Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lucia Carlucci' _publ_contact_author_email LUCIA.CARLUCCI@UNIMI.IT _publ_section_title ; Metal-organic coordination frameworks assembled with the long flexible ligand 4,4'-bis(imidazol-1-ylmethyl)biphenyl ; loop_ _publ_author_name 'Lucia Carlucci' 'Gianfranco Ciani' 'Simona Maggini' 'Davide Proserpio' # Attachment 'ALL_12_rev.CIF' data_Lu630_bimb _database_code_depnum_ccdc_archive 'CCDC 680065' _chemical_formula_sum 'C20 H18 N4' _chemical_formula_weight 314.38 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' _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 10.9570(11) _cell_length_b 9.9635(10) _cell_length_c 15.4573(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.426(2) _cell_angle_gamma 90.00 _cell_volume 1682.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1661 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 19757 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4892 _reflns_number_observed 2064 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The best refinement was obtained considering one of the imidazole ring with a disorder over the C/N position. The Fourier difference did not allow unambiguous assignement of the C/N, and a split atom model with C:N 50%:50% and 50% H on both center was applied. This is also consistent with possible weak CH...N bond pattern. ; _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^)+(0.0752P)^2^+0.1459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4892 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_obs 0.0590 _refine_ls_wR_factor_all 0.1770 _refine_ls_wR_factor_obs 0.1340 _refine_ls_goodness_of_fit_all 0.986 _refine_ls_restrained_S_all 0.986 _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 N1 N 0.46700(14) 0.14130(15) 0.27341(10) 0.0440(4) Uani 1 1 d . B . N2 N 1.02802(15) -0.29872(17) -0.27440(11) 0.0533(5) Uani 1 1 d . . . C3 C 0.58441(17) 0.1213(2) 0.14244(12) 0.0460(5) Uani 1 1 d . B . C4 C 0.70875(16) -0.03866(18) 0.02675(11) 0.0427(5) Uani 1 1 d . . . C5 C 0.8081(2) -0.3331(2) -0.10481(13) 0.0562(6) Uani 1 1 d . . . H5 H 0.7847 -0.4218 -0.1150 0.067 Uiso 1 1 calc R . . C6 C 0.35232(18) 0.0900(2) 0.27163(13) 0.0507(5) Uani 1 1 d . . . H6 H 0.2935 0.0961 0.2251 0.061 Uiso 1 1 calc R A 1 C7 C 0.77637(16) -0.12241(19) -0.03248(11) 0.0424(5) Uani 1 1 d . . . C8 C 0.74517(19) -0.25546(19) -0.04889(13) 0.0504(5) Uani 1 1 d . . . H8 H 0.6806 -0.2932 -0.0217 0.060 Uiso 1 1 calc R . . N9 N 0.4446(2) 0.0431(2) 0.39732(12) 0.0625(5) Uani 0.50 1 d P B 1 C9 C 0.4446(2) 0.0431(2) 0.39732(12) 0.0625(5) Uani 0.50 1 d P B 2 H9 H 0.4600 0.0109 0.4536 0.075 Uiso 0.50 1 calc PR B 2 C10 C 0.5225(2) 0.1097(2) 0.35210(13) 0.0545(5) Uani 1 1 d . . . H10 H 0.6026 0.1314 0.3713 0.065 Uiso 1 1 calc R B 1 C11 C 0.5217(2) 0.2121(2) 0.20350(13) 0.0534(5) Uani 1 1 d . . . H11A H 0.5811 0.2760 0.2287 0.064 Uiso 1 1 calc R B . H11B H 0.4583 0.2623 0.1704 0.064 Uiso 1 1 calc R . . C12 C 0.65809(19) -0.0931(2) 0.09811(13) 0.0556(6) Uani 1 1 d . B . H12 H 0.6646 -0.1850 0.1080 0.067 Uiso 1 1 calc R . . N13 N 0.33687(19) 0.0299(2) 0.34612(14) 0.0605(5) Uani 0.50 1 d P B 1 C13 C 0.33687(19) 0.0299(2) 0.34612(14) 0.0605(5) Uani 0.50 1 d P B 2 H13 H 0.2663 -0.0132 0.3612 0.073 Uiso 0.50 1 calc PR B 2 C14 C 0.87514(18) -0.0710(2) -0.07380(12) 0.0485(5) Uani 1 1 d . . . H14 H 0.8988 0.0177 -0.0639 0.058 Uiso 1 1 calc R . . C15 C 0.6937(2) 0.0982(2) 0.01401(13) 0.0631(6) Uani 1 1 d . B . H15 H 0.7256 0.1384 -0.0337 0.076 Uiso 1 1 calc R . . N16 N 1.1673(2) -0.2011(2) -0.34797(15) 0.0762(6) Uani 1 1 d . . . C17 C 0.93848(18) -0.1488(2) -0.12903(13) 0.0531(5) Uani 1 1 d . . . H17 H 1.0044 -0.1122 -0.1553 0.064 Uiso 1 1 calc R . . C18 C 0.59813(18) -0.0149(2) 0.15506(13) 0.0558(6) Uani 1 1 d . . . H18 H 0.5664 -0.0549 0.2029 0.067 Uiso 1 1 calc R B . C19 C 1.1449(2) -0.2652(3) -0.27819(16) 0.0726(7) Uani 1 1 d . . . H19 H 1.2052 -0.2860 -0.2346 0.087 Uiso 1 1 calc R . . C20 C 0.9052(2) -0.2806(2) -0.14586(14) 0.0566(6) Uani 1 1 d . . . C21 C 0.6326(2) 0.1764(2) 0.07054(14) 0.0661(7) Uani 1 1 d . . . H21 H 0.6238 0.2679 0.0600 0.079 Uiso 1 1 calc R B . C22 C 0.9711(2) -0.2502(2) -0.34803(16) 0.0681(7) Uani 1 1 d . . . H22 H 0.8880 -0.2559 -0.3651 0.082 Uiso 1 1 calc R . . C23 C 1.0574(3) -0.1924(2) -0.39171(16) 0.0736(7) Uani 1 1 d . . . H23 H 1.0430 -0.1514 -0.4456 0.088 Uiso 1 1 calc R . . C24 C 0.9734(3) -0.3700(2) -0.20517(17) 0.0841(8) Uani 1 1 d . . . H24A H 1.0375 -0.4171 -0.1706 0.101 Uiso 1 1 calc R . . H24B H 0.9171 -0.4367 -0.2307 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 N1 0.0450(9) 0.0474(10) 0.0407(9) -0.0052(7) 0.0102(7) 0.0023(7) N2 0.0494(10) 0.0538(10) 0.0599(11) -0.0053(9) 0.0242(9) 0.0043(8) C3 0.0507(11) 0.0437(11) 0.0449(11) 0.0008(9) 0.0112(9) -0.0001(9) C4 0.0461(10) 0.0441(11) 0.0390(10) 0.0020(8) 0.0091(9) -0.0015(9) C5 0.0675(14) 0.0439(12) 0.0604(13) -0.0001(10) 0.0258(11) -0.0036(10) C6 0.0449(11) 0.0571(13) 0.0507(12) -0.0036(10) 0.0062(9) -0.0010(9) C7 0.0470(11) 0.0449(11) 0.0362(10) 0.0032(8) 0.0083(8) -0.0008(9) C8 0.0542(12) 0.0489(12) 0.0506(12) 0.0033(10) 0.0199(10) -0.0062(9) N9 0.0822(15) 0.0598(13) 0.0468(11) 0.0028(10) 0.0124(11) 0.0091(11) C9 0.0822(15) 0.0598(13) 0.0468(11) 0.0028(10) 0.0124(11) 0.0091(11) C10 0.0558(13) 0.0576(13) 0.0492(12) -0.0079(10) -0.0013(10) 0.0067(10) C11 0.0579(13) 0.0504(12) 0.0547(12) 0.0015(10) 0.0222(10) -0.0001(10) C12 0.0702(14) 0.0419(11) 0.0585(13) 0.0086(10) 0.0299(11) 0.0019(10) N13 0.0629(13) 0.0573(12) 0.0641(13) 0.0040(10) 0.0230(11) -0.0006(10) C13 0.0629(13) 0.0573(12) 0.0641(13) 0.0040(10) 0.0230(11) -0.0006(10) C14 0.0516(12) 0.0473(12) 0.0480(11) 0.0013(9) 0.0134(10) -0.0069(9) C15 0.0955(17) 0.0488(13) 0.0491(12) 0.0094(10) 0.0327(12) 0.0008(12) N16 0.0714(14) 0.0830(15) 0.0782(14) -0.0062(12) 0.0320(12) -0.0097(11) C17 0.0506(12) 0.0541(14) 0.0576(13) 0.0042(10) 0.0226(10) -0.0022(10) C18 0.0653(14) 0.0481(13) 0.0587(13) 0.0089(10) 0.0349(11) 0.0023(10) C19 0.0478(13) 0.104(2) 0.0668(16) 0.0003(14) 0.0092(12) 0.0079(13) C20 0.0627(14) 0.0500(13) 0.0604(13) 0.0065(10) 0.0267(11) 0.0071(10) C21 0.1037(18) 0.0428(13) 0.0563(13) 0.0069(10) 0.0342(13) 0.0034(12) C22 0.0525(14) 0.0842(18) 0.0669(15) -0.0151(13) -0.0003(12) 0.0043(12) C23 0.102(2) 0.0693(17) 0.0519(14) -0.0029(12) 0.0184(15) 0.0092(15) C24 0.108(2) 0.0573(15) 0.0965(19) 0.0077(14) 0.0654(17) 0.0142(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.354(2) . ? N1 C6 1.355(2) . ? N1 C11 1.458(2) . ? N2 C19 1.329(3) . ? N2 C22 1.345(3) . ? N2 C24 1.451(3) . ? C3 C18 1.378(3) . ? C3 C21 1.381(3) . ? C3 C11 1.510(3) . ? C4 C12 1.383(2) . ? C4 C15 1.386(3) . ? C4 C7 1.479(2) . ? C5 C8 1.383(3) . ? C5 C20 1.384(3) . ? C5 H5 0.9300 . ? C6 N13 1.320(3) . ? C6 H6 0.9300 . ? C7 C8 1.387(3) . ? C7 C14 1.396(2) . ? C8 H8 0.9300 . ? N9 C10 1.323(3) . ? N9 N13 1.376(3) . ? C10 H10 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C18 1.379(3) . ? C12 H12 0.9300 . ? C14 C17 1.380(3) . ? C14 H14 0.9300 . ? C15 C21 1.382(3) . ? C15 H15 0.9300 . ? N16 C19 1.293(3) . ? N16 C23 1.338(3) . ? C17 C20 1.382(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C24 1.516(3) . ? C21 H21 0.9300 . ? C22 C23 1.334(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? 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 C10 N1 C6 106.39(17) . . ? C10 N1 C11 126.59(17) . . ? C6 N1 C11 126.98(17) . . ? C19 N2 C22 104.96(19) . . ? C19 N2 C24 127.5(2) . . ? C22 N2 C24 127.5(2) . . ? C18 C3 C21 117.48(18) . . ? C18 C3 C11 123.47(17) . . ? C21 C3 C11 119.05(18) . . ? C12 C4 C15 116.67(18) . . ? C12 C4 C7 121.55(17) . . ? C15 C4 C7 121.78(16) . . ? C8 C5 C20 120.9(2) . . ? C8 C5 H5 119.6 . . ? C20 C5 H5 119.6 . . ? N13 C6 N1 109.54(18) . . ? N13 C6 H6 125.2 . . ? N1 C6 H6 125.2 . . ? C8 C7 C14 117.12(17) . . ? C8 C7 C4 121.60(16) . . ? C14 C7 C4 121.28(17) . . ? C5 C8 C7 121.41(18) . . ? C5 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 N9 N13 107.69(17) . . ? N9 C10 N1 109.12(19) . . ? N9 C10 H10 125.4 . . ? N1 C10 H10 125.4 . . ? N1 C11 C3 113.99(16) . . ? N1 C11 H11A 108.8 . . ? C3 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C3 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C18 C12 C4 121.84(19) . . ? C18 C12 H12 119.1 . . ? C4 C12 H12 119.1 . . ? C6 N13 N9 107.24(18) . . ? C17 C14 C7 121.44(19) . . ? C17 C14 H14 119.3 . . ? C7 C14 H14 119.3 . . ? C21 C15 C4 121.52(18) . . ? C21 C15 H15 119.2 . . ? C4 C15 H15 119.2 . . ? C19 N16 C23 103.4(2) . . ? C14 C17 C20 120.85(18) . . ? C14 C17 H17 119.6 . . ? C20 C17 H17 119.6 . . ? C3 C18 C12 121.20(18) . . ? C3 C18 H18 119.4 . . ? C12 C18 H18 119.4 . . ? N16 C19 N2 114.0(2) . . ? N16 C19 H19 123.0 . . ? N2 C19 H19 123.0 . . ? C17 C20 C5 118.29(18) . . ? C17 C20 C24 122.47(19) . . ? C5 C20 C24 119.2(2) . . ? C3 C21 C15 121.3(2) . . ? C3 C21 H21 119.4 . . ? C15 C21 H21 119.4 . . ? C23 C22 N2 106.4(2) . . ? C23 C22 H22 126.8 . . ? N2 C22 H22 126.8 . . ? C22 C23 N16 111.2(2) . . ? C22 C23 H23 124.4 . . ? N16 C23 H23 124.4 . . ? N2 C24 C20 114.16(18) . . ? N2 C24 H24A 108.7 . . ? C20 C24 H24A 108.7 . . ? N2 C24 H24B 108.7 . . ? C20 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.256 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.038 data_lu677_bimb(H2O) _database_code_depnum_ccdc_archive 'CCDC 680066' _chemical_formula_sum 'C20 H20 N4 O' _chemical_formula_weight 332.40 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 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.7126(10) _cell_length_b 15.269(3) _cell_length_c 24.148(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.024(3) _cell_angle_gamma 90.00 _cell_volume 1733.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2270 _cell_measurement_theta_min 3 _cell_measurement_theta_max 21 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 21474 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 29.39 _reflns_number_total 4493 _reflns_number_observed 2054 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The H atoms on the chlatrate water molecules are modelled over 3 positions to explain the compatibility of the observed H-bond pattern with the presence of a center of symmetry in the middle of one O...O H-bond: N..HO 2.81, O...O 2.75,2.77 ; _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^)+(0.0528P)^2^+0.3984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4493 _refine_ls_number_parameters 235 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1641 _refine_ls_R_factor_obs 0.0690 _refine_ls_wR_factor_all 0.1625 _refine_ls_wR_factor_obs 0.1291 _refine_ls_goodness_of_fit_all 1.007 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 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 C1 C -0.4707(6) 0.50667(18) -0.33051(11) 0.0769(8) Uani 1 1 d . . . H1 H -0.5823 0.4587 -0.3417 0.092 Uiso 1 1 calc R . . C2 C -0.1763(6) 0.60978(18) -0.33009(11) 0.0718(7) Uani 1 1 d . . . H2 H -0.0399 0.6488 -0.3412 0.086 Uiso 1 1 calc R . . C3 C -0.2853(6) 0.61097(16) -0.28032(10) 0.0664(7) Uani 1 1 d . . . H3 H -0.2395 0.6496 -0.2513 0.080 Uiso 1 1 calc R . . C4 C -0.6326(5) 0.51503(16) -0.23409(9) 0.0636(6) Uani 1 1 d . . . H4A H -0.7814 0.4747 -0.2473 0.076 Uiso 1 1 calc R . . H4B H -0.7218 0.5650 -0.2176 0.076 Uiso 1 1 calc R . . C5 C -0.4375(5) 0.47034(15) -0.19094(9) 0.0532(6) Uani 1 1 d . . . C6 C -0.3319(6) 0.51312(16) -0.14416(10) 0.0671(7) Uani 1 1 d . . . H6 H -0.3882 0.5705 -0.1380 0.081 Uiso 1 1 calc R . . C7 C -0.1441(5) 0.47292(15) -0.10602(10) 0.0666(7) Uani 1 1 d . . . H7 H -0.0800 0.5036 -0.0743 0.080 Uiso 1 1 calc R . . C8 C -0.0479(4) 0.38899(13) -0.11316(8) 0.0462(5) Uani 1 1 d . . . C9 C -0.1570(6) 0.34689(16) -0.16045(10) 0.0714(7) Uani 1 1 d . . . H9 H -0.0995 0.2898 -0.1671 0.086 Uiso 1 1 calc R . . C10 C -0.3480(6) 0.38647(17) -0.19819(10) 0.0741(7) Uani 1 1 d . . . H10 H -0.4176 0.3553 -0.2293 0.089 Uiso 1 1 calc R . . C11 C 0.1582(4) 0.34519(13) -0.07305(8) 0.0467(5) Uani 1 1 d . . . C12 C 0.3033(5) 0.39004(15) -0.03013(10) 0.0653(7) Uani 1 1 d . . . H12 H 0.2682 