0.004(5) -0.004(5) -0.007(5) O1B 0.026(4) 0.033(4) 0.055(5) -0.003(4) -0.003(4) -0.006(3) C2B 0.045(5) 0.050(7) 0.023(6) -0.003(5) -0.007(5) -0.012(5) C21B 0.037(5) 0.017(5) 0.035(7) 0.002(5) -0.009(5) 0.000(4) N2B 0.042(4) 0.034(5) 0.012(5) 0.007(4) -0.014(4) -0.001(3) C22B 0.033(5) 0.045(6) 0.042(8) 0.029(5) 0.005(5) 0.003(4) C23B 0.043(6) 0.041(7) 0.050(8) 0.012(6) -0.010(6) -0.008(5) C24B 0.049(7) 0.065(8) 0.043(9) 0.006(7) 0.002(7) 0.006(6) C25B 0.026(6) 0.050(7) 0.050(9) 0.018(6) 0.007(6) 0.008(5) C26B 0.028(5) 0.048(7) 0.045(8) 0.012(6) -0.001(6) 0.012(5) C27B 0.029(5) 0.036(6) 0.049(8) 0.024(5) -0.001(6) 0.005(4) C3B 0.031(6) 0.039(7) 0.039(7) 0.000(5) -0.006(5) 0.003(5) C4B 0.023(5) 0.031(6) 0.062(8) 0.004(5) 0.009(6) 0.006(5) C41B 0.048(8) 0.044(8) 0.076(10) 0.015(6) 0.002(6) -0.009(6) C42B 0.090(12) 0.110(14) 0.081(12) 0.035(9) 0.033(9) 0.024(10) C43B 0.095(12) 0.049(8) 0.088(11) 0.026(7) -0.012(9) -0.033(9) C44B 0.078(9) 0.069(10) 0.056(10) 0.010(7) 0.002(7) 0.012(8) C5B 0.034(6) 0.038(7) 0.071(9) -0.001(5) -0.011(6) -0.003(5) C6B 0.034(5) 0.041(7) 0.042(7) -0.005(5) -0.003(5) -0.005(5) C61B 0.034(6) 0.043(6) 0.048(8) 0.003(5) 0.007(6) 0.001(5) N62B 0.029(5) 0.040(5) 0.039(5) 0.008(5) -0.003(4) -0.012(4) C63B 0.037(7) 0.076(9) 0.041(6) 0.000(6) -0.002(6) 0.003(6) C64B 0.038(8) 0.058(8) 0.072(8) -0.004(7) -0.009(6) -0.007(6) C65B 0.054(9) 0.061(9) 0.086(9) -0.009(8) -0.014(8) 0.006(7) C66B 0.071(10) 0.058(8) 0.085(9) 0.020(9) -0.016(8) 0.013(7) C67B 0.052(7) 0.062(8) 0.042(7) 0.011(7) -0.012(6) 0.002(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 Ni1 O1A 1.966(7) . ? Ni1 N2B 2.027(9) . ? Ni1 O1B 2.061(7) . ? Ni1 N2A 2.080(9) . ? Ni1 O2S 2.086(7) . ? Ni1 O1S 2.108(7) . ? Ni1 S1S 2.696(4) . ? S1S O4S 1.434(8) . ? S1S O3S 1.462(9) . ? S1S O2S 1.516(8) . ? S1S O1S 1.537(8) . ? C1A O1A 1.354(13) . ? C1A C2A 1.364(17) . ? C1A C6A 1.393(16) . ? C2A C3A 1.429(16) . ? C2A C21A 1.532(18) . ? C21A N2A 1.287(14) . ? N2A C22A 1.434(15) . ? C22A C27A 1.373(16) . ? C22A C23A 1.381(16) . ? C23A C24A 1.457(17) . ? C24A C25A 1.337(18) . ? C25A C26A 1.461(19) . ? C26A C27A 1.445(18) . ? C27A C27B 1.484(17) . ? C3A C4A 1.391(17) . ? C4A C5A 1.336(17) . ? C4A C41A 1.509(17) . ? C41A C44A 1.45(2) . ? C41A C43A 1.498(17) . ? C41A