0.4495 -0.0257 0.078 Uiso 1 1 calc R . . C13 C 0.4983(5) 0.34905(17) 0.00623(10) 0.0697(7) Uani 1 1 d . . . H13 H 0.5896 0.3812 0.0349 0.084 Uiso 1 1 calc R . . C14 C 0.5608(5) 0.26228(16) 0.00117(9) 0.0583(6) Uani 1 1 d . . . C15 C 0.4124(6) 0.21636(17) -0.04044(10) 0.0719(7) Uani 1 1 d . . . H15 H 0.4457 0.1567 -0.0442 0.086 Uiso 1 1 calc R . . C16 C 0.2163(6) 0.25697(15) -0.07650(9) 0.0664(7) Uani 1 1 d . . . H16 H 0.1195 0.2239 -0.1041 0.080 Uiso 1 1 calc R . . C17 C 0.8651(7) 0.2769(2) 0.13497(15) 0.0920(9) Uani 1 1 d . . . H17 H 1.0085 0.3159 0.1270 0.110 Uiso 1 1 calc R . . C18 C 0.5709(8) 0.2073(3) 0.17687(13) 0.0985(10) Uani 1 1 d . . . H18 H 0.4632 0.1867 0.2050 0.118 Uiso 1 1 calc R . . C19 C 0.5432(6) 0.17908(18) 0.12424(12) 0.0753(7) Uani 1 1 d . . . H19 H 0.4172 0.1369 0.1095 0.090 Uiso 1 1 calc R . . C20 C 0.7852(5) 0.21761(19) 0.03880(10) 0.0770(8) Uani 1 1 d . . . H20A H 0.7935 0.1562 0.0287 0.092 Uiso 1 1 calc R . . H20B H 0.9688 0.2435 0.0330 0.092 Uiso 1 1 calc R . . N1 N -0.4761(4) 0.54444(12) -0.28083(7) 0.0546(5) Uani 1 1 d . . . N2 N -0.2910(5) 0.54455(17) -0.36175(9) 0.0818(7) Uani 1 1 d . . . N3 N 0.7339(4) 0.22412(12) 0.09723(7) 0.0551(5) Uani 1 1 d . . . N4 N 0.7709(8) 0.2681(2) 0.18394(12) 0.1154(11) Uani 1 1 d . . . O1 O -0.2588(5) -0.01310(15) -0.02870(8) 0.1070(7) Uani 1 1 d D . . H1W H -0.274(6) 0.0115(18) -0.0644(6) 0.128 Uiso 1 1 d D . . H2W H -0.156(9) 0.029(2) -0.0061(13) 0.128 Uiso 0.50 1 d PD . . H3W H -0.443(4) -0.017(4) -0.0163(16) 0.128 Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.090(2) 0.0867(19) 0.0541(15) -0.0114(14) 0.0060(14) -0.0142(16) C2 0.0783(18) 0.0742(18) 0.0634(16) 0.0239(14) 0.0079(14) 0.0009(15) C3 0.0855(18) 0.0599(15) 0.0534(15) 0.0075(12) 0.0020(13) -0.0025(14) C4 0.0547(14) 0.0824(17) 0.0538(14) 0.0096(13) 0.0053(11) 0.0048(13) C5 0.0542(13) 0.0607(15) 0.0456(13) 0.0064(11) 0.0089(10) 0.0009(11) C6 0.0839(18) 0.0540(14) 0.0623(15) -0.0024(12) -0.0029(14) 0.0139(13) C7 0.0843(18) 0.0597(16) 0.0536(14) -0.0093(12) -0.0098(13) 0.0117(13) C8 0.0546(13) 0.0467(12) 0.0382(11) 0.0016(10) 0.0100(10) -0.0024(11) C9 0.0931(19) 0.0524(15) 0.0660(16) -0.0088(12) -0.0125(14) 0.0118(14) C10 0.0935(19) 0.0700(17) 0.0560(15) -0.0104(13) -0.0145(14) 0.0082(15) C11 0.0526(12) 0.0465(12) 0.0418(11) 0.0031(10) 0.0104(10) 0.0011(10) C12 0.0826(17) 0.0472(13) 0.0637(15) 0.0011(12) -0.0114(13) 0.0007(13) C13 0.0763(17) 0.0659(17) 0.0643(16) 0.0021(13) -0.0127(13) 0.0002(14) C14 0.0584(14) 0.0693(16) 0.0489(13) 0.0113(12) 0.0151(11) 0.0163(12) C15 0.098(2) 0.0627(16) 0.0552(14) -0.0033(13) 0.0038(14) 0.0283(15) C16 0.0897(18) 0.0595(15) 0.0490(13) -0.0061(12) -0.0026(13) 0.0144(14) C17 0.091(2) 0.080(2) 0.101(2) -0.0029(19) -0.022(2) -0.0090(17) C18 0.108(3) 0.131(3) 0.0583(19) 0.022(2) 0.0203(18) 0.037(2) C19 0.0780(18) 0.0783(18) 0.0699(18) 0.0146(15) 0.0072(14) -0.0059(15) C20 0.0700(17) 0.103(2) 0.0590(15) 0.0174(14) 0.0127(13) 0.0290(15) N1 0.0578(11) 0.0636(12) 0.0421(11) 0.0069(9) 0.0002(9) 0.0058(10) N2 0.0975(18) 0.0970(17) 0.0519(13) -0.0019(13) 0.0139(12) -0.0006(14) N3 0.0541(11) 0.0599(12) 0.0508(11) 0.0059(10) 0.0000(9) 0.0052(10) N4 0.147(3) 0.120(3) 0.075(2) -0.0218(18) -0.020(2) 0.038(2) O1 0.138(2) 0.1180(17) 0.0661(13) 0.0206(12) 0.0168(12) -0.0062(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.308(3) . ? C1 N1 1.333(3) . ? C1 H1 0.9300 . ? C2 C3 1.340(3) . ? C2 N2 1.346(3) . ? C2 H2 0.9300 . ? C3 N1 1.356(3) . ? C3 H3 0.9300 . ? C4 N1 1.462(3) . ? C4 C5 1.504(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.363(3) . ? C5 C6 1.368(3) . ? C6 C7 1.376(3) . ? C6 H6 0.9300 . ? C7 C8 1.374(3) . ? C7 H7 0.9300 . ? C8 C9 1.378(3) . ? C8 C11 1.482(3) . ? C9 C10 1.375(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.378(3) . ? C11 C12 1.383(3) . ? C12 C13 1.376(3) . ? C12 H12 0.9300 . ? C13 C14 1.365(3) . ? C13 H13 0.9300 . ? C14 C15 1.375(3) . ? C14 C20 1.508(3) . ? C15 C16 1.373(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N4 1.299(4) . ? C17 N3 1.336(3) . ? C17 H17 0.9300 . ? C18 N4 1.326(4) . ? C18 C19 1.340(4) . ? C18 H18 0.9300 . ? C19 N3 1.337(3) . ? C19 H19 0.9300 . ? C20 N3 1.452(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? O1 H1W 0.939(10) . ? O1 H2W 0.948(10) . ? O1 H3W 0.939(10) . ? 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 N2 C1 N1 112.4(2) . . ? N2 C1 H1 123.8 . . ? N1 C1 H1 123.8 . . ? C3 C2 N2 110.8(2) . . ? C3 C2 H2 124.6 . . ? N2 C2 H2 124.6 . . ? C2 C3 N1 106.1(2) . . ? C2 C3 H3 126.9 . . ? N1 C3 H3 126.9 . . ? N1 C4 C5 110.95(18) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C10 C5 C6 117.2(2) . . ? C10 C5 C4 121.1(2) . . ? C6 C5 C4 121.6(2) . . ? C5 C6 C7 121.3(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 122.3(2) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 115.6(2) . . ? C7 C8 C11 123.06(19) . . ? C9 C8 C11 121.3(2) . . ? C10 C9 C8 122.2(2) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C5 C10 C9 121.5(2) . . ? C5 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C16 C11 C12 116.1(2) . . ? C16 C11 C8 121.7(2) . . ? C12 C11 C8 122.23(19) . . ? C13 C12 C11 121.7(2) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C14 C13 C12 121.5(2) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.3(2) . . ? C13 C14 C20 122.1(2) . . ? C15 C14 C20 120.6(2) . . ? C16 C15 C14 121.2(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 122.1(2) . . ? C15 C16 H16 119.0 . . ? C11 C16 H16 119.0 . . ? N4 C17 N3 112.8(3) . . ? N4 C17 H17 123.6 . . ? N3 C17 H17 123.6 . . ? N4 C18 C19 111.6(3) . . ? N4 C18 H18 124.2 . . ? C19 C18 H18 124.2 . . ? N3 C19 C18 105.9(3) . . ? N3 C19 H19 127.1 . . ? C18 C19 H19 127.1 . . ? N3 C20 C14 113.39(18) . . ? N3 C20 H20A 108.9 . . ? C14 C20 H20A 108.9 . . ? N3 C20 H20B 108.9 . . ? C14 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C1 N1 C3 106.1(2) . . ? C1 N1 C4 127.2(2) . . ? C3 N1 C4 126.4(2) . . ? C1 N2 C2 104.5(2) . . ? C17 N3 C19 105.8(2) . . ? C17 N3 C20 127.2(3) . . ? C19 N3 C20 127.0(2) . . ? C17 N4 C18 103.9(3) . . ? H1W O1 H2W 105(2) . . ? H1W O1 H3W 108(2) . . ? H2W O1 H3W 107(2) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.136 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.034 data_lu746_BimbH.PF6 _database_code_depnum_ccdc_archive 'CCDC 680067' _chemical_formula_sum 'C20 H19 F6 N4 P' _chemical_formula_weight 460.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.459(2) _cell_length_b 14.670(3) _cell_length_c 15.634(3) _cell_angle_alpha 75.506(2) _cell_angle_beta 75.031(3) _cell_angle_gamma 88.204(3) _cell_volume 2027.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2514 _cell_measurement_theta_min 2 _cell_measurement_theta_max 21 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6511 _exptl_absorpt_correction_T_max 0.7459 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 24236 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 29.29 _reflns_number_total 10081 _reflns_number_observed 4516 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. ; _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^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10081 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1651 _refine_ls_R_factor_obs 0.0727 _refine_ls_wR_factor_all 0.2447 _refine_ls_wR_factor_obs 0.1873 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 P1 P 0.89815(12) 0.87762(7) 0.43384(7) 0.0377(3) Uani 1 1 d . . . P2 P 0.87894(13) 0.57663(9) 0.25189(8) 0.0501(3) Uani 1 1 d . . . C105 C 0.4278(4) 0.7024(2) 0.0231(2) 0.0313(8) Uani 1 1 d . . . N8 N 0.4530(4) 0.9797(2) 0.3793(2) 0.0429(9) Uani 1 1 d . . . N4 N 0.6398(4) 0.5199(2) -0.3302(2) 0.0364(8) Uani 1 1 d . . . N1 N 0.3482(4) 0.7641(2) 0.3293(2) 0.0375(8) Uani 1 1 d . . . N2 N 0.5813(3) 1.0582(2) 0.2438(2) 0.0330(7) Uani 1 1 d . . . C10 C 0.6010(6) 0.4693(3) -0.2331(2) 0.0473(11) Uani 1 1 d . . . H10A H 0.6855 0.4366 -0.2181 0.057 Uiso 1 1 calc R . . H10B H 0.5238 0.4225 -0.2220 0.057 Uiso 1 1 calc R . . N3 N 1.2086(4) 0.7550(2) -0.3537(2) 0.0360(8) Uani 1 1 d . . . N6 N 0.6162(4) 0.5951(2) -0.4622(2) 0.0434(9) Uani 1 1 d . . . H6 H 0.5773 0.6200 -0.5063 0.052 Uiso 1 1 calc R . . F23 F 0.8488(5) 0.4979(2) 0.3470(2) 0.1076(13) Uani 1 1 d . . . C15 C 0.4659(4) 0.6492(3) -0.0486(3) 0.0341(9) Uani 1 1 d . . . C16 C 0.8977(4) 0.8980(3) -0.1803(2) 0.0316(8) Uani 1 1 d . . . H16 H 0.8654 0.9588 -0.1971 0.038 Uiso 1 1 calc R . . C17 C 0.8882(4) 0.8977(3) 0.0578(2) 0.0329(9) Uani 1 1 d . . . H17 H 0.9541 0.8506 0.0685 0.039 Uiso 1 1 calc R . . C18 C 0.5834(5) 0.9969(3) 0.3221(3) 0.0402(10) Uani 1 1 d . . . H18 H 0.6679 0.9693 0.3349 0.048 Uiso 1 1 calc R . . C19 C 0.8345(4) 0.9104(3) -0.0185(2) 0.0287(8) Uani 1 1 d . . . C101 C 0.3628(4) 0.7929(2) 0.1666(2) 0.0329(9) Uani 1 1 d . . . F25 F 1.0307(3) 0.5296(2) 0.2237(2) 0.0907(11) Uani 1 1 d . . . C22 C 0.7459(4) 1.0237(3) 0.1047(2) 0.0335(9) Uani 1 1 d . . . C100 C 0.3319(5) 0.8340(3) 0.2477(3) 0.0434(10) Uani 1 1 d . . . H10C H 0.3989 0.8873 0.2351 0.052 Uiso 1 1 calc R . . H10D H 0.2330 0.8565 0.2588 0.052 Uiso 1 1 calc R . . C24 C 0.8896(4) 0.8574(2) -0.0882(2) 0.0285(8) Uani 1 1 d . . . C25 C 0.5504(5) 0.5349(3) -0.1722(3) 0.0399(10) Uani 1 1 d . . . C102 C 0.5071(4) 0.7826(3) 0.1208(2) 0.0343(9) Uani 1 1 d . . . H102 H 0.5831 0.8062 0.1377 0.041 Uiso 1 1 calc R . . C103 C 0.5390(4) 0.7380(3) 0.0505(2) 0.0341(9) Uani 1 1 d . . . H103 H 0.6362 0.7316 0.0209 0.041 Uiso 1 1 calc R . . C28 C 1.0015(4) 0.7607(3) -0.2247(3) 0.0348(9) Uani 1 1 d . . . C107 C 0.5458(5) 0.5478(3) -0.3797(3) 0.0373(9) Uani 1 1 d . . . H107 H 0.4451 0.5360 -0.3594 0.045 Uiso 1 1 calc R . . F21 F 0.9196(4) 0.6516(3) 0.1596(2) 0.1154(14) Uani 1 1 d . . . F16 F 0.7330(3) 0.8461(2) 0.45268(19) 0.0776(9) Uani 1 1 d . . . C108 C 0.7613(5) 0.5978(3) -0.4658(3) 0.0471(11) Uani 1 1 d . . . H108 H 0.8361 0.6266 -0.5162 0.057 Uiso 1 1 calc R . . C33 C 0.7294(4) 0.9782(3) -0.0299(2) 0.0322(9) Uani 1 1 d . . . H33 H 0.6878 0.9857 -0.0789 0.039 Uiso 1 1 calc R . . F15 F 0.8496(4) 0.9744(2) 0.4494(3) 0.1156(14) Uani 1 1 d . . . N7 N 1.3695(4) 0.8476(2) -0.4583(2) 0.0421(9) Uani 1 1 d . . . H7 H 1.4101 0.8891 -0.5076 0.051 Uiso 1 1 calc R . . C36 C 1.0656(4) 0.7117(3) -0.2984(3) 0.0422(10) Uani 1 1 d . . . H36A H 1.0768 0.6457 -0.2712 0.051 Uiso 1 1 calc R . . H36B H 0.9996 0.7154 -0.3374 0.051 Uiso 1 1 calc R . . C37 C 0.9394(4) 0.7658(3) -0.0672(3) 0.0344(9) Uani 1 1 d . . . H37 H 0.9352 0.7362 -0.0065 0.041 Uiso 1 1 calc R . . C38 C 0.3735(4) 0.5768(3) -0.0485(3) 0.0374(9) Uani 1 1 d . . . H38 H 0.2816 0.5664 -0.0072 0.045 Uiso 1 1 calc R . . C39 C 0.4710(5) 0.7464(3) 0.3578(3) 0.0440(10) Uani 1 1 d . . . H39 H 0.5589 0.7808 0.3302 0.053 Uiso 1 1 calc R . . C41 C 0.5998(5) 0.6641(3) -0.1138(3) 0.0391(10) Uani 1 1 d . . . H41 H 0.6623 0.7132 -0.1169 0.047 Uiso 1 1 calc R . . C42 C 0.3607(4) 1.0341(3) 0.3345(3) 0.0418(10) Uani 1 1 d . . . H42 H 0.2603 1.0372 0.3580 0.050 Uiso 1 1 calc R . . C43 C 0.4161(5) 0.5208(3) -0.1086(3) 0.0402(10) Uani 1 1 d . . . H43 H 0.3531 0.4724 -0.1063 0.048 Uiso 1 1 calc R . . C44 C 0.4384(4) 1.0827(3) 0.2507(3) 0.0380(9) Uani 1 1 d . . . H44 H 0.4021 1.1243 0.2066 0.046 Uiso 1 1 calc R . . C45 C 1.2315(5) 0.8192(3) -0.4325(3) 0.0380(9) Uani 1 1 d . . . H45 H 1.1614 0.8407 -0.4643 0.046 Uiso 1 1 calc R . . N5 N 0.4509(4) 0.6742(2) 0.4296(2) 0.0472(9) Uani 1 1 d . . . C47 C 0.2525(5) 0.7589(3) 0.1383(3) 0.0392(10) Uani 1 1 d . . . H47 H 0.1553 0.7660 0.1674 0.047 Uiso 1 1 calc R . . F26 F 0.7303(5) 0.6170(3) 0.2817(5) 0.218(3) Uani 1 1 d . . . C49 C 0.9947(4) 0.7180(3) -0.1334(3) 0.0372(9) Uani 1 1 d . . . H49 H 1.0274 0.6573 -0.1171 0.045 Uiso 1 1 calc R . . C50 C 0.9517(4) 0.8510(3) -0.2469(2) 0.0345(9) Uani 1 1 d . . . H50 H 0.9549 0.8801 -0.3075 0.041 Uiso 1 1 calc R . . C109 C 0.7076(4) 1.0913(3) 0.1657(3) 0.0385(10) Uani 1 1 d . . . H10E H 0.7915 1.1002 0.1881 0.046 Uiso 1 1 calc R . . H10F H 0.6870 1.1520 0.1298 0.046 Uiso 1 1 calc R . . C52 C 0.8456(4) 0.9539(3) 0.1183(2) 0.0360(9) Uani 1 1 d . . . H52 H 0.8842 0.9448 0.1687 0.043 Uiso 1 1 calc R . . C104 C 0.2839(4) 0.7146(3) 0.0675(3) 0.0359(9) Uani 1 1 d . . . H104 H 0.2078 0.6928 0.0494 0.043 Uiso 1 1 calc R . . F24 F 0.9566(6) 0.6412(3) 0.2910(3) 0.154(2) Uani 1 1 d . . . C55 C 0.6422(5) 0.6078(3) -0.1740(3) 0.0422(10) Uani 1 1 d . . . H55 H 0.7331 0.6188 -0.2163 0.051 Uiso 1 1 calc R . . F22 F 0.8080(5) 0.5020(3) 0.2178(3) 0.1193(15) Uani 1 1 d . . . C57 C 0.3095(6) 0.6446(3) 0.4475(3) 0.0484(11) Uani 1 1 d . . . H57 H 0.2641 0.5945 0.4955 0.058 Uiso 1 1 calc R . . C58 C 1.3376(5) 0.7425(3) -0.3289(3) 0.0422(10) Uani 1 1 d . . . H58 H 1.3526 0.7015 -0.2763 0.051 Uiso 1 1 calc R . . C59 C 1.4386(5) 0.8004(3) -0.3945(3) 0.0425(10) Uani 1 1 d . . . H59 H 1.5368 0.8073 -0.3962 0.051 Uiso 1 1 calc R . . C60 C 0.6865(4) 1.0342(3) 0.0306(2) 0.0338(9) Uani 1 1 d . . . H60 H 0.6171 1.0795 0.0216 0.041 Uiso 1 1 calc R . . C61 C 0.7769(5) 0.5514(3) -0.3836(3) 0.0477(11) Uani 1 1 d . . . H61 H 0.8641 0.5423 -0.3661 0.057 Uiso 1 1 calc R . . C62 C 0.2434(5) 0.6982(3) 0.3857(3) 0.0466(11) Uani 1 1 d . . . H62 H 0.1476 0.6916 0.3824 0.056 Uiso 1 1 calc R . . F12 F 0.9453(4) 0.7808(2) 0.4160(3) 0.1215(15) Uani 1 1 d . . . F13 F 1.0669(3) 0.9068(2) 0.41190(18) 0.0687(8) Uani 1 1 d . . . F11 F 0.9071(3) 0.9186(3) 0.32955(18) 0.0931(12) Uani 1 1 d . . . F14 F 0.8889(4) 0.8366(3) 0.53731(19) 0.1027(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0361(6) 0.0349(6) 0.0376(6) -0.0043(5) -0.0063(5) 0.0028(5) P2 0.0463(7) 0.0452(7) 0.0487(7) -0.0058(6) 0.0006(6) -0.0061(6) C105 0.040(2) 0.0266(19) 0.0224(18) 0.0006(15) -0.0048(16) -0.0044(16) N8 0.050(2) 0.043(2) 0.0313(18) -0.0110(16) -0.0004(16) -0.0015(17) N4 0.055(2) 0.0281(17) 0.0290(17) -0.0083(14) -0.0151(16) 0.0037(15) N1 0.049(2) 0.0322(18) 0.0263(17) -0.0041(14) -0.0054(15) 0.0067(16) N2 0.0328(18) 0.0358(18) 0.0282(17) -0.0084(14) -0.0039(14) 0.0015(14) C10 0.086(3) 0.031(2) 0.024(2) -0.0031(17) -0.017(2) 0.002(2) N3 0.0389(19) 0.0318(18) 0.0344(18) -0.0093(15) -0.0038(15) 0.0037(15) N6 0.063(3) 0.0382(19) 0.0297(18) -0.0059(15) -0.0167(17) 0.0082(18) F23 0.156(4) 0.087(2) 0.0532(19) -0.0003(18) 0.008(2) -0.033(2) C15 0.038(2) 0.030(2) 0.032(2) -0.0008(16) -0.0110(17) -0.0033(17) C16 0.034(2) 0.0260(19) 0.032(2) -0.0032(16) -0.0086(16) 0.0001(16) C17 0.029(2) 0.037(2) 0.0269(19) -0.0023(17) -0.0038(16) 0.0024(17) C18 0.041(2) 0.045(2) 0.035(2) -0.0089(19) -0.0109(19) 0.0054(19) C19 0.0252(18) 0.032(2) 0.0234(18) -0.0033(15) 0.0003(14) -0.0040(15) C101 0.046(2) 0.0246(19) 0.0243(19) 0.0000(15) -0.0077(17) -0.0001(17) F25 0.0534(19) 0.087(2) 0.114(3) -0.003(2) -0.0122(18) 0.0097(17) C22 0.032(2) 0.036(2) 0.027(2) -0.0056(17) 0.0014(16) -0.0064(17) C100 0.062(3) 0.031(2) 0.033(2) -0.0028(17) -0.009(2) 0.008(2) C24 0.0246(18) 0.0289(19) 0.0286(19) -0.0027(16) -0.0049(15) -0.0009(15) C25 0.064(3) 0.033(2) 0.024(2) -0.0038(17) -0.0163(19) 0.001(2) C102 0.041(2) 0.030(2) 0.030(2) -0.0036(16) -0.0089(17) -0.0082(17) C103 0.033(2) 0.036(2) 0.030(2) -0.0072(17) -0.0021(16) -0.0046(17) C28 0.033(2) 0.032(2) 0.034(2) -0.0083(17) 0.0011(17) -0.0074(17) C107 0.044(2) 0.034(2) 0.035(2) -0.0092(18) -0.0114(19) 0.0049(18) F21 0.109(3) 0.116(3) 0.080(2) 0.045(2) -0.020(2) 0.008(2) F16 0.0353(15) 0.097(2) 0.074(2) 0.0194(17) -0.0064(13) -0.0097(15) C108 0.055(3) 0.042(2) 0.040(2) -0.011(2) -0.003(2) -0.010(2) C33 0.034(2) 0.037(2) 0.0249(19) -0.0064(17) -0.0072(16) -0.0017(17) F15 0.132(3) 0.056(2) 0.145(3) -0.044(2) 0.005(3) 0.023(2) N7 0.055(2) 0.0383(19) 0.0260(17) -0.0083(15) 0.0033(16) -0.0051(17) C36 0.043(2) 0.037(2) 0.041(2) -0.0124(19) 0.0003(19) -0.0063(19) C37 0.029(2) 0.038(2) 0.030(2) 0.0006(17) -0.0059(16) -0.0014(17) C38 0.039(2) 0.039(2) 0.034(2) -0.0052(18) -0.0135(18) 0.0011(18) C39 0.051(3) 0.042(2) 0.040(2) -0.011(2) -0.013(2) 0.006(2) C41 0.047(3) 0.036(2) 0.032(2) -0.0080(18) -0.0060(18) -0.0085(19) C42 0.030(2) 0.048(3) 0.047(3) -0.018(2) -0.0034(19) 0.0028(19) C43 0.056(3) 0.033(2) 0.036(2) -0.0054(18) -0.021(2) -0.0036(19) C44 0.034(2) 0.042(2) 0.039(2) -0.0125(19) -0.0097(18) 0.0081(18) C45 0.047(3) 0.038(2) 0.027(2) -0.0092(17) -0.0041(18) 0.0004(19) N5 0.069(3) 0.039(2) 0.0323(19) -0.0086(16) -0.0128(18) 0.0134(19) C47 0.042(2) 0.036(2) 0.032(2) -0.0003(18) -0.0046(18) 0.0079(18) F26 0.082(3) 0.081(3) 0.378(8) -0.007(4) 0.086(4) 0.026(2) C49 0.041(2) 0.028(2) 0.038(2) -0.0062(18) -0.0043(18) 0.0040(17) C50 0.037(2) 0.038(2) 0.0233(19) -0.0026(17) -0.0045(16) -0.0028(18) C109 0.033(2) 0.043(2) 0.034(2) -0.0087(18) 0.0027(17) -0.0062(18) C52 0.033(2) 0.047(2) 0.027(2) -0.0063(18) -0.0087(16) -0.0010(18) C104 0.037(2) 0.033(2) 0.035(2) 0.0007(17) -0.0135(18) -0.0026(17) F24 0.241(6) 0.108(3) 0.111(3) -0.048(3) -0.012(3) -0.090(3) C55 0.052(3) 0.038(2) 0.031(2) -0.0053(18) -0.0018(19) -0.004(2) F22 0.143(4) 0.096(3) 0.164(4) -0.038(3) -0.111(3) -0.004(2) C57 0.072(3) 0.033(2) 0.032(2) -0.0048(18) -0.002(2) 0.006(2) C58 0.050(3) 0.037(2) 0.034(2) -0.0062(19) -0.006(2) 0.006(2) C59 0.042(2) 0.045(2) 0.039(2) -0.014(2) -0.0037(19) 0.001(2) C60 0.033(2) 0.033(2) 0.030(2) -0.0036(17) -0.0045(16) 0.0016(17) C61 0.048(3) 0.048(3) 0.049(3) -0.011(2) -0.014(2) -0.010(2) C62 0.047(3) 0.046(3) 0.039(2) -0.004(2) -0.005(2) 0.005(2) F12 0.083(3) 0.0563(19) 0.207(4) -0.060(3) 0.021(3) -0.0008(18) F13 0.0498(17) 0.085(2) 0.0667(19) -0.0007(16) -0.0214(14) -0.0210(15) F11 0.0579(19) 0.164(3) 0.0410(16) 0.0025(19) -0.0099(14) -0.017(2) F14 0.086(2) 0.161(3) 0.0433(17) 0.015(2) -0.0256(16) -0.005(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 P1 F15 1.536(3) . ? P1 F12 1.546(3) . ? P1 F14 1.559(3) . ? P1 F11 1.571(3) . ? P1 F16 1.575(3) . ? P1 F13 1.592(3) . ? P2 F26 1.513(4) . ? P2 F24 1.541(4) . ? P2 F21 1.544(3) . ? P2 F22 1.567(3) . ? P2 F25 1.579(3) . ? P2 F23 1.602(3) . ? C105 C104 1.387(5) . ? C105 C103 1.394(5) . ? C105 C15 1.486(5) . ? N8 C18 1.312(5) . ? N8 C42 1.372(5) . ? N4 C107 1.316(5) . ? N4 C61 1.370(5) . ? N4 C10 1.469(5) . ? N1 C39 1.344(5) . ? N1 C62 1.370(5) . ? N1 C100 1.462(5) . ? N2 C18 1.331(5) . ? N2 C44 1.371(5) . ? N2 C109 1.463(4) . ? C10 C25 1.501(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N3 C45 1.321(5) . ? N3 C58 1.367(5) . ? N3 C36 1.468(5) . ? N6 C107 1.314(5) . ? N6 C108 1.361(5) . ? N6 H6 0.8600 . ? C15 C41 1.389(5) . ? C15 C38 1.396(5) . ? C16 C50 1.373(5) . ? C16 C24 1.397(5) . ? C16 H16 0.9300 . ? C17 C19 1.382(5) . ? C17 C52 1.383(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C33 1.396(5) . ? C19 C24 1.473(5) . ? C101 C47 1.384(5) . ? C101 C102 1.391(5) . ? C101 C100 1.495(5) . ? C22 C52 1.384(5) . ? C22 C60 1.386(5) . ? C22 C109 1.516(5) . ? C100 H10C 0.9700 . ? C100 H10D 0.9700 . ? C24 C37 1.399(5) . ? C25 C43 1.381(6) . ? C25 C55 1.388(6) . ? C102 C103 1.380(5) . ? C102 H102 0.9300 . ? C103 H103 0.9300 . ? C28 C50 1.383(5) . ? C28 C49 1.393(5) . ? C28 C36 1.497(5) . ? C107 H107 0.9300 . ? C108 C61 1.338(6) . ? C108 H108 0.9300 . ? C33 C60 1.380(5) . ? C33 H33 0.9300 . ? N7 C45 1.311(5) . ? N7 C59 1.366(5) . ? N7 H7 0.8600 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C49 1.377(5) . ? C37 H37 0.9300 . ? C38 C43 1.374(5) . ? C38 H38 0.9300 . ? C39 N5 1.313(5) . ? C39 H39 0.9300 . ? C41 C55 1.379(5) . ? C41 H41 0.9300 . ? C42 C44 1.353(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? N5 C57 1.356(6) . ? C47 C104 1.383(5) . ? C47 H47 0.9300 . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C52 H52 0.9300 . ? C104 H104 0.9300 . ? C55 H55 0.9300 . ? C57 C62 1.358(6) . ? C57 H57 0.9300 . ? C58 C59 1.340(5) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? 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 F15 P1 F12 178.5(3) . . ? F15 P1 F14 91.8(2) . . ? F12 P1 F14 89.5(2) . . ? F15 P1 F11 88.4(2) . . ? F12 P1 F11 90.3(2) . . ? F14 P1 F11 179.7(2) . . ? F15 P1 F16 89.7(2) . . ? F12 P1 F16 89.63(19) . . ? F14 P1 F16 89.26(17) . . ? F11 P1 F16 90.53(16) . . ? F15 P1 F13 92.3(2) . . ? F12 P1 F13 88.33(18) . . ? F14 P1 F13 91.94(17) . . ? F11 P1 F13 88.26(15) . . ? F16 P1 F13 177.62(18) . . ? F26 P2 F24 93.6(3) . . ? F26 P2 F21 92.9(3) . . ? F24 P2 F21 87.8(2) . . ? F26 P2 F22 90.3(3) . . ? F24 P2 F22 173.9(3) . . ? F21 P2 F22 96.7(2) . . ? F26 P2 F25 177.2(2) . . ? F24 P2 F25 87.8(3) . . ? F21 P2 F25 89.56(19) . . ? F22 P2 F25 88.1(2) . . ? F26 P2 F23 90.8(3) . . ? F24 P2 F23 90.4(2) . . ? F21 P2 F23 176.0(2) . . ? F22 P2 F23 84.9(2) . . ? F25 P2 F23 86.8(2) . . ? C104 C105 C103 118.0(3) . . ? C104 C105 C15 122.3(3) . . ? C103 C105 C15 119.6(3) . . ? C18 N8 C42 105.2(3) . . ? C107 N4 C61 108.0(3) . . ? C107 N4 C10 125.1(4) . . ? C61 N4 C10 126.8(4) . . ? C39 N1 C62 107.3(3) . . ? C39 N1 C100 126.8(4) . . ? C62 N1 C100 125.6(4) . . ? C18 N2 C44 106.6(3) . . ? C18 N2 C109 126.0(3) . . ? C44 N2 C109 127.4(3) . . ? N4 C10 C25 111.8(3) . . ? N4 C10 H10A 109.3 . . ? C25 C10 H10A 109.3 . . ? N4 C10 H10B 109.3 . . ? C25 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C45 N3 C58 108.4(3) . . ? C45 N3 C36 125.3(4) . . ? C58 N3 C36 126.1(3) . . ? C107 N6 C108 108.1(4) . . ? C107 N6 H6 126.0 . . ? C108 N6 H6 126.0 . . ? C41 C15 C38 117.3(4) . . ? C41 C15 C105 121.4(3) . . ? C38 C15 C105 121.1(4) . . ? C50 C16 C24 122.1(3) . . ? C50 C16 H16 119.0 . . ? C24 C16 H16 119.0 . . ? C19 C17 C52 121.1(4) . . ? C19 C17 H17 119.4 . . ? C52 C17 H17 119.4 . . ? N8 C18 N2 112.4(4) . . ? N8 C18 H18 123.8 . . ? N2 C18 H18 123.8 . . ? C17 C19 C33 118.0(3) . . ? C17 C19 C24 121.6(3) . . ? C33 C19 C24 120.3(3) . . ? C47 C101 C102 118.0(3) . . ? C47 C101 C100 122.3(4) . . ? C102 C101 C100 119.5(4) . . ? C52 C22 C60 118.7(4) . . ? C52 C22 C109 121.3(4) . . ? C60 C22 C109 119.9(4) . . ? N1 C100 C101 111.1(3) . . ? N1 C100 H10C 109.4 . . ? C101 C100 H10C 109.4 . . ? N1 C100 H10D 109.4 . . ? C101 C100 H10D 109.4 . . ? H10C C100 H10D 108.0 . . ? C16 C24 C37 116.4(3) . . ? C16 C24 C19 120.9(3) . . ? C37 C24 C19 122.7(3) . . ? C43 C25 C55 118.0(4) . . ? C43 C25 C10 121.2(4) . . ? C55 C25 C10 120.6(4) . . ? C103 C102 C101 120.8(4) . . ? C103 C102 H102 119.6 . . ? C101 C102 H102 119.6 . . ? C102 C103 C105 121.1(4) . . ? C102 C103 H103 119.5 . . ? C105 C103 H103 119.5 . . ? C50 C28 C49 118.8(4) . . ? C50 C28 C36 120.0(4) . . ? C49 C28 C36 121.2(4) . . ? N6 C107 N4 109.5(4) . . ? N6 C107 H107 125.3 . . ? N4 C107 H107 125.3 . . ? C61 C108 N6 107.6(4) . . ? C61 C108 H108 126.2 . . ? N6 C108 H108 126.2 . . ? C60 C33 C19 120.8(3) . . ? C60 C33 H33 119.6 . . ? C19 C33 H33 119.6 . . ? C45 N7 C59 109.1(3) . . ? C45 N7 H7 125.5 . . ? C59 N7 H7 125.5 . . ? N3 C36 C28 110.6(3) . . ? N3 C36 H36A 109.5 . . ? C28 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C49 C37 C24 122.1(4) . . ? C49 C37 H37 118.9 . . ? C24 C37 H37 118.9 . . ? C43 C38 C15 121.0(4) . . ? C43 C38 H38 119.5 . . ? C15 C38 H38 119.5 . . ? N5 C39 N1 111.3(4) . . ? N5 C39 H39 124.3 . . ? N1 C39 H39 124.3 . . ? C55 C41 C15 121.5(4) . . ? C55 C41 H41 119.3 . . ? C15 C41 H41 119.3 . . ? C44 C42 N8 109.5(4) . . ? C44 C42 H42 125.3 . . ? N8 C42 H42 125.3 . . ? C38 C43 C25 121.5(4) . . ? C38 C43 H43 119.3 . . ? C25 C43 H43 119.3 . . ? C42 C44 N2 106.4(4) . . ? C42 C44 H44 126.8 . . ? N2 C44 H44 126.8 . . ? N7 C45 N3 108.6(4) . . ? N7 C45 H45 125.7 . . ? N3 C45 H45 125.7 . . ? C39 N5 C57 105.5(4) . . ? C104 C47 C101 121.3(4) . . ? C104 C47 H47 119.3 . . ? C101 C47 H47 119.3 . . ? C37 C49 C28 120.0(4) . . ? C37 C49 H49 120.0 . . ? C28 C49 H49 120.0 . . ? C16 C50 C28 120.6(3) . . ? C16 C50 H50 119.7 . . ? C28 C50 H50 119.7 . . ? N2 C109 C22 112.9(3) . . ? N2 C109 H10E 109.0 . . ? C22 C109 H10E 109.0 . . ? N2 C109 H10F 109.0 . . ? C22 C109 H10F 109.0 . . ? H10E C109 H10F 107.8 . . ? C17 C52 C22 120.6(4) . . ? C17 C52 H52 119.7 . . ? C22 C52 H52 119.7 . . ? C47 C104 C105 120.7(4) . . ? C47 C104 H104 119.7 . . ? C105 C104 H104 119.7 . . ? C41 C55 C25 120.7(4) . . ? C41 C55 H55 119.6 . . ? C25 C55 H55 119.6 . . ? N5 C57 C62 110.6(4) . . ? N5 C57 H57 124.7 . . ? C62 C57 H57 124.7 . . ? C59 C58 N3 107.2(4) . . ? C59 C58 H58 126.4 . . ? N3 C58 H58 126.4 . . ? C58 C59 N7 106.7(4) . . ? C58 C59 H59 126.6 . . ? N7 C59 H59 126.6 . . ? C33 C60 C22 120.6(4) . . ? C33 C60 H60 119.7 . . ? C22 C60 H60 119.7 . . ? C108 C61 N4 106.9(4) . . ? C108 C61 H61 126.6 . . ? N4 C61 H61 126.6 . . ? C57 C62 N1 105.2(4) . . ? C57 C62 H62 127.4 . . ? N1 C62 H62 127.4 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.681 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.081 data_1_lu667_Cd(bimb)(H2O)(SO4) _database_code_depnum_ccdc_archive 'CCDC 680068' _chemical_formula_sum 'C20 H20 Cd N4 O5 S' _chemical_formula_weight 540.