C42A 1.68(2) . ? C5A C6A 1.410(16) . ? C6A C61A 1.506(17) . ? C61A N62A 1.508(14) . ? N62A C63A 1.462(16) . ? N62A C67A 1.467(14) . ? C63A C64A 1.549(17) . ? C64A C65A 1.51(2) . ? C65A C66A 1.449(18) . ? C66A C67A 1.566(17) . ? C1B C6B 1.332(15) . ? C1B O1B 1.347(14) . ? C1B C2B 1.386(17) . ? C2B C21B 1.385(16) . ? C2B C3B 1.492(17) . ? C21B N2B 1.309(13) . ? N2B C22B 1.436(14) . ? C22B C27B 1.381(17) . ? C22B C23B 1.464(17) . ? C23B C24B 1.272(17) . ? C24B C25B 1.378(17) . ? C25B C26B 1.436(17) . ? C26B C27B 1.346(15) . ? C3B C4B 1.261(16) . ? C4B C5B 1.427(17) . ? C4B C41B 1.602(17) . ? C41B C44B 1.455(19) . ? C41B C42B 1.55(2) . ? C41B C43B 1.58(2) . ? C5B C6B 1.410(16) . ? C6B C61B 1.477(16) . ? C61B N62B 1.477(14) . ? N62B C63B 1.534(14) . ? N62B C67B 1.537(14) . ? C63B C64B 1.461(18) . ? C64B C65B 1.554(18) . ? C65B C66B 1.588(19) . ? C66B C67B 1.491(18) . ? 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 O1A Ni1 N2B 96.0(3) . . ? O1A Ni1 O1B 93.7(3) . . ? N2B Ni1 O1B 90.3(3) . . ? O1A Ni1 N2A 89.0(4) . . ? N2B Ni1 N2A 89.8(4) . . ? O1B Ni1 N2A 177.3(4) . . ? O1A Ni1 O2S 160.6(3) . . ? N2B Ni1 O2S 103.5(3) . . ? O1B Ni1 O2S 85.9(3) . . ? N2A Ni1 O2S 91.5(4) . . ? O1A Ni1 O1S 91.9(3) . . ? N2B Ni1 O1S 172.1(3) . . ? O1B Ni1 O1S 88.6(3) . . ? N2A Ni1 O1S 90.9(3) . . ? O2S Ni1 O1S 68.7(3) . . ? O1A Ni1 S1S 126.5(2) . . ? N2B Ni1 S1S 137.4(3) . . ? O1B Ni1 S1S 85.1(2) . . ? N2A Ni1 S1S 92.9(3) . . ? O2S Ni1 S1S 34.0(2) . . ? O1S Ni1 S1S 34.7(2) . . ? O4S S1S O3S 109.8(5) . . ? O4S S1S O2S 114.0(5) . . ? O3S S1S O2S 108.9(5) . . ? O4S S1S O1S 111.3(5) . . ? O3S S1S O1S 111.1(5) . . ? O2S S1S O1S 101.5(4) . . ? O4S S1S Ni1 130.1(4) . . ? O3S S1S Ni1 120.1(4) . . ? O2S S1S Ni1 50.4(3) . . ? O1S S1S Ni1 51.3(3) . . ? S1S O1S Ni1 94.1(3) . . ? S1S O2S Ni1 95.6(4) . . ? O1A C1A C2A 124.0(12) . . ? O1A C1A C6A 118.1(12) . . ? C2A C1A C6A 117.8(12) . . ? C1A O1A Ni1 123.8(8) . . ? C1A C2A C3A 122.6(13) . . ? C1A C2A C21A 125.2(12) . . ? C3A C2A C21A 112.2(12) . . ? N2A C21A C2A 120.5(12) . . ? C21A N2A C22A 119.8(10) . . ? C21A N2A Ni1 127.0(9) . . ? C22A N2A Ni1 113.0(7) . . ? C27A C22A C23A 126.5(12) . . ? C27A C22A N2A 116.7(11) . . ? C23A C22A N2A 115.9(11) . . ? C22A C23A C24A 115.3(12) . . ? C25A C24A C23A 121.4(13) . . ? C24A