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pnma ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.6483(4) _cell_length_b 30.7546(16) _cell_length_c 11.2156(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2638.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3320 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description colum _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 10 _diffrn_reflns_number 33232 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2372 _reflns_number_observed 2003 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The crystal is unstable in air, was collected under mineral oil. The structure contains disordered solvents Methanol and water. Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.0702 for 1915 Fo > 4sig(Fo) and 0.0904 for all 2372 data for 193 parameters refined using 3 restraints ; _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^)+(0.0669P)^2^+9.5023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2372 _refine_ls_number_parameters 148 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_obs 0.0609 _refine_ls_wR_factor_all 0.1579 _refine_ls_wR_factor_obs 0.1503 _refine_ls_goodness_of_fit_all 1.156 _refine_ls_restrained_S_all 1.160 _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 C1 C -0.4054(9) 0.3477(2) -0.3766(6) 0.0456(16) Uani 1 1 d . . . H1 H -0.3798 0.3384 -0.4536 0.055 Uiso 1 1 calc R . . C2 C -0.4601(9) 0.3484(2) -0.1884(6) 0.0446(16) Uani 1 1 d . . . H2 H -0.4806 0.3391 -0.1107 0.053 Uiso 1 1 calc R . . C3 C -0.4588(11) 0.3898(3) -0.2250(7) 0.060(2) Uani 1 1 d . . . H3 H -0.4767 0.4143 -0.1780 0.072 Uiso 1 1 calc R . . C4 C -0.4115(10) 0.4271(3) -0.4233(8) 0.061(2) Uani 1 1 d . . . H4A H -0.3624 0.4183 -0.4993 0.073 Uiso 1 1 calc R . . H4B H -0.3333 0.4483 -0.3877 0.073 Uiso 1 1 calc R . . C5 C -0.5910(11) 0.4478(3) -0.4434(7) 0.059(2) Uani 1 1 d . . . C6 C -0.6451(10) 0.4828(2) -0.3753(8) 0.057(2) Uani 1 1 d . . . H6 H -0.5737 0.4932 -0.3145 0.069 Uiso 1 1 calc R . . C7 C -0.8072(9) 0.5028(2) -0.3972(6) 0.0490(18) Uani 1 1 d . . . H7 H -0.8426 0.5258 -0.3491 0.059 Uiso 1 1 calc R . . C8 C -0.9144(11) 0.4893(2) -0.4876(7) 0.058(2) Uani 1 1 d . . . C9 C -0.8572(13) 0.4531(3) -0.5530(8) 0.084(3) Uani 1 1 d . . . H9 H -0.9278 0.4423 -0.6135 0.100 Uiso 1 1 calc R . . C10 C -0.6995(13) 0.4334(3) -0.5299(8) 0.080(3) Uani 1 1 d . . . H10 H -0.6667 0.4093 -0.5750 0.096 Uiso 1 1 calc R . . N1 N -0.4258(7) 0.32166(17) -0.2845(5) 0.0411(13) Uani 1 1 d . . . N2 N -0.4262(7) 0.38920(18) -0.3448(5) 0.0466(14) Uani 1 1 d . . . O1W O -0.1934(8) 0.2500 -0.1231(5) 0.0402(15) Uani 1 2 d S . . H1W1 H -0.2075 0.2244 -0.0735 0.048 Uiso 0.50 1 calc PR . . H1W2 H -0.2075 0.2756 -0.0735 0.048 Uiso 0.50 1 calc PR . . O11 O -0.5820(8) 0.2886(3) 0.0645(6) 0.102(3) Uani 1 1 d D . . O12 O -0.6148(8) 0.2500 -0.1199(5) 0.0421(15) Uani 1 2 d SD . . O13 O -0.8502(9) 0.2500 0.0159(6) 0.080(3) Uani 1 2 d SD . . S S -0.6551(3) 0.2500 0.0077(2) 0.0568(8) Uani 1 2 d S . . Cd Cd -0.40477(9) 0.2500 -0.28167(5) 0.0371(2) Uani 1 2 d S . . 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 C1 0.041(4) 0.049(4) 0.047(4) 0.006(3) 0.004(3) 0.006(3) C2 0.045(4) 0.045(4) 0.043(4) 0.004(3) 0.004(3) 0.011(3) C3 0.063(5) 0.052(4) 0.065(5) 0.000(4) 0.014(4) 0.019(4) C4 0.058(5) 0.052(4) 0.072(5) 0.023(4) 0.009(4) 0.019(4) C5 0.063(5) 0.057(5) 0.058(4) 0.016(4) 0.006(4) 0.023(4) C6 0.054(5) 0.045(4) 0.073(5) 0.015(4) 0.003(4) 0.009(3) C7 0.047(4) 0.040(4) 0.060(5) 0.006(3) 0.007(4) 0.011(3) C8 0.072(5) 0.048(4) 0.053(4) 0.006(3) -0.005(4) 0.024(4) C9 0.099(7) 0.085(6) 0.066(5) -0.022(5) -0.024(5) 0.055(6) C10 0.101(7) 0.071(6) 0.068(5) -0.011(5) -0.020(6) 0.053(5) N1 0.038(3) 0.044(3) 0.042(3) 0.005(2) -0.001(3) 0.000(2) N2 0.038(3) 0.047(3) 0.055(4) 0.007(3) 0.009(3) 0.016(3) O1W 0.049(4) 0.042(4) 0.029(3) 0.000 0.005(3) 0.000 O11 0.058(4) 0.173(7) 0.076(4) -0.077(5) 0.008(3) -0.016(4) O12 0.042(4) 0.053(4) 0.031(3) 0.000 0.004(3) 0.000 O13 0.033(4) 0.164(9) 0.044(4) 0.000 0.008(3) 0.000 S 0.0331(12) 0.109(2) 0.0286(12) 0.000 0.0037(10) 0.000 Cd 0.0412(4) 0.0387(4) 0.0314(4) 0.000 0.0021(3) 0.000 _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 C1 N1 1.316(8) . ? C1 N2 1.336(9) . ? C1 H1 0.9300 . ? C2 C3 1.338(10) . ? C2 N1 1.380(8) . ? C2 H2 0.9300 . ? C3 N2 1.366(10) . ? C3 H3 0.9300 . ? C4 N2 1.466(9) . ? C4 C5 1.530(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.352(12) . ? C5 C6 1.384(11) . ? C6 C7 1.405(10) . ? C6 H6 0.9300 . ? C7 C8 1.368(11) . ? C7 H7 0.9300 . ? C8 C9 1.401(11) . ? C8 C8 1.492(15) 5_364 ? C9 C10 1.376(12) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? N1 Cd 2.210(5) . ? O1W Cd 2.404(6) . ? O1W Cd 2.453(6) 6_655 ? O1W H1W1 0.9700 . ? O1W H1W2 0.9700 . ? O11 S 1.458(7) . ? O12 S 1.464(6) . ? O12 Cd 2.423(6) . ? O12 Cd 2.477(6) 6 ? O13 S 1.495(8) . ? S O11 1.458(7) 8_565 ? Cd N1 2.210(5) 8_565 ? Cd O1W 2.453(6) 6 ? Cd O12 2.477(6) 6_655 ? Cd O13 2.660(7) 6_655 ? 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 N1 C1 N2 110.9(6) . . ? N1 C1 H1 124.5 . . ? N2 C1 H1 124.5 . . ? C3 C2 N1 109.0(6) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 106.9(7) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 C5 110.6(6) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C10 C5 C6 118.0(7) . . ? C10 C5 C4 121.3(8) . . ? C6 C5 C4 120.7(8) . . ? C5 C6 C7 120.5(8) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 121.7(7) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 116.2(7) . . ? C7 C8 C8 121.9(9) . 5_364 ? C9 C8 C8 121.8(10) . 5_364 ? C10 C9 C8 121.7(9) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C5 C10 C9 121.8(8) . . ? C5 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C1 N1 C2 105.9(6) . . ? C1 N1 Cd 127.5(5) . . ? C2 N1 Cd 126.6(4) . . ? C1 N2 C3 107.3(6) . . ? C1 N2 C4 126.2(6) . . ? C3 N2 C4 126.5(6) . . ? Cd O1W Cd 106.4(2) . 6_655 ? Cd O1W H1W1 110.4 . . ? Cd O1W H1W1 110.4 6_655 . ? Cd O1W H1W2 110.4 . . ? Cd O1W H1W2 110.4 6_655 . ? H1W1 O1W H1W2 108.6 . . ? S O12 Cd 150.6(4) . . ? S O12 Cd 104.3(3) . 6 ? Cd O12 Cd 105.1(2) . 6 ? O11 S O11 108.9(7) . 8_565 ? O11 S O12 110.3(3) . . ? O11 S O12 110.3(3) 8_565 . ? O11 S O13 110.9(3) . . ? O11 S O13 110.9(3) 8_565 . ? O12 S O13 105.7(4) . . ? N1 Cd N1 171.5(3) 8_565 . ? N1 Cd O1W 93.41(14) 8_565 . ? N1 Cd O1W 93.41(14) . . ? N1 Cd O12 87.84(14) 8_565 . ? N1 Cd O12 87.84(14) . . ? O1W Cd O12 83.8(2) . . ? N1 Cd O1W 85.88(14) 8_565 6 ? N1 Cd O1W 85.88(14) . 6 ? O1W Cd O1W 158.09(18) . 6 ? O12 Cd O1W 74.29(19) . 6 ? N1 Cd O12 93.38(14) 8_565 6_655 ? N1 Cd O12 93.38(14) . 6_655 ? O1W Cd O12 74.20(19) . 6_655 ? O12 Cd O12 157.99(17) . 6_655 ? O1W Cd O12 127.72(18) 6 6_655 ? N1 Cd O13 89.85(14) 8_565 6_655 ? N1 Cd O13 89.85(14) . 6_655 ? O1W Cd O13 128.7(2) . 6_655 ? O12 Cd O13 147.5(2) . 6_655 ? O1W Cd O13 73.2(2) 6 6_655 ? O12 Cd O13 54.5(2) 6_655 6_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.003 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.124 data_2_lu742_Cd(bimb)2(NO3)2 _database_code_depnum_ccdc_archive 'CCDC 680069' _chemical_formula_sum 'C40 H36 Cd N10 O6' _chemical_formula_weight 865.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 9.9460(8) _cell_length_b 13.3417(11) _cell_length_c 14.7986(12) _cell_angle_alpha 75.8580(10) _cell_angle_beta 87.6710(10) _cell_angle_gamma 81.2440(10) _cell_volume 1882.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5357 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71003 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 32457 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.49 _reflns_number_total 8774 _reflns_number_observed 6623 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. ; _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^)+(0.0501P)^2^+0.6685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8774 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_obs 0.0463 _refine_ls_wR_factor_all 0.1078 _refine_ls_wR_factor_obs 0.0975 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_restrained_S_all 1.027 _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 Cd Cd 0.23660(2) 0.014076(17) 0.249811(15) 0.02750(9) Uani 1 1 d . . . C1 C 0.0710(3) 0.1296(2) 0.3937(2) 0.0295(7) Uani 1 1 d . . . H1 H 0.0153 0.1675 0.3443 0.035 Uiso 1 1 calc R . . C15 C 0.7476(4) -0.2909(3) 0.1023(3) 0.0556(12) Uani 1 1 d . . . H15 H 0.8047 -0.2442 0.0718 0.067 Uiso 1 1 calc R . . N3 N 0.3001(3) -0.0431(2) 0.11883(18) 0.0317(6) Uani 1 1 d . . . N5 N 0.1062(3) 0.16377(19) 0.16651(17) 0.0277(6) Uani 1 1 d . . . C8 C -0.2968(4) 0.3791(3) 0.3303(3) 0.0466(10) Uani 1 1 d . . . H8 H -0.3801 0.3792 0.3040 0.056 Uiso 1 1 calc R . . O1 O 0.0352(3) -0.06569(19) 0.27269(17) 0.0427(6) Uani 1 1 d . . . C36 C 0.6971(3) -0.3477(2) 0.5127(2) 0.0248(6) Uani 1 1 d . . . N9 N -0.0101(3) -0.1215(2) 0.2268(2) 0.0404(7) Uani 1 1 d . . . C16 C 0.6138(3) -0.2747(2) 0.0772(2) 0.0278(7) Uani 1 1 d . . . N4 N 0.4371(3) -0.12189(19) 0.02908(18) 0.0290(6) Uani 1 1 d . . . N1 N 0.1799(3) 0.06401(19) 0.38487(18) 0.0292(6) Uani 1 1 d . . . O5 O 0.5377(3) 0.0856(2) 0.3473(2) 0.0697(9) Uani 1 1 d . . . C29 C -0.1738(3) 0.3968(2) -0.1708(2) 0.0264(7) Uani 1 1 d . . . H29 H -0.1279 0.3672 -0.2162 0.032 Uiso 1 1 calc R . . C22 C 0.1462(3) 0.2603(2) 0.1434(2) 0.0305(7) Uani 1 1 d . . . H22 H 0.2350 0.2732 0.1467 0.037 Uiso 1 1 calc R . . C10 C -0.2270(3) 0.4634(2) 0.2965(2) 0.0243(6) Uani 1 1 d . . . O4 O 0.4319(3) 0.1038(3) 0.22149(19) 0.0648(9) Uani 1 1 d . . . N6 N -0.0708(3) 0.28221(19) 0.11929(17) 0.0265(6) Uani 1 1 d . . . N7 N 0.3681(3) -0.13597(19) 0.33144(17) 0.0281(6) Uani 1 1 d . . . O3 O -0.0490(4) -0.0812(3) 0.1471(2) 0.1049(14) Uani 1 1 d . . . C25 C -0.2233(3) 0.3873(2) -0.0087(2) 0.0252(7) Uani 1 1 d . . . N8 N 0.5503(2) -0.24919(18) 0.37988(16) 0.0240(5) Uani 1 1 d . . . C19 C 0.2384(3) -0.0277(3) 0.0335(2) 0.0352(8) Uani 1 1 d . . . H19 H 0.1525 0.0096 0.0170 0.042 Uiso 1 1 calc R . . C30 C 0.7426(3) -0.5066(2) 0.8023(2) 0.0214(6) Uani 1 1 d . . . C37 C 0.6900(3) -0.2916(3) 0.4110(2) 0.0298(7) Uani 1 1 d . . . H37A H 0.7439 -0.2350 0.4004 0.036 Uiso 1 1 calc R . . H37B H 0.7293 -0.3398 0.3741 0.036 Uiso 1 1 calc R . . C27 C -0.1579(3) 0.3445(2) -0.0778(2) 0.0285(7) Uani 1 1 d . . . H27 H -0.1029 0.2799 -0.0618 0.034 Uiso 1 1 calc R . . C18 C 0.3229(3) -0.0753(3) -0.0221(2) 0.0348(8) Uani 1 1 d . . . H18 H 0.3067 -0.0762 -0.0834 0.042 Uiso 1 1 calc R . . O2 O -0.0082(4) -0.2142(2) 0.2607(2) 0.0748(10) Uani 1 1 d . . . C35 C 0.7356(3) -0.4552(2) 0.5397(2) 0.0305(7) Uani 1 1 d . . . H35 H 0.7515 -0.4936 0.4946 0.037 Uiso 1 1 calc R . . C31 C 0.7245(3) -0.4518(2) 0.7026(2) 0.0232(6) Uani 1 1 d . . . C38 C 0.4512(3) -0.3054(2) 0.3691(2) 0.0297(7) Uani 1 1 d . . . H38 H 0.4587 -0.3777 0.3804 0.036 Uiso 1 1 calc R . . C6 C -0.2471(4) 0.2959(3) 0.4010(3) 0.0455(10) Uani 1 1 d . . . H6 H -0.2978 0.2416 0.4224 0.055 Uiso 1 1 calc R . . O6 O 0.5759(4) 0.2010(3) 0.2201(2) 0.1019(15) Uani 1 1 d . . . C23 C 0.0380(3) 0.3341(2) 0.1152(2) 0.0331(8) Uani 1 1 d . . . H23 H 0.0377 0.4060 0.0966 0.040 Uiso 1 1 calc R . . C33 C 0.7505(3) -0.5057(2) 0.6327(2) 0.0289(7) Uani 1 1 d . . . H33 H 0.7786 -0.5775 0.6492 0.035 Uiso 1 1 calc R . . C17 C 0.5577(3) -0.1841(2) -0.0013(2) 0.0325(7) Uani 1 1 d . . . H17A H 0.6271 -0.1399 -0.0228 0.039 Uiso 1 1 calc R . . H17B H 0.5334 -0.2105 -0.0530 0.039 Uiso 1 1 calc R . . C5 C -0.1237(3) 0.2918(2) 0.4406(2) 0.0274(7) Uani 1 1 d . . . C34 C 0.6689(3) -0.2934(2) 0.5807(2) 0.0280(7) Uani 1 1 d . . . H34 H 0.6404 -0.2217 0.5638 0.034 Uiso 1 1 calc R . . N10 N 0.5208(3) 0.1275(2) 0.2619(2) 0.0366(7) Uani 1 1 d . . . C21 C -0.0254(3) 0.1804(2) 0.1504(2) 0.0299(7) Uani 1 1 d . . . H21 H -0.0799 0.1280 0.1596 0.036 Uiso 1 1 calc R . . C28 C -0.3235(3) 0.5347(2) -0.1273(2) 0.0244(6) Uani 1 1 d . . . H28 H -0.3810 0.5982 -0.1431 0.029 Uiso 1 1 calc R . . C40 C 0.4965(3) -0.1483(2) 0.3573(2) 0.0287(7) Uani 1 1 d . . . H40 H 0.5433 -0.0937 0.3595 0.034 Uiso 1 1 calc R . . C11 C 0.7190(3) -0.4459(2) 0.2206(2) 0.0254(6) Uani 1 1 d . . . C24 C -0.2101(3) 0.3302(3) 0.0934(2) 0.0333(8) Uani 1 1 d . . . H24A H -0.2411 0.3792 0.1313 0.040 Uiso 1 1 calc R . . H24B H -0.2686 0.2765 0.1064 0.040 Uiso 1 1 calc R . . C9 C -0.1014(3) 0.4576(3) 0.3364(2) 0.0345(8) Uani 1 1 d . . . H9 H -0.0498 0.5114 0.3150 0.041 Uiso 1 1 calc R . . C4 C -0.0662(3) 0.1997(2) 0.5166(2) 0.0316(7) Uani 1 1 d . . . H4A H -0.0358 0.2243 0.5677 0.038 Uiso 1 1 calc R . . H4B H -0.1367 0.1571 0.5401 0.038 Uiso 1 1 calc R . . C32 C 0.6823(3) -0.3444(2) 0.6745(2) 0.0271(7) Uani 1 1 d . . . H32 H 0.6627 -0.3061 0.7194 0.033 Uiso 1 1 calc R . . C13 C 0.7991(4) -0.3755(3) 0.1720(3) 0.0588(13) Uani 1 1 d . . . H13 H 0.8909 -0.3851 0.1866 0.071 Uiso 1 1 calc R . . C26 C -0.3055(3) 0.4832(2) -0.0343(2) 0.0274(7) Uani 1 1 d . . . H26 H -0.3491 0.5133 0.0115 0.033 Uiso 1 1 calc R . . C14 C 0.5324(3) -0.3450(2) 0.1249(2) 0.0324(7) Uani 1 1 d . . . H14 H 0.4411 -0.3359 0.1089 0.039 Uiso 1 1 calc R . . N2 N 0.0490(3) 0.13583(19) 0.48163(17) 0.0276(6) Uani 1 1 d . . . C3 C 0.1495(3) 0.0681(2) 0.5341(2) 0.0293(7) Uani 1 1 d . . . H3 H 0.1599 0.0545 0.5983 0.035 Uiso 1 1 calc R . . C2 C 0.2308(3) 0.0247(2) 0.4743(2) 0.0302(7) Uani 1 1 d . . . H2 H 0.3088 -0.0239 0.4906 0.036 Uiso 1 1 calc R . . C39 C 0.3399(3) -0.2352(2) 0.3385(2) 0.0280(7) Uani 1 1 d . . . H39 H 0.2568 -0.2516 0.3245 0.034 Uiso 1 1 calc R . . C20 C 0.4190(3) -0.0997(2) 0.1123(2) 0.0299(7) Uani 1 1 d . . . H20 H 0.4828 -0.1216 0.1600 0.036 Uiso 1 1 calc R . . C12 C 0.5833(3) -0.4284(2) 0.1957(2) 0.0322(7) Uani 1 1 d . . . H12 H 0.5254 -0.4738 0.2275 0.039 Uiso 1 1 calc R . . C7 C -0.0516(3) 0.3735(3) 0.4074(3) 0.0381(8) Uani 1 1 d . . . H7 H 0.0324 0.3721 0.4334 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.03257(14) 0.02101(12) 0.02411(13) -0.00024(8) -0.00357(9) 0.00344(9) C1 0.0329(17) 0.0277(17) 0.0263(17) -0.0069(13) -0.0048(13) 0.0019(14) C15 0.034(2) 0.063(3) 0.054(3) 0.027(2) -0.0068(18) -0.0236(19) N3 0.0380(16) 0.0281(14) 0.0258(14) -0.0037(11) -0.0085(12) 0.0021(12) N5 0.0320(14) 0.0229(13) 0.0260(14) -0.0022(10) -0.0066(11) -0.0016(11) C8 0.036(2) 0.051(2) 0.047(2) 0.0118(17) -0.0213(17) -0.0220(18) O1 0.0487(15) 0.0490(15) 0.0376(14) -0.0158(12) 0.0062(11) -0.0227(13) C36 0.0191(14) 0.0283(16) 0.0250(16) -0.0026(12) -0.0054(12) -0.0015(13) N9 0.0412(17) 0.0442(19) 0.0362(17) -0.0056(14) -0.0101(14) -0.0118(15) C16 0.0307(17) 0.0282(16) 0.0228(16) -0.0064(13) 0.0033(13) 0.0005(14) N4 0.0359(15) 0.0250(14) 0.0240(14) -0.0032(11) -0.0034(11) -0.0015(12) N1 0.0341(15) 0.0235(13) 0.0269(14) -0.0031(11) -0.0047(11) 0.0014(12) O5 0.101(3) 0.0544(18) 0.0521(19) -0.0040(14) -0.0341(17) -0.0114(17) C29 0.0198(15) 0.0292(16) 0.0289(17) -0.0052(13) -0.0016(12) -0.0023(13) C22 0.0311(17) 0.0270(17) 0.0319(18) -0.0012(13) -0.0074(14) -0.0078(14) C10 0.0213(15) 0.0308(16) 0.0208(15) -0.0062(12) -0.0004(12) -0.0041(13) O4 0.0581(18) 0.093(2) 0.0458(17) 0.0005(15) -0.0136(14) -0.0425(17) N6 0.0294(14) 0.0253(14) 0.0221(13) -0.0014(10) -0.0054(11) -0.0015(11) N7 0.0327(15) 0.0247(14) 0.0240(14) -0.0019(10) -0.0053(11) -0.0006(12) O3 0.135(3) 0.127(3) 0.053(2) 0.007(2) -0.049(2) -0.050(3) C25 0.0202(15) 0.0293(16) 0.0242(16) -0.0011(12) -0.0048(12) -0.0056(13) N8 0.0271(13) 0.0232(13) 0.0204(13) -0.0028(10) -0.0037(10) -0.0032(11) C19 0.0334(18) 0.0359(19) 0.0350(19) -0.0075(15) -0.0109(15) 0.0001(15) C30 0.0160(14) 0.0233(15) 0.0249(16) -0.0017(12) -0.0051(11) -0.0080(12) C37 0.0257(16) 0.0353(18) 0.0250(16) -0.0022(13) -0.0069(13) -0.0005(14) C27 0.0215(15) 0.0266(16) 0.0323(18) 0.0001(13) -0.0048(13) 0.0015(13) C18 0.0394(19) 0.0371(19) 0.0264(17) -0.0033(14) -0.0118(14) -0.0051(16) O2 0.111(3) 0.0443(18) 0.075(2) -0.0204(16) -0.020(2) -0.0155(18) C35 0.0394(19) 0.0288(17) 0.0253(17) -0.0090(13) -0.0048(14) -0.0060(14) C31 0.0192(14) 0.0230(15) 0.0271(16) -0.0032(12) -0.0035(12) -0.0055(12) C38 0.0323(17) 0.0186(15) 0.0370(18) -0.0041(13) -0.0098(14) -0.0018(13) C6 0.042(2) 0.044(2) 0.045(2) 0.0123(17) -0.0143(17) -0.0251(18) O6 0.151(4) 0.114(3) 0.073(2) -0.040(2) 0.045(2) -0.106(3) C23 0.0367(19) 0.0198(16) 0.041(2) -0.0019(14) -0.0103(15) -0.0056(14) C33 0.0360(18) 0.0191(15) 0.0310(18) -0.0037(13) -0.0067(14) -0.0044(13) C17 0.0360(18) 0.0306(17) 0.0264(17) -0.0022(13) 0.0028(14) 0.0010(15) C5 0.0261(16) 0.0294(16) 0.0247(16) -0.0062(13) 0.0018(13) 0.0004(13) C34 0.0292(16) 0.0224(15) 0.0290(17) -0.0022(13) -0.0051(13) 0.0015(13) N10 0.0376(17) 0.0312(16) 0.0436(18) -0.0095(13) -0.0030(14) -0.0116(13) C21 0.0350(18) 0.0227(16) 0.0291(17) 0.0020(13) -0.0083(14) -0.0063(14) C28 0.0217(15) 0.0199(15) 0.0301(17) -0.0026(12) -0.0050(12) -0.0030(12) C40 0.0332(17) 0.0239(16) 0.0282(17) -0.0042(13) -0.0065(13) -0.0037(14) C11 0.0201(15) 0.0312(16) 0.0248(16) -0.0056(13) -0.0013(12) -0.0050(13) C24 0.0275(17) 0.0394(19) 0.0258(17) 0.0021(14) -0.0010(13) 0.0017(15) C9 0.0220(16) 0.0311(18) 0.046(2) 0.0019(15) -0.0033(14) -0.0078(14) C4 0.0318(17) 0.0318(17) 0.0284(17) -0.0050(14) 0.0023(14) 0.0000(14) C32 0.0294(16) 0.0257(16) 0.0264(16) -0.0091(13) -0.0027(13) 0.0010(13) C13 0.0286(19) 0.070(3) 0.061(3) 0.029(2) -0.0168(18) -0.024(2) C26 0.0251(16) 0.0307(17) 0.0247(16) -0.0039(13) 0.0005(12) -0.0039(13) C14 0.0220(16) 0.0306(17) 0.042(2) -0.0016(14) -0.0069(14) -0.0054(14) N2 0.0293(14) 0.0257(14) 0.0256(14) -0.0025(11) -0.0022(11) -0.0027(11) C3 0.0336(17) 0.0276(17) 0.0246(16) -0.0009(13) -0.0064(13) -0.0049(14) C2 0.0350(18) 0.0233(16) 0.0282(17) 0.0006(13) -0.0084(14) -0.0001(14) C39 0.0298(17) 0.0238(16) 0.0296(17) -0.0025(13) -0.0058(13) -0.0059(13) C20 0.0366(18) 0.0291(17) 0.0216(16) -0.0055(13) -0.0072(13) 0.0033(15) C12 0.0241(16) 0.0275(17) 0.041(2) 0.0026(14) -0.0019(14) -0.0096(14) C7 0.0209(16) 0.0366(19) 0.050(2) 0.0022(16) -0.0075(15) -0.0031(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N1 2.281(3) . ? Cd N3 2.283(3) . ? Cd N7 2.308(2) . ? Cd N5 2.308(2) . ? Cd O1 2.382(2) . ? Cd O4 2.404(3) . ? C1 N1 1.309(4) . ? C1 N2 1.331(4) . ? C1 H1 0.9300 . ? C15 C16 1.367(5) . ? C15 C13 1.377(5) . ? C15 H15 0.9300 . ? N3 C20 1.316(4) . ? N3 C19 1.383(4) . ? N5 C21 1.316(4) . ? N5 C22 1.365(4) . ? C8 C6 1.371(5) . ? C8 C10 1.389(4) . ? C8 H8 0.9300 . ? O1 N9 1.262(3) . ? C36 C34 1.375(4) . ? C36 C35 1.389(4) . ? C36 C37 1.507(4) . ? N9 O2 1.214(4) . ? N9 O3 1.221(4) . ? C16 C14 1.376(4) . ? C16 C17 1.511(4) . ? N4 C20 1.335(4) . ? N4 C18 1.369(4) . ? N4 C17 1.472(4) . ? N1 C2 1.385(4) . ? O5 N10 1.257(4) . ? C29 C27 1.385(4) . ? C29 C30 1.400(4) 1_464 ? C29 H29 0.9300 . ? C22 C23 1.348(4) . ? C22 H22 0.9300 . ? C10 C9 1.388(4) . ? C10 C11 1.484(4) 1_465 ? O4 N10 1.209(4) . ? N6 C21 1.336(4) . ? N6 C23 1.363(4) . ? N6 C24 1.459(4) . ? N7 C40 1.323(4) . ? N7 C39 1.373(4) . ? C25 C27 1.384(4) . ? C25 C26 1.385(4) . ? C25 C24 1.517(4) . ? N8 C40 1.337(4) . ? N8 C38 1.362(4) . ? N8 C37 1.466(4) . ? C19 C18 1.351(5) . ? C19 H19 0.9300 . ? C30 C28 1.392(4) 1_646 ? C30 C29 1.400(4) 1_646 ? C30 C31 1.483(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C27 H27 0.9300 . ? C18 H18 0.9300 . ? C35 C33 1.380(4) . ? C35 H35 0.9300 . ? C31 C33 1.391(4) . ? C31 C32 1.394(4) . ? C38 C39 1.351(4) . ? C38 H38 0.9300 . ? C6 C5 1.369(4) . ? C6 H6 0.9300 . ? O6 N10 1.218(4) . ? C23 H23 0.9300 . ? C33 H33 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C5 C7 1.375(4) . ? C5 C4 1.505(4) . ? C34 C32 1.391(4) . ? C34 H34 0.9300 . ? C21 H21 0.9300 . ? C28 C26 1.387(4) . ? C28 C30 1.392(4) 1_464 ? C28 H28 0.9300 . ? C40 H40 0.9300 . ? C11 C13 1.373(4) . ? C11 C12 1.383(4) . ? C11 C10 1.484(4) 1_645 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C9 C7 1.380(4) . ? C9 H9 0.9300 . ? C4 N2 1.475(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C32 H32 0.9300 . ? C13 H13 0.9300 . ? C26 H26 0.9300 . ? C14 C12 1.377(4) . ? C14 H14 0.9300 . ? N2 C3 1.365(4) . ? C3 C2 1.350(4) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C39 H39 0.9300 . ? C20 H20 0.9300 . ? C12 H12 0.9300 . ? C7 H7 0.9300 . ? 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 N1 Cd N3 177.14(9) . . ? N1 Cd N7 90.60(9) . . ? N3 Cd N7 86.54(9) . . ? N1 Cd N5 90.08(9) . . ? N3 Cd N5 92.78(9) . . ? N7 Cd N5 179.31(9) . . ? N1 Cd O1 86.30(9) . . ? N3 Cd O1 93.93(9) . . ? N7 Cd O1 92.52(9) . . ? N5 Cd O1 87.67(9) . . ? N1 Cd O4 93.75(10) . . ? N3 Cd O4 86.19(10) . . ? N7 Cd O4 90.86(10) . . ? N5 Cd O4 88.94(10) . . ? O1 Cd O4 176.62(9) . . ? N1 C1 N2 112.3(3) . . ? N1 C1 H1 123.9 . . ? N2 C1 H1 123.9 . . ? C16 C15 C13 121.0(3) . . ? C16 C15 H15 119.5 . . ? C13 C15 H15 119.5 . . ? C20 N3 C19 105.4(3) . . ? C20 N3 Cd 121.7(2) . . ? C19 N3 Cd 132.9(2) . . ? C21 N5 C22 105.4(3) . . ? C21 N5 Cd 128.4(2) . . ? C22 N5 Cd 124.6(2) . . ? C6 C8 C10 122.3(3) . . ? C6 C8 H8 118.8 . . ? C10 C8 H8 118.8 . . ? N9 O1 Cd 129.9(2) . . ? C34 C36 C35 118.5(3) . . ? C34 C36 C37 120.8(3) . . ? C35 C36 C37 120.6(3) . . ? O2 N9 O3 121.5(4) . . ? O2 N9 O1 119.7(3) . . ? O3 N9 O1 118.7(3) . . ? C15 C16 C14 117.7(3) . . ? C15 C16 C17 121.3(3) . . ? C14 C16 C17 121.1(3) . . ? C20 N4 C18 107.0(3) . . ? C20 N4 C17 126.1(3) . . ? C18 N4 C17 127.0(3) . . ? C1 N1 C2 105.0(3) . . ? C1 N1 Cd 123.1(2) . . ? C2 N1 Cd 131.1(2) . . ? C27 C29 C30 121.3(3) . 1_464 ? C27 C29 H29 119.3 . . ? C30 C29 H29 119.3 1_464 . ? C23 C22 N5 109.9(3) . . ? C23 C22 H22 125.0 . . ? N5 C22 H22 125.0 . . ? C9 C10 C8 116.3(3) . . ? C9 C10 C11 121.2(3) . 1_465 ? C8 C10 C11 122.5(3) . 1_465 ? N10 O4 Cd 141.6(2) . . ? C21 N6 C23 107.2(3) . . ? C21 N6 C24 127.1(3) . . ? C23 N6 C24 125.7(3) . . ? C40 N7 C39 105.3(3) . . ? C40 N7 Cd 128.2(2) . . ? C39 N7 Cd 124.2(2) . . ? C27 C25 C26 118.7(3) . . ? C27 C25 C24 121.5(3) . . ? C26 C25 C24 119.7(3) . . ? C40 N8 C38 107.4(2) . . ? C40 N8 C37 126.3(3) . . ? C38 N8 C37 126.3(3) . . ? C18 C19 N3 109.1(3) . . ? C18 C19 H19 125.5 . . ? N3 C19 H19 125.5 . . ? C28 C30 C29 117.3(3) 1_646 1_646 ? C28 C30 C31 121.7(3) 1_646 . ? C29 C30 C31 121.0(3) 1_646 . ? N8 C37 C36 112.5(2) . . ? N8 C37 H37A 109.1 . . ? C36 C37 H37A 109.1 . . ? N8 C37 H37B 109.1 . . ? C36 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C25 C27 C29 120.6(3) . . ? C25 C27 H27 119.7 . . ? C29 C27 H27 119.7 . . ? C19 C18 N4 106.7(3) . . ? C19 C18 H18 126.7 . . ? N4 C18 H18 126.7 . . ? C33 C35 C36 120.6(3) . . ? C33 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C33 C31 C32 117.1(3) . . ? C33 C31 C30 121.2(3) . . ? C32 C31 C30 121.7(3) . . ? C39 C38 N8 106.4(3) . . ? C39 C38 H38 126.8 . . ? N8 C38 H38 126.8 . . ? C5 C6 C8 120.8(3) . . ? C5 C6 H6 119.6 . . ? C8 C6 H6 119.6 . . ? C22 C23 N6 106.1(3) . . ? C22 C23 H23 126.9 . . ? N6 C23 H23 126.9 . . ? C35 C33 C31 121.6(3) . . ? C35 C33 H33 119.2 . . ? C31 C33 H33 119.2 . . ? N4 C17 C16 111.2(2) . . ? N4 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? N4 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C6 C5 C7 118.0(3) . . ? C6 C5 C4 121.3(3) . . ? C7 C5 C4 120.6(3) . . ? C36 C34 C32 120.8(3) . . ? C36 C34 H34 119.6 . . ? C32 C34 H34 119.6 . . ? O4 N10 O6 117.1(3) . . ? O4 N10 O5 118.5(3) . . ? O6 N10 O5 123.6(3) . . ? N5 C21 N6 111.4(3) . . ? N5 C21 H21 124.3 . . ? N6 C21 H21 124.3 . . ? C26 C28 C30 121.3(3) . 1_464 ? C26 C28 H28 119.3 . . ? C30 C28 H28 119.3 1_464 . ? N7 C40 N8 111.3(3) . . ? N7 C40 H40 124.3 . . ? N8 C40 H40 124.3 . . ? C13 C11 C12 116.7(3) . . ? C13 C11 C10 122.5(3) . 1_645 ? C12 C11 C10 120.7(3) . 