C25A C26A 121.8(13) . . ? C27A C26A C25A 117.2(12) . . ? C22A C27A C26A 117.3(12) . . ? C22A C27A C27B 125.8(12) . . ? C26A C27A C27B 116.8(11) . . ? C4A C3A C2A 118.5(12) . . ? C5A C4A C3A 118.2(12) . . ? C5A C4A C41A 124.2(12) . . ? C3A C4A C41A 117.5(12) . . ? C44A C41A C43A 112.7(13) . . ? C44A C41A C4A 116.2(14) . . ? C43A C41A C4A 112.8(12) . . ? C44A C41A C42A 101.5(13) . . ? C43A C41A C42A 104.5(14) . . ? C4A C41A C42A 107.7(11) . . ? C4A C5A C6A 124.1(13) . . ? C1A C6A C5A 118.6(12) . . ? C1A C6A C61A 120.4(11) . . ? C5A C6A C61A 121.0(12) . . ? C6A C61A N62A 110.2(10) . . ? C63A N62A C67A 113.3(10) . . ? C63A N62A C61A 112.4(10) . . ? C67A N62A C61A 109.6(10) . . ? N62A C63A C64A 109.2(11) . . ? C65A C64A C63A 110.9(12) . . ? C66A C65A C64A 112.2(12) . . ? C65A C66A C67A 113.1(12) . . ? N62A C67A C66A 110.3(11) . . ? C6B C1B O1B 114.5(12) . . ? C6B C1B C2B 124.8(13) . . ? O1B C1B C2B 120.3(11) . . ? C1B O1B Ni1 121.7(7) . . ? C21B C2B C1B 129.8(12) . . ? C21B C2B C3B 118.1(11) . . ? C1B C2B C3B 111.9(11) . . ? N2B C21B C2B 125.0(11) . . ? C21B N2B C22B 112.7(9) . . ? C21B N2B Ni1 123.6(8) . . ? C22B N2B Ni1 123.1(7) . . ? C27B C22B N2B 127.1(12) . . ? C27B C22B C23B 114.2(11) . . ? N2B C22B C23B 118.7(11) . . ? C24B C23B C22B 122.9(13) . . ? C23B C24B C25B 124.3(14) . . ? C24B C25B C26B 114.2(12) . . ? C27B C26B C25B 122.4(13) . . ? C26B C27B C22B 121.9(13) . . ? C26B C27B C27A 117.8(12) . . ? C22B C27B C27A 120.3(11) . . ? C4B C3B C2B 127.2(12) . . ? C3B C4B C5B 116.2(12) . . ? C3B C4B C41B 121.5(12) . . ? C5B C4B C41B 122.1(11) . . ? C44B C41B C42B 112.8(14) . . ? C44B C41B C43B 108.3(12) . . ? C42B C41B C43B 107.9(13) . . ? C44B C41B C4B 113.3(12) . . ? C42B C41B C4B 110.1(11) . . ? C43B C41B C4B 103.9(12) . . ? C6B C5B C4B 121.3(11) . . ? C1B C6B C5B 118.5(12) . . ? C1B C6B C61B 124.4(12) . . ? C5B C6B C61B 117.1(11) . . ? N62B C61B C6B 115.8(10) . . ? C61B N62B C63B 113.8(10) . . ? C61B N62B C67B 110.2(9) . . ? C63B N62B C67B 110.1(9) . . ? C64B C63B N62B 112.1(11) . . ? C63B C64B C65B 112.4(12) . . ? C64B C65B C66B 107.6(12) . . ? C67B C66B C65B 110.7(12) . . ? C66B C67B N62B 113.9(11) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.016 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.100 #===END