1_645 ? N6 C24 C25 112.7(2) . . ? N6 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? N6 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C7 C9 C10 121.1(3) . . ? C7 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? N2 C4 C5 110.9(2) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C34 C32 C31 121.2(3) . . ? C34 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C11 C13 C15 122.1(3) . . ? C11 C13 H13 119.0 . . ? C15 C13 H13 119.0 . . ? C25 C26 C28 120.7(3) . . ? C25 C26 H26 119.6 . . ? C28 C26 H26 119.6 . . ? C16 C14 C12 121.4(3) . . ? C16 C14 H14 119.3 . . ? C12 C14 H14 119.3 . . ? C1 N2 C3 107.1(3) . . ? C1 N2 C4 126.5(3) . . ? C3 N2 C4 126.4(3) . . ? C2 C3 N2 106.4(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? C3 C2 N1 109.2(3) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C38 C39 N7 109.6(3) . . ? C38 C39 H39 125.2 . . ? N7 C39 H39 125.2 . . ? N3 C20 N4 111.9(3) . . ? N3 C20 H20 124.1 . . ? N4 C20 H20 124.1 . . ? C14 C12 C11 121.2(3) . . ? C14 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C5 C7 C9 121.4(3) . . ? C5 C7 H7 119.3 . . ? C9 C7 H7 119.3 . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.902 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.087 data_3_lu727_Cd(bimb)(H2O)2(Tosylate)2 _database_code_depnum_ccdc_archive 'CCDC 680070' _chemical_formula_sum 'C34 H36 Cd N4 O8 S2' _chemical_formula_weight 805.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 7.7149(7) _cell_length_b 9.1923(9) _cell_length_c 12.6485(12) _cell_angle_alpha 91.8400(10) _cell_angle_beta 92.2170(10) _cell_angle_gamma 110.6680(10) _cell_volume 837.64(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3226 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 10334 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 29.39 _reflns_number_total 4214 _reflns_number_observed 3650 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. ; _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^)+(0.0384P)^2^+0.0036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4214 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_obs 0.0334 _refine_ls_wR_factor_all 0.0784 _refine_ls_wR_factor_obs 0.0739 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _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 Cd Cd 0.5000 0.5000 0.5000 0.03428(9) Uani 1 2 d S . . S S 0.20705(8) 0.56091(7) 0.68970(4) 0.03806(14) Uani 1 1 d . . . O1 O 0.3887(2) 0.5993(2) 0.64573(12) 0.0468(4) Uani 1 1 d . . . O3 O 0.1322(3) 0.6829(2) 0.67598(15) 0.0580(5) Uani 1 1 d . . . N1 N 0.5004(3) 0.7111(2) 0.41582(14) 0.0375(4) Uani 1 1 d . . . O2 O 0.0799(2) 0.4092(2) 0.65077(13) 0.0522(4) Uani 1 1 d . . . N2 N 0.4197(3) 0.9086(2) 0.37497(14) 0.0396(4) Uani 1 1 d . . . C10 C 0.0452(3) 0.9998(3) 0.05299(17) 0.0378(5) Uani 1 1 d . . . O4 O 0.1864(3) 0.3567(2) 0.45143(17) 0.0554(5) Uani 1 1 d . . . C1 C 0.3674(3) 0.7681(3) 0.41485(17) 0.0387(5) Uani 1 1 d . . . H1 H 0.2502 0.7167 0.4391 0.046 Uiso 1 1 calc R . . C5 C 0.2174(3) 0.9985(3) 0.25378(18) 0.0388(5) Uani 1 1 d . . . C8 C 0.1895(4) 0.9451(3) 0.06599(19) 0.0460(6) Uani 1 1 d . . . H8 H 0.2318 0.9082 0.0066 0.055 Uiso 1 1 calc R . . C2 C 0.6471(3) 0.8212(3) 0.37228(19) 0.0453(6) Uani 1 1 d . . . H2 H 0.7616 0.8125 0.3613 0.054 Uiso 1 1 calc R . . C6 C 0.0752(4) 1.0553(3) 0.2422(2) 0.0533(7) Uani 1 1 d . . . H6 H 0.0355 1.0942 0.3017 0.064 Uiso 1 1 calc R . . C16 C 0.3004(4) 0.5457(3) 1.04523(19) 0.0473(6) Uani 1 1 d . . . C3 C 0.5986(4) 0.9439(3) 0.3479(2) 0.0485(6) Uani 1 1 d . . . H3 H 0.6728 1.0349 0.3184 0.058 Uiso 1 1 calc R . . C7 C 0.2732(4) 0.9432(3) 0.1644(2) 0.0486(6) Uani 1 1 d . . . H7 H 0.3687 0.9038 0.1699 0.058 Uiso 1 1 calc R . . C12 C 0.1443(4) 0.4240(3) 0.8794(2) 0.0531(7) Uani 1 1 d . . . H12 H 0.0579 0.3385 0.8423 0.064 Uiso 1 1 calc R . . C13 C 0.3750(4) 0.6758(3) 0.8828(2) 0.0514(6) Uani 1 1 d . . . H13 H 0.4442 0.7629 0.8475 0.062 Uiso 1 1 calc R . . C14 C 0.1730(4) 0.4232(3) 0.9880(2) 0.0605(8) Uani 1 1 d . . . H14 H 0.1031 0.3364 1.0233 0.073 Uiso 1 1 calc R . . C4 C 0.3072(4) 1.0068(3) 0.3632(2) 0.0519(7) Uani 1 1 d . . . H4A H 0.3851 1.1139 0.3812 0.062 Uiso 1 1 calc R . . H4B H 0.2106 0.9767 0.4136 0.062 Uiso 1 1 calc R . . C15 C 0.4033(4) 0.6714(3) 0.9902(2) 0.0540(7) Uani 1 1 d . . . H15 H 0.4939 0.7550 1.0267 0.065 Uiso 1 1 calc R . . C9 C -0.0096(4) 1.0556(4) 0.1444(2) 0.0570(7) Uani 1 1 d . . . H9 H -0.1058 1.0941 0.1394 0.068 Uiso 1 1 calc R . . C11 C 0.2443(3) 0.5518(3) 0.82734(17) 0.0359(5) Uani 1 1 d . . . C17 C 0.3272(5) 0.5430(4) 1.1634(2) 0.0690(9) Uani 1 1 d . . . H17A H 0.2487 0.4444 1.1870 0.103 Uiso 1 1 calc R . . H17B H 0.2955 0.6248 1.1968 0.103 Uiso 1 1 calc R . . H17C H 0.4544 0.5581 1.1818 0.103 Uiso 1 1 calc R . . H4S H 0.122(5) 0.366(4) 0.404(3) 0.083 Uiso 1 1 d . . . H5S H 0.132(5) 0.369(4) 0.511(3) 0.083 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd 0.03794(14) 0.03681(14) 0.03126(13) 0.00647(9) 0.00102(9) 0.01685(10) S 0.0385(3) 0.0466(3) 0.0318(3) 0.0043(2) 0.0022(2) 0.0182(3) O1 0.0443(10) 0.0575(11) 0.0359(9) -0.0002(8) 0.0071(7) 0.0147(8) O3 0.0691(13) 0.0656(12) 0.0539(11) 0.0080(9) -0.0036(9) 0.0420(10) N1 0.0408(11) 0.0420(11) 0.0314(10) 0.0074(8) -0.0014(8) 0.0166(9) O2 0.0465(10) 0.0592(11) 0.0405(9) -0.0021(8) -0.0010(8) 0.0063(9) N2 0.0464(11) 0.0413(11) 0.0335(10) 0.0035(8) -0.0060(8) 0.0192(9) C10 0.0442(13) 0.0372(12) 0.0363(12) 0.0068(10) 0.0008(10) 0.0194(10) O4 0.0457(11) 0.0701(13) 0.0483(11) -0.0026(10) -0.0118(8) 0.0198(10) C1 0.0387(12) 0.0426(13) 0.0352(12) 0.0077(10) -0.0003(9) 0.0146(10) C5 0.0473(13) 0.0353(12) 0.0355(12) 0.0055(9) -0.0033(10) 0.0171(10) C8 0.0507(15) 0.0571(15) 0.0391(13) -0.0040(11) -0.0028(11) 0.0310(13) C2 0.0412(13) 0.0548(15) 0.0417(13) 0.0154(11) 0.0036(10) 0.0177(12) C6 0.0683(18) 0.0741(19) 0.0340(13) 0.0045(12) 0.0050(12) 0.0453(16) C16 0.0547(16) 0.0612(16) 0.0361(13) 0.0006(12) -0.0003(11) 0.0334(14) C3 0.0459(14) 0.0489(15) 0.0463(14) 0.0180(11) -0.0005(11) 0.0104(12) C7 0.0531(15) 0.0565(16) 0.0468(14) -0.0055(12) -0.0103(12) 0.0346(13) C12 0.0628(17) 0.0490(15) 0.0393(13) 0.0033(11) -0.0015(12) 0.0099(13) C13 0.0569(16) 0.0466(15) 0.0453(14) 0.0013(12) 0.0064(12) 0.0115(12) C14 0.076(2) 0.0545(17) 0.0424(15) 0.0128(13) 0.0027(14) 0.0119(15) C4 0.0691(18) 0.0540(16) 0.0422(14) -0.0029(12) -0.0113(12) 0.0357(14) C15 0.0538(16) 0.0599(17) 0.0456(15) -0.0135(13) -0.0046(12) 0.0191(14) C9 0.0690(18) 0.087(2) 0.0381(13) 0.0095(13) 0.0034(12) 0.0562(17) C11 0.0356(12) 0.0424(13) 0.0331(11) 0.0026(10) 0.0044(9) 0.0178(10) C17 0.089(2) 0.095(2) 0.0368(15) 0.0009(15) -0.0058(15) 0.050(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 Cd N1 2.2419(18) . ? Cd N1 2.2419(18) 2_666 ? Cd O1 2.3528(16) 2_666 ? Cd O1 2.3528(16) . ? Cd O4 2.3559(19) . ? Cd O4 2.3559(19) 2_666 ? S O3 1.4433(18) . ? S O2 1.4497(18) . ? S O1 1.4565(17) . ? S C11 1.763(2) . ? N1 C1 1.307(3) . ? N1 C2 1.372(3) . ? N2 C1 1.332(3) . ? N2 C3 1.361(3) . ? N2 C4 1.464(3) . ? C10 C8 1.381(3) . ? C10 C9 1.390(3) . ? C10 C10 1.487(4) 2_575 ? O4 H4S 0.79(4) . ? O4 H5S 0.90(4) . ? C1 H1 0.9300 . ? C5 C7 1.370(3) . ? C5 C6 1.377(3) . ? C5 C4 1.511(3) . ? C8 C7 1.383(3) . ? C8 H8 0.9300 . ? C2 C3 1.349(3) . ? C2 H2 0.9300 . ? C6 C9 1.377(3) . ? C6 H6 0.9300 . ? C16 C14 1.367(4) . ? C16 C15 1.377(4) . ? C16 C17 1.503(4) . ? C3 H3 0.9300 . ? C7 H7 0.9300 . ? C12 C11 1.363(3) . ? C12 C14 1.384(4) . ? C12 H12 0.9300 . ? C13 C15 1.372(4) . ? C13 C11 1.375(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C15 H15 0.9300 . ? C9 H9 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd N1 180.0 . 2_666 ? N1 Cd O1 92.97(6) . 2_666 ? N1 Cd O1 87.03(6) 2_666 2_666 ? N1 Cd O1 87.03(6) . . ? N1 Cd O1 92.97(6) 2_666 . ? O1 Cd O1 180.0 2_666 . ? N1 Cd O4 93.87(7) . . ? N1 Cd O4 86.13(7) 2_666 . ? O1 Cd O4 93.85(7) 2_666 . ? O1 Cd O4 86.15(7) . . ? N1 Cd O4 86.13(7) . 2_666 ? N1 Cd O4 93.87(7) 2_666 2_666 ? O1 Cd O4 86.15(7) 2_666 2_666 ? O1 Cd O4 93.85(7) . 2_666 ? O4 Cd O4 180.0 . 2_666 ? O3 S O2 112.94(12) . . ? O3 S O1 111.81(11) . . ? O2 S O1 112.09(11) . . ? O3 S C11 106.32(11) . . ? O2 S C11 107.35(11) . . ? O1 S C11 105.79(10) . . ? S O1 Cd 133.85(10) . . ? C1 N1 C2 105.46(19) . . ? C1 N1 Cd 125.61(15) . . ? C2 N1 Cd 127.97(15) . . ? C1 N2 C3 106.8(2) . . ? C1 N2 C4 126.6(2) . . ? C3 N2 C4 126.5(2) . . ? C8 C10 C9 116.2(2) . . ? C8 C10 C10 121.8(3) . 2_575 ? C9 C10 C10 122.0(3) . 2_575 ? Cd O4 H4S 131(3) . . ? Cd O4 H5S 101(2) . . ? H4S O4 H5S 106(3) . . ? N1 C1 N2 112.0(2) . . ? N1 C1 H1 124.0 . . ? N2 C1 H1 124.0 . . ? C7 C5 C6 117.7(2) . . ? C7 C5 C4 124.1(2) . . ? C6 C5 C4 118.1(2) . . ? C10 C8 C7 122.2(2) . . ? C10 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C3 C2 N1 109.1(2) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C5 C6 C9 121.3(2) . . ? C5 C6 H6 119.3 . . ? C9 C6 H6 119.3 . . ? C14 C16 C15 117.3(2) . . ? C14 C16 C17 121.3(3) . . ? C15 C16 C17 121.4(3) . . ? C2 C3 N2 106.6(2) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C5 C7 C8 121.0(2) . . ? C5 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C11 C12 C14 119.2(3) . . ? C11 C12 H12 120.4 . . ? C14 C12 H12 120.4 . . ? C15 C13 C11 120.1(2) . . ? C15 C13 H13 120.0 . . ? C11 C13 H13 120.0 . . ? C16 C14 C12 122.3(3) . . ? C16 C14 H14 118.9 . . ? C12 C14 H14 118.9 . . ? N2 C4 C5 114.7(2) . . ? N2 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N2 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C13 C15 C16 121.4(2) . . ? C13 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C6 C9 C10 121.7(2) . . ? C6 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C12 C11 C13 119.7(2) . . ? C12 C11 S 120.80(19) . . ? C13 C11 S 119.48(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.331 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.066 data_4_Lu731_[Cd(bimb)2(H2O)2](OTs)2(MeOH)4 _database_code_depnum_ccdc_archive 'CCDC 680071' _chemical_formula_sum 'C58 H70 Cd N8 O12 S2' _chemical_formula_weight 1247.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 9.0753(19) _cell_length_b 9.997(2) _cell_length_c 17.486(4) _cell_angle_alpha 91.871(3) _cell_angle_beta 93.356(3) _cell_angle_gamma 108.918(2) _cell_volume 1495.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4837 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 21364 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.53 _reflns_number_total 6960 _reflns_number_observed 5461 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. ; _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^)+(0.0476P)^2^+0.4219P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6960 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_obs 0.0431 _refine_ls_wR_factor_all 0.1044 _refine_ls_wR_factor_obs 0.0961 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C -0.0338(3) 0.2157(3) -0.13752(15) 0.0294(6) Uani 1 1 d . . . H1 H 0.0704 0.2393 -0.1483 0.035 Uiso 1 1 calc R . . C1S C 0.6781(7) 0.4478(5) -0.0071(3) 0.0949(17) Uani 1 1 d . . . H1S1 H 0.7521 0.3977 -0.0068 0.142 Uiso 1 1 calc R . . H1S2 H 0.6610 0.4747 -0.0582 0.142 Uiso 1 1 calc R . . H1S3 H 0.5812 0.3878 0.0099 0.142 Uiso 1 1 calc R . . C2 C -0.2524(3) 0.1173(3) -0.09150(16) 0.0316(6) Uani 1 1 d . . . H2 H -0.3293 0.0581 -0.0636 0.038 Uiso 1 1 calc R . . C2S C 0.2201(4) 0.1853(4) 0.22933(19) 0.0528(9) Uani 1 1 d . . . H2S1 H 0.2845 0.1844 0.2747 0.079 Uiso 1 1 calc R . . H2S2 H 0.1615 0.0897 0.2118 0.079 Uiso 1 1 calc R . . H2S3 H 0.1496 0.2357 0.2408 0.079 Uiso 1 1 calc R . . C3 C -0.2737(3) 0.2143(3) -0.13878(16) 0.0323(6) Uani 1 1 d . . . H3 H -0.3657 0.2344 -0.1492 0.039 Uiso 1 1 calc R . . C4 C -0.0982(4) 0.3898(3) -0.22135(16) 0.0330(7) Uani 1 1 d . . . H4A H 0.0139 0.4366 -0.2181 0.040 Uiso 1 1 calc R . . H4B H -0.1457 0.4591 -0.2051 0.040 Uiso 1 1 calc R . . C5 C -0.1530(3) 0.3433(3) -0.30422(15) 0.0270(6) Uani 1 1 d . . . C6 C -0.2403(3) 0.2057(3) 0.67187(16) 0.0299(6) Uani 1 1 d . . . H6 H -0.2708 0.1374 0.7079 0.036 Uiso 1 1 calc R . . C7 C -0.1118(3) 0.4427(3) 0.64116(16) 0.0290(6) Uani 1 1 d . . . H7 H -0.0544 0.5359 0.6565 0.035 Uiso 1 1 calc R . . C8 C -0.2827(3) 0.1687(3) 0.59490(16) 0.0290(6) Uani 1 1 d . . . H8 H -0.3419 0.0757 0.5800 0.035 Uiso 1 1 calc R . . C9 C -0.1536(3) 0.4069(3) 0.56472(16) 0.0282(6) Uani 1 1 d . . . H9 H -0.1250 0.4764 0.5292 0.034 Uiso 1 1 calc R . . C10 C -0.2387(3) 0.2676(3) 0.53937(15) 0.0250(6) Uani 1 1 d . . . C11 C -0.2196(3) 0.0443(3) 0.13091(15) 0.0282(6) Uani 1 1 d . . . H11 H -0.2587 -0.0534 0.1342 0.034 Uiso 1 1 calc R . . C12 C -0.0856(4) 0.2499(3) 0.09987(18) 0.0371(7) Uani 1 1 d . . . H12 H -0.0124 0.3229 0.0773 0.045 Uiso 1 1 calc R . . C13 C -0.1891(4) 0.2668(3) 0.14792(18) 0.0380(7) Uani 1 1 d . . . H13 H -0.2006 0.3521 0.1643 0.046 Uiso 1 1 calc R . . C14 C -0.4051(3) 0.0984(3) 0.21699(15) 0.0316(6) Uani 1 1 d . . . H14A H -0.4559 -0.0034 0.2126 0.038 Uiso 1 1 calc R . . H14B H -0.4805 0.1421 0.1986 0.038 Uiso 1 1 calc R . . C15 C -0.3579(3) 0.1439(3) 0.30012(15) 0.0262(6) Uani 1 1 d . . . C16 C -0.3309(3) 0.0509(3) 0.35121(16) 0.0328(7) Uani 1 1 d . . . H16 H -0.3389 -0.0402 0.3337 0.039 Uiso 1 1 calc R . . C17 C -0.3429(3) 0.2802(3) 0.32783(16) 0.0322(7) Uani 1 1 d . . . H17 H -0.3597 0.3448 0.2942 0.039 Uiso 1 1 calc R . . C18 C -0.2925(4) 0.0905(3) 0.42751(17) 0.0329(7) Uani 1 1 d . . . H18 H -0.2757 0.0254 0.4608 0.040 Uiso 1 1 calc R . . C19 C -0.3033(3) 0.3206(3) 0.40465(15) 0.0293(6) Uani 1 1 d . . . H19 H -0.2934 0.4123 0.4219 0.035 Uiso 1 1 calc R . . C20 C -0.2780(3) 0.2269(3) 0.45644(15) 0.0247(6) Uani 1 1 d . . . C21 C 0.6555(3) 0.6602(3) 0.32356(15) 0.0261(6) Uani 1 1 d . . . C22 C 0.5516(4) 0.6272(3) 0.37971(17) 0.0332(7) Uani 1 1 d . . . H22 H 0.4465 0.5779 0.3668 0.040 Uiso 1 1 calc R . . C23 C 0.8109(3) 0.7341(3) 0.34368(17) 0.0337(7) Uani 1 1 d . . . H23 H 0.8817 0.7571 0.3060 0.040 Uiso 1 1 calc R . . C24 C 0.6040(4) 0.6676(3) 0.45513(17) 0.0405(8) Uani 1 1 d . . . H24 H 0.5330 0.6454 0.4928 0.049 Uiso 1 1 calc R . . C25 C 0.8612(4) 0.7735(3) 0.41919(18) 0.0402(8) Uani 1 1 d . . . H25 H 0.9661 0.8236 0.4320 0.048 Uiso 1 1 calc R . . C26 C 0.7591(4) 0.7403(3) 0.47631(18) 0.0402(8) Uani 1 1 d . . . C27 C 0.8147(5) 0.7839(4) 0.55925(19) 0.0588(10) Uani 1 1 d . . . H27A H 0.9248 0.8347 0.5629 0.088 Uiso 1 1 calc R . . H27B H 0.7946 0.7011 0.5885 0.088 Uiso 1 1 calc R . . H27C H 0.7601 0.8437 0.5790 0.088 Uiso 1 1 calc R . . N1 N -0.1011(3) 0.1190(2) -0.09061(12) 0.0288(5) Uani 1 1 d . . . N2 N -0.1335(3) 0.2770(2) -0.16827(12) 0.0277(5) Uani 1 1 d . . . N3 N -0.1040(3) 0.1093(2) 0.08917(12) 0.0279(5) Uani 1 1 d . . . N4 N -0.2740(3) 0.1356(2) 0.16795(12) 0.0264(5) Uani 1 1 d . . . O1 O 0.6914(2) 0.5420(2) 0.19551(11) 0.0344(5) Uani 1 1 d . . . O1S O 0.7334(5) 0.5632(3) 0.03979(16) 0.0924(12) Uani 1 1 d . . . H7S H 0.700(6) 0.548(5) 0.094(3) 0.111 Uiso 1 1 d . . . O2 O 0.6131(3) 0.7498(2) 0.19071(12) 0.0410(5) Uani 1 1 d . . . O2S O 0.3147(3) 0.2523(3) 0.17198(12) 0.0464(6) Uani 1 1 d . . . H6S H 0.364(4) 0.350(4) 0.186(2) 0.056 Uiso 1 1 d . . . O3 O 0.4291(2) 0.5280(2) 0.22334(12) 0.0400(5) Uani 1 1 d . . . O4 O -0.2405(2) -0.1829(2) -0.01887(13) 0.0367(5) Uani 1 1 d . . . H4S H -0.264(4) -0.273(3) -0.0001(16) 0.044 Uiso 1 1 d D . . H5S H -0.260(4) -0.202(3) -0.0677(17) 0.044 Uiso 1 1 d D . . S1 S 0.59163(8) 0.61659(7) 0.22550(4) 0.02822(16) Uani 1 1 d . . . Cd Cd 0.0000 0.0000 0.0000 0.02436(10) Uani 1 2 d S . . 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 C1 0.0292(15) 0.0376(16) 0.0231(14) 0.0013(12) -0.0008(11) 0.0139(13) C1S 0.151(5) 0.070(3) 0.064(3) -0.008(2) -0.020(3) 0.044(3) C2 0.0327(16) 0.0373(16) 0.0264(15) 0.0031(12) 0.0008(12) 0.0138(13) C2S 0.060(2) 0.055(2) 0.038(2) 0.0000(17) 0.0004(17) 0.0132(19) C3 0.0308(16) 0.0381(16) 0.0307(15) 0.0006(13) -0.0035(12) 0.0158(13) C4 0.0386(17) 0.0294(15) 0.0294(16) 0.0027(12) -0.0064(13) 0.0103(13) C5 0.0249(14) 0.0308(15) 0.0275(15) 0.0054(12) -0.0002(11) 0.0121(12) C6 0.0332(16) 0.0289(15) 0.0283(15) 0.0095(12) 0.0018(12) 0.0105(13) C7 0.0314(16) 0.0233(14) 0.0316(15) 0.0022(12) 0.0009(12) 0.0082(12) C8 0.0322(16) 0.0240(14) 0.0305(15) 0.0039(12) 0.0016(12) 0.0085(12) C9 0.0308(15) 0.0265(14) 0.0294(15) 0.0081(12) 0.0061(12) 0.0110(12) C10 0.0262(14) 0.0275(14) 0.0250(14) 0.0049(11) 0.0035(11) 0.0134(12) C11 0.0370(16) 0.0253(14) 0.0245(14) 0.0009(11) 0.0057(12) 0.0128(12) C12 0.0445(19) 0.0242(15) 0.0415(18) 0.0017(13) 0.0109(14) 0.0083(14) C13 0.0452(19) 0.0265(15) 0.0446(18) -0.0038(13) 0.0111(15) 0.0142(14) C14 0.0281(15) 0.0373(16) 0.0299(15) -0.0031(13) 0.0057(12) 0.0110(13) C15 0.0255(14) 0.0308(15) 0.0254(14) -0.0010(11) 0.0046(11) 0.0133(12) C16 0.0432(18) 0.0237(14) 0.0335(16) -0.0038(12) 0.0041(13) 0.0142(13) C17 0.0457(18) 0.0319(15) 0.0256(15) 0.0070(12) 0.0074(13) 0.0205(14) C18 0.0445(18) 0.0262(15) 0.0330(16) 0.0065(12) 0.0037(13) 0.0176(13) C19 0.0407(17) 0.0267(14) 0.0257(14) 0.0010(11) 0.0069(12) 0.0173(13) C20 0.0245(14) 0.0268(14) 0.0254(14) 0.0036(11) 0.0053(11) 0.0111(12) C21 0.0311(15) 0.0231(13) 0.0305(15) 0.0062(11) 0.0057(12) 0.0166(12) C22 0.0345(17) 0.0329(16) 0.0372(17) 0.0080(13) 0.0098(13) 0.0160(13) C23 0.0288(16) 0.0392(17) 0.0368(17) 0.0037(13) 0.0065(13) 0.0155(13) C24 0.054(2) 0.0484(19) 0.0320(17) 0.0116(14) 0.0181(15) 0.0303(17) C25 0.0351(18) 0.0430(18) 0.0452(19) -0.0059(15) -0.0055(14) 0.0187(15) C26 0.059(2) 0.0402(18) 0.0332(17) -0.0015(14) -0.0010(15) 0.0338(17) C27 0.087(3) 0.063(2) 0.039(2) -0.0059(17) -0.0074(19) 0.043(2) N1 0.0324(13) 0.0365(13) 0.0215(12) 0.0035(10) 0.0020(10) 0.0165(11) N2 0.0329(13) 0.0293(12) 0.0218(12) 0.0025(10) -0.0044(10) 0.0124(11) N3 0.0349(13) 0.0262(12) 0.0246(12) 0.0010(10) 0.0041(10) 0.0125(10) N4 0.0285(13) 0.0271(12) 0.0242(12) -0.0029(9) 0.0035(10) 0.0100(10) O1 0.0453(13) 0.0413(12) 0.0256(10) 0.0052(9) 0.0077(9) 0.0251(10) O1S 0.185(4) 0.0459(16) 0.0406(16) 0.0049(13) 0.024(2) 0.027(2) O2 0.0526(14) 0.0327(11) 0.0414(13) 0.0129(9) -0.0028(10) 0.0189(10) O2S 0.0576(15) 0.0417(13) 0.0333(12) -0.0033(10) -0.0018(11) 0.0086(12) O3 0.0330(12) 0.0381(12) 0.0446(13) -0.0017(10) 0.0027(10) 0.0064(10) O4 0.0413(13) 0.0342(12) 0.0301(11) 0.0004(9) 0.0015(10) 0.0064(10) S1 0.0318(4) 0.0270(4) 0.0293(4) 0.0060(3) 0.0033(3) 0.0137(3) Cd 0.03006(17) 0.02833(17) 0.01835(15) 0.00174(11) 0.00170(11) 0.01454(13) _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 C1 N1 1.307(4) . ? C1 N2 1.345(3) . ? C1 H1 0.9300 . ? C1S O1S 1.330(5) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2 C3 1.347(4) . ? C2 N1 1.368(4) . ? C2 H2 0.9300 . ? C2S O2S 1.401(4) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3 N2 1.363(4) . ? C3 H3 0.9300 . ? C4 N2 1.451(3) . ? C4 C5 1.512(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C7 1.379(4) 1_554 ? C5 C6 1.383(4) 1_554 ? C6 C8 1.382(4) . ? C6 C5 1.383(4) 1_556 ? C6 H6 0.9300 . ? C7 C9 1.371(4) . ? C7 C5 1.379(4) 1_556 ? C7 H7 0.9300 . ? C8 C10 1.390(4) . ? C8 H8 0.9300 . ? C9 C10 1.399(4) . ? C9 H9 0.9300 . ? C10 C20 1.484(4) . ? C11 N3 1.317(3) . ? C11 N4 1.337(3) . ? C11 H11 0.9300 . ? C12 C13 1.343(4) . ? C12 N3 1.366(3) . ? C12 H12 0.9300 . ? C13 N4 1.358(4) . ? C13 H13 0.9300 . ? C14 N4 1.464(3) . ? C14 C15 1.504(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.378(4) . ? C15 C17 1.392(4) . ? C16 C18 1.371(4) . ? C16 H16 0.9300 . ? C17 C19 1.382(4) . ? C17 H17 0.9300 . ? C18 C20 1.401(4) . ? C18 H18 0.9300 . ? C19 C20 1.386(4) . ? C19 H19 0.9300 . ? C21 C22 1.375(4) . ? C21 C23 1.381(4) . ? C21 S1 1.771(3) . ? C22 C24 1.377(4) . ? C22 H22 0.9300 . ? C23 C25 1.374(4) . ? C23 H23 0.9300 . ? C24 C26 1.380(5) . ? C24 H24 0.9300 . ? C25 C26 1.378(4) . ? C25 H25 0.9300 . ? C26 C27 1.509(4) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N1 Cd 2.330(2) . ? N3 Cd 2.290(2) . ? O1 S1 1.4556(19) . ? O1S H7S 1.02(5) . ? O2 S1 1.442(2) . ? O2S H6S 0.95(4) . ? O3 S1 1.451(2) . ? O4 Cd 2.346(2) . ? O4 H4S 0.94(3) . ? O4 H5S 0.86(3) . ? Cd N3 2.290(2) 2 ? Cd N1 2.330(2) 2 ? Cd O4 2.346(2) 2 ? 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 N1 C1 N2 111.8(3) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3 C2 N1 109.8(3) . . ? C3 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C2 C3 N2 106.4(2) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 115.1(2) . . ? N2 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C7 C5 C6 118.4(3) 1_554 1_554 ? C7 C5 C4 118.3(2) 1_554 . ? C6 C5 C4 123.3(2) 1_554 . ? C8 C6 C5 120.6(3) . 1_556 ? C8 C6 H6 119.7 . . ? C5 C6 H6 119.7 1_556 . ? C9 C7 C5 121.4(3) . 1_556 ? C9 C7 H7 119.3 . . ? C5 C7 H7 119.3 1_556 . ? C6 C8 C10 121.4(3) . . ? C6 C8 H8 119.3 . . ? C10 C8 H8 119.3 . . ? C7 C9 C10 121.0(3) . . ? C7 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C8 C10 C9 117.3(2) . . ? C8 C10 C20 121.5(2) . . ? C9 C10 C20 121.2(2) . . ? N3 C11 N4 111.9(2) . . ? N3 C11 H11 124.0 . . ? N4 C11 H11 124.0 . . ? C13 C12 N3 109.8(3) . . ? C13 C12 H12 125.1 . . ? N3 C12 H12 125.1 . . ? C12 C13 N4 106.9(3) . . ? C12 C13 H13 126.6 . . ? N4 C13 H13 126.6 . . ? N4 C14 C15 113.6(2) . . ? N4 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? N4 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C17 118.2(2) . . ? C16 C15 C14 120.8(2) . . ? C17 C15 C14 121.0(3) . . ? C18 C16 C15 121.0(2) . . ? C18 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C19 C17 C15 120.9(3) . . ? C19 C17 H17 119.6 . . ? C15 C17 H17 119.6 . . ? C16 C18 C20 121.5(3) . . ? C16 C18 H18 119.3 . . ? C20 C18 H18 119.3 . . ? C17 C19 C20 121.1(2) . . ? C17 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C18 117.3(2) . . ? C19 C20 C10 121.9(2) . . ? C18 C20 C10 120.9(2) . . ? C22 C21 C23 119.4(3) . . ? C22 C21 S1 121.0(2) . . ? C23 C21 S1 119.5(2) . . ? C21 C22 C24 119.6(3) . . ? C21 C22 H22 120.2 . . ? C24 C22 H22 120.2 . . ? C25 C23 C21 120.3(3) . . ? C25 C23 H23 119.9 . . ? C21 C23 H23 119.9 . . ? C22 C24 C26 121.8(3) . . ? C22 C24 H24 119.1 . . ? C26 C24 H24 119.1 . . ? C23 C25 C26 121.1(3) . . ? C23 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C24 117.9(3) . . ? C25 C26 C27 121.0(3) . . ? C24 C26 C27 121.1(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 N1 C2 105.4(2) . . ? C1 N1 Cd 131.96(19) . . ? C2 N1 Cd 121.42(18) . . ? C1 N2 C3 106.6(2) . . ? C1 N2 C4 126.7(2) . . ? C3 N2 C4 126.6(2) . . ? C11 N3 C12 104.9(2) . . ? C11 N3 Cd 125.09(18) . . ? C12 N3 Cd 128.76(19) . . ? C11 N4 C13 106.5(2) . . ? C11 N4 C14 125.9(2) . . ? C13 N4 C14 127.5(2) . . ? C1S O1S H7S 114(3) . . ? C2S O2S H6S 111(2) . . ? Cd O4 H4S 126.2(19) . . ? Cd O4 H5S 108(2) . . ? H4S O4 H5S 101(2) . . ? O2 S1 O3 113.02(13) . . ? O2 S1 O1 112.27(13) . . ? O3 S1 O1 112.59(13) . . ? O2 S1 C21 105.72(12) . . ? O3 S1 C21 106.54(13) . . ? O1 S1 C21 106.01(12) . . ? N3 Cd N3 180.00(12) . 2 ? N3 Cd N1 94.04(8) . 2 ? N3 Cd N1 85.96(8) 2 2 ? N3 Cd N1 85.96(8) . . ? N3 Cd N1 94.04(8) 2 . ? N1 Cd N1 180.00(13) 2 . ? N3 Cd O4 90.51(8) . 2 ? N3 Cd O4 89.49(8) 2 2 ? N1 Cd O4 86.36(8) 2 2 ? N1 Cd O4 93.64(8) . 2 ? N3 Cd O4 89.49(8) . . ? N3 Cd O4 90.51(8) 2 . ? N1 Cd O4 93.64(8) 2 . ? N1 Cd O4 86.36(8) . . ? O4 Cd O4 180.00(9) 2 . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.840 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.076 data_5_lu682_Co(bimb)2(SO4) _database_code_depnum_ccdc_archive 'CCDC 680072' _chemical_formula_sum 'C40 H36 Co N8 O4 S' _chemical_formula_weight 783.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 34.742(11) _cell_length_b 9.127(3) _cell_length_c 12.180(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.640(5) _cell_angle_gamma 90.00 _cell_volume 3700(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 275 _cell_measurement_theta_min 3 _cell_measurement_theta_max 14 _exptl_crystal_description column _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 18600 _diffrn_reflns_av_R_equivalents 0.2890 _diffrn_reflns_av_sigmaI/netI 0.2946 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.19 _reflns_number_total 3856 _reflns_number_observed 1479 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The poor diffraction of the crystal produce high value of Rint. One of the benzene ring of the ligand is modelled as disordered on two position with occupation 75%:25%. The lowest occupied model is also refined isotropically. ; _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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3856 _refine_ls_number_parameters 263 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2461 _refine_ls_R_factor_obs 0.0786 _refine_ls_wR_factor_all 0.1589 _refine_ls_wR_factor_obs 0.1115 _refine_ls_goodness_of_fit_all 0.946 _refine_ls_restrained_S_all 0.946 _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 0.7381(3) 0.0144(13) 0.5864(9) 0.036(3) Uani 0.751(13) 1 d P A 1 H1A H 0.7426 -0.0816 0.5675 0.043 Uiso 0.751(13) 1 calc PR A 1 C2A C 0.6990(3) 0.0627(11) 0.5654(9) 0.035(3) Uani 0.751(13) 1 d P A 1 H2A H 0.6778 -0.0012 0.5345 0.042 Uiso 0.751(13) 1 calc PR A 1 C3A C 0.7622(3) 0.2477(11) 0.6583(9) 0.035(3) Uani 0.751(13) 1 d P A 1 H3A H 0.7835 0.3112 0.6899 0.041 Uiso 0.751(13) 1 calc PR A 1 C4A C 0.7238(3) 0.2982(11) 0.6369(9) 0.033(3) Uani 0.751(13) 1 d P A 1 H4A H 0.7192 0.3950 0.6534 0.039 Uiso 0.751(13) 1 calc PR A 1 C1B C 0.7602(10) 0.181(4) 0.718(3) 0.048(10) Uiso 0.249(13) 1 d P A 2 H1B H 0.7780 0.1971 0.7897 0.058 Uiso 0.249(13) 1 calc PR A 2 C2B C 0.7209(11) 0.236(4) 0.687(3) 0.053(12) Uiso 0.249(13) 1 d P A 2 H2B H 0.7144 0.2997 0.7382 0.064 Uiso 0.249(13) 1 calc PR A 2 C3B C 0.7014(9) 0.116(3) 0.511(3) 0.033(9) Uiso 0.249(13) 1 d P A 2 H3B H 0.6816 0.0897 0.4447 0.040 Uiso 0.249(13) 1 calc PR A 2 C4B C 0.7404(9) 0.064(3) 0.527(3) 0.043(10) Uiso 0.249(13) 1 d P A 2 H4B H 0.7470 0.0077 0.4711 0.052 Uiso 0.249(13) 1 calc PR A 2 C16 C 0.46183(17) 0.2044(6) 0.6425(5) 0.0251(16) Uani 1 1 d . . . H16 H 0.4593 0.1266 0.6893 0.030 Uiso 1 1 calc R . . C3 C 0.58884(18) 0.0119(8) 0.6712(5) 0.0322(16) Uani 1 1 d . . . H3 H 0.5832 -0.0549 0.7221 0.039 Uiso 1 1 calc R . . C11 C 0.38262(19) 0.5727(7) 0.7657(5) 0.0332(17) Uani 1 1 d . . . H11 H 0.4023 0.6228 0.8208 0.040 Uiso 1 1 calc R . . C14 C 0.45794(19) 0.4245(7) 0.5701(5) 0.0361(18) Uani 1 1 d . . . H14 H 0.4533 0.5243 0.5575 0.043 Uiso 1 1 calc R . . C2 C 0.6248(2) 0.0754(7) 0.6825(6) 0.0369(18) Uani 1 1 d . A . H2 H 0.6481 0.0614 0.7421 0.044 Uiso 1 1 calc R . . C15 C 0.47377(18) 0.3317(7) 0.5084(5) 0.0319(17) Uani 1 1 d . . . H15 H 0.4812 0.3574 0.4434 0.038 Uiso 1 1 calc R . . C10 C 0.39303(19) 0.4520(7) 0.7101(5) 0.0280(17) Uani 1 1 d . . . C13 C 0.43574(17) 0.3988(7) 0.7474(5) 0.0262(16) Uani 1 1 d . . . H13A H 0.4530 0.4789 0.7843 0.031 Uiso 1 1 calc R . . H13B H 0.4380 0.3218 0.8038 0.031 Uiso 1 1 calc R . . C8 C 0.3239(2) 0.4325(7) 0.6025(6) 0.0392(19) Uani 1 1 d . . . H8 H 0.3043 0.3839 0.5461 0.047 Uiso 1 1 calc R . . C12 C 0.3429(2) 0.6183(7) 0.7392(6) 0.0393(19) Uani 1 1 d . . . H12 H 0.3367 0.6986 0.7780 0.047 Uiso 1 1 calc R . . C1 C 0.5815(2) 0.1525(7) 0.5237(6) 0.0306(17) Uani 1 1 d . A . H1 H 0.5704 0.2010 0.4548 0.037 Uiso 1 1 calc R . . C5 C 0.6913(2) 0.2047(8) 0.5900(6) 0.0359(18) Uani 1 1 d . . . C9 C 0.3627(2) 0.3855(7) 0.6272(6) 0.0363(18) Uani 1 1 d . . . H9 H 0.3688 0.3065 0.5870 0.044 Uiso 1 1 calc R . . C6 C 0.7707(2) 0.1028(7) 0.6342(6) 0.0337(17) Uani 1 1 d . . . C7 C 0.31263(19) 0.5506(7) 0.6587(6) 0.0316(18) Uani 1 1 d . . . C4 C 0.64947(19) 0.2685(7) 0.5656(6) 0.042(2) Uani 1 1 d . A . H4C H 0.6506 0.3551 0.6125 0.051 Uiso 1 1 calc R . . H4D H 0.6404 0.2987 0.4859 0.051 Uiso 1 1 calc R . . N4 N 0.47734(14) 0.1942(5) 0.5554(4) 0.0238(13) Uani 1 1 d . . . N1 N 0.56161(15) 0.0625(5) 0.5713(4) 0.0256(13) Uani 1 1 d . . . N3 N 0.45013(14) 0.3428(5) 0.6541(4) 0.0244(13) Uani 1 1 d . . . N2 N 0.62019(15) 0.1656(5) 0.5879(5) 0.0297(14) Uani 1 1 d . . . O1 O 0.53660(16) 0.2777(5) 0.2821(4) 0.0724(19) Uani 1 1 d D . . O2 O 0.49939(12) 0.0944(5) 0.3461(3) 0.0400(13) Uani 1 1 d D . . S S 0.5000 0.1896(3) 0.2500 0.0270(6) Uani 1 2 d SD . . Co Co 0.5000 0.0000 0.5000 0.0220(3) Uani 1 2 d S . . 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 0.023(6) 0.039(6) 0.045(7) -0.007(7) 0.009(5) 0.004(6) C2A 0.023(6) 0.030(6) 0.051(8) -0.001(5) 0.009(5) -0.014(5) C3A 0.022(6) 0.034(6) 0.043(7) 0.000(5) 0.002(5) 0.001(5) C4A 0.030(6) 0.019(5) 0.043(7) 0.002(5) 0.002(5) 0.007(5) C16 0.029(4) 0.016(4) 0.036(4) -0.005(3) 0.017(3) -0.003(3) C3 0.022(4) 0.036(4) 0.038(4) 0.001(4) 0.009(3) 0.000(4) C11 0.026(4) 0.035(4) 0.038(4) -0.002(4) 0.009(3) -0.003(3) C14 0.058(5) 0.022(4) 0.031(4) 0.003(3) 0.017(4) 0.009(4) C2 0.031(5) 0.034(4) 0.044(5) 0.008(4) 0.008(4) 0.003(4) C15 0.038(4) 0.031(4) 0.030(4) 0.006(3) 0.014(3) 0.002(3) C10 0.026(4) 0.031(4) 0.027(4) 0.002(3) 0.007(3) 0.005(3) C13 0.021(4) 0.031(4) 0.026(4) 0.000(3) 0.007(3) 0.004(3) C8 0.031(5) 0.036(4) 0.043(5) -0.013(4) -0.002(4) -0.003(4) C12 0.031(5) 0.046(5) 0.045(5) -0.008(4) 0.017(4) 0.015(4) C1 0.030(4) 0.032(4) 0.030(4) -0.003(3) 0.010(4) 0.002(4) C5 0.026(5) 0.040(5) 0.042(5) 0.000(4) 0.012(4) -0.002(4) C9 0.031(5) 0.032(4) 0.042(5) -0.010(4) 0.004(4) 0.008(4) C6 0.033(5) 0.031(4) 0.036(4) 0.000(3) 0.008(4) 0.002(4) C7 0.024(4) 0.031(4) 0.037(5) 0.004(3) 0.003(4) -0.002(3) C4 0.028(5) 0.042(5) 0.060(5) -0.003(4) 0.019(4) -0.005(4) N4 0.024(3) 0.021(3) 0.028(3) -0.001(3) 0.009(3) 0.001(3) N1 0.024(3) 0.026(3) 0.026(3) -0.004(3) 0.006(3) 0.003(3) N3 0.026(3) 0.025(3) 0.024(3) 0.000(3) 0.009(3) 0.001(3) N2 0.020(3) 0.026(3) 0.045(4) 0.002(3) 0.012(3) 0.002(3) O1 0.095(4) 0.061(4) 0.045(3) 0.006(3) -0.006(3) -0.060(3) O2 0.042(3) 0.053(3) 0.025(3) 0.018(2) 0.010(2) -0.007(2) S 0.0386(17) 0.0223(14) 0.0198(14) 0.000 0.0076(12) 0.000 Co 0.0256(7) 0.0191(7) 0.0215(7) 0.0002(7) 0.0072(5) -0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C6 1.376(10) . ? C1A C2A 1.383(11) . ? C1A H1A 0.9300 . ? C2A C5 1.374(11) . ? C2A H2A 0.9300 . ? C3A C4A 1.365(11) . ? C3A C6 1.405(11) . ? C3A H3A 0.9300 . ? C4A C5 1.401(11) . ? C4A H4A 0.9300 . ? C1B C6 1.37(3) . ? C1B C2B 1.40(4) . ? C1B H1B 0.9300 . ? C2B C5 1.35(4) . ? C2B H2B 0.9300 . ? C3B C5 1.38(3) . ? C3B C4B 1.40(4) . ? C3B H3B 0.9300 . ? C4B C6 1.47(3) . ? C4B H4B 0.9300 . ? C16 N4 1.323(7) . ? C16 N3 1.347(7) . ? C16 H16 0.9300 . ? C3 C2 1.347(8) . ? C3 N1 1.389(7) . ? C3 H3 0.9300 . ? C11 C12 1.387(8) . ? C11 C10 1.394(8) . ? C11 H11 0.9300 . ? C14 C15 1.350(8) . ? C14 N3 1.355(7) . ? C14 H14 0.9300 . ? C2 N2 1.388(7) . ? C2 H2 0.9300 . ? C15 N4 1.370(7) . ? C15 H15 0.9300 . ? C10 C9 1.374(8) . ? C10 C13 1.503(8) . ? C13 N3 1.458(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C8 C9 1.363(8) . ? C8 C7 1.391(8) . ? C8 H8 0.9300 . ? C12 C7 1.365(8) . ? C12 H12 0.9300 . ? C1 N1 1.310(7) . ? C1 N2 1.353(7) . ? C1 H1 0.9300 . ? C5 C4 1.512(8) . ? C9 H9 0.9300 . ? C6 C7 1.479(8) 3_545 ? C7 C6 1.479(8) 3_455 ? C4 N2 1.466(7) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? N4 Co 2.126(5) . ? N1 Co 2.144(5) . ? O1 S 1.460(4) . ? O2 S 1.462(4) . ? O2 Co 2.058(4) . ? S O1 1.460(4) 2_655 ? S O2 1.462(4) 2_655 ? Co O2 2.058(4) 5_656 ? Co N4 2.126(5) 5_656 ? Co N1 2.144(5) 5_656 ? 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 C6 C1A C2A 122.6(9) . . ? C6 C1A H1A 118.7 . . ? C2A C1A H1A 118.7 . . ? C5 C2A C1A 120.2(8) . . ? C5 C2A H2A 119.9 . . ? C1A C2A H2A 119.9 . . ? C4A C3A C6 122.0(9) . . ? C4A C3A H3A 119.0 . . ? C6 C3A H3A 119.0 . . ? C3A C4A C5 120.2(8) . . ? C3A C4A H4A 119.9 . . ? C5 C4A H4A 119.9 . . ? C6 C1B C2B 116(3) . . ? C6 C1B H1B 122.2 . . ? C2B C1B H1B 122.2 . . ? C5 C2B C1B 127(3) . . ? C5 C2B H2B 116.6 . . ? C1B C2B H2B 116.6 . . ? C5 C3B C4B 122(3) . . ? C5 C3B H3B 118.8 . . ? C4B C3B H3B 118.8 . . ? C3B C4B C6 117(3) . . ? C3B C4B H4B 121.3 . . ? C6 C4B H4B 121.3 . . ? N4 C16 N3 110.8(5) . . ? N4 C16 H16 124.6 . . ? N3 C16 H16 124.6 . . ? C2 C3 N1 109.0(6) . . ? C2 C3 H3 125.5 . . ? N1 C3 H3 125.5 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C15 C14 N3 106.0(6) . . ? C15 C14 H14 127.0 . . ? N3 C14 H14 127.0 . . ? C3 C2 N2 106.7(6) . . ? C3 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? C14 C15 N4 110.2(6) . . ? C14 C15 H15 124.9 . . ? N4 C15 H15 124.9 . . ? C9 C10 C11 117.1(6) . . ? C9 C10 C13 124.2(6) . . ? C11 C10 C13 118.7(6) . . ? N3 C13 C10 114.0(5) . . ? N3 C13 H13A 108.7 . . ? C10 C13 H13A 108.7 . . ? N3 C13 H13B 108.7 . . ? C10 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C9 C8 C7 122.3(6) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C7 C12 C11 122.8(6) . . ? C7 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? N1 C1 N2 111.3(6) . . ? N1 C1 H1 124.4 . . ? N2 C1 H1 124.4 . . ? C2B C5 C2A 103.8(17) . . ? C2B C5 C3B 117(2) . . ? C2A C5 C3B 35.8(12) . . ? C2B C5 C4A 36.4(15) . . ? C2A C5 C4A 118.6(7) . . ? C3B C5 C4A 107.7(14) . . ? C2B C5 C4 122.6(17) . . ? C2A C5 C4 123.8(7) . . ? C3B C5 C4 120.8(14) . . ? C4A C5 C4 117.6(7) . . ? C8 C9 C10 121.7(6) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C1B C6 C1A 104.9(15) . . ? C1B C6 C3A 40.4(14) . . ? C1A C6 C3A 116.4(8) . . ? C1B C6 C4B 121(2) . . ? C1A C6 C4B 35.9(12) . . ? C3A C6 C4B 105.8(14) . . ? C1B C6 C7 118.3(16) . 3_545 ? C1A C6 C7 122.6(7) . 3_545 ? C3A C6 C7 121.0(7) . 3_545 ? C4B C6 C7 121.0(14) . 3_545 ? C12 C7 C8 115.9(6) . . ? C12 C7 C6 120.7(6) . 3_455 ? C8 C7 C6 123.4(6) . 3_455 ? N2 C4 C5 113.3(5) . . ? N2 C4 H4C 108.9 . . ? C5 C4 H4C 108.9 . . ? N2 C4 H4D 108.9 . . ? C5 C4 H4D 108.9 . . ? H4C C4 H4D 107.7 . . ? C16 N4 C15 105.2(5) . . ? C16 N4 Co 125.8(4) . . ? C15 N4 Co 128.9(4) . . ? C1 N1 C3 106.4(6) . . ? C1 N1 Co 125.4(5) . . ? C3 N1 Co 128.1(4) . . ? C16 N3 C14 107.8(5) . . ? C16 N3 C13 126.3(5) . . ? C14 N3 C13 125.7(5) . . ? C1 N2 C2 106.6(5) . . ? C1 N2 C4 125.3(6) . . ? C2 N2 C4 127.9(6) . . ? S O2 Co 168.2(3) . . ? O1 S O1 113.2(5) . 2_655 ? O1 S O2 109.3(3) . 2_655 ? O1 S O2 108.9(2) 2_655 2_655 ? O1 S O2 108.9(2) . . ? O1 S O2 109.3(3) 2_655 . ? O2 S O2 107.1(4) 2_655 . ? O2 Co O2 180.0(2) . 5_656 ? O2 Co N4 91.83(18) . . ? O2 Co N4 88.17(18) 5_656 . ? O2 Co N4 88.17(18) . 5_656 ? O2 Co N4 91.83(18) 5_656 5_656 ? N4 Co N4 180.000(1) . 5_656 ? O2 Co N1 89.64(18) . 5_656 ? O2 Co N1 90.36(18) 5_656 5_656 ? N4 Co N1 86.15(17) . 5_656 ? N4 Co N1 93.85(17) 5_656 5_656 ? O2 Co N1 90.36(18) . . ? O2 Co N1 89.64(18) 5_656 . ? N4 Co N1 93.85(17) . . ? N4 Co N1 86.15(17) 5_656 . ? N1 Co N1 180.00(13) 5_656 . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.632 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.101 data_6_Lu622_[Co(bimb)2(H2O)2][Co(bimb)3](NO3)4(EtOH)4(H2O)2 _database_code_depnum_ccdc_archive 'CCDC 680073' _chemical_formula_sum 'C108 H122 Co2 N24 O20' _chemical_formula_weight 2194.16 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7796(19) _cell_length_b 14.857(3) _cell_length_c 21.621(5) _cell_angle_alpha 72.212(4) _cell_angle_beta 81.686(4) _cell_angle_gamma 83.572(4) _cell_volume 2650.3(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3825 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.395 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 25 _diffrn_reflns_number 21054 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.04 _reflns_number_total 9331 _reflns_number_observed 5947 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The crystal are unstable, high decay 25% The chlatrate water molecules were refined without hydrogen atoms. ; _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^)+(0.1784P)^2^+8.4022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9331 _refine_ls_number_parameters 673 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1551 _refine_ls_R_factor_obs 0.1080 _refine_ls_wR_factor_all 0.3327 _refine_ls_wR_factor_obs 0.2928 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.003 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 C1 C -0.0381(8) -0.1996(5) 0.6032(3) 0.0501(18) Uani 1 1 d D . . H1 H -0.0031 -0.1780 0.6344 0.060 Uiso 1 1 calc R . . C1S C -0.036(5) -0.355(3) -0.043(2) 0.36(2) Uiso 1 1 d . . . H1S1 H 0.0499 -0.3958 -0.0543 0.437 Uiso 1 1 calc R . . H1S2 H -0.0698 -0.3713 0.0036 0.437 Uiso 1 1 calc R . . C2 C -0.1156(9) -0.2043(6) 0.5152(3) 0.0556(19) Uani 1 1 d D . . H2 H -0.1451 -0.1864 0.4732 0.067 Uiso 1 1 calc R . . C2S C -0.184(4) -0.326(3) -0.0942(19) 0.333(19) Uiso 1 1 d . . . H2S1 H -0.2440 -0.3797 -0.0853 0.500 Uiso 1 1 calc R . . H2S2 H -0.1392 -0.3092 -0.1391 0.500 Uiso 1 1 calc R . . H2S3 H -0.2493 -0.2734 -0.0863 0.500 Uiso 1 1 calc R . . C3 C -0.1122(10) -0.2933(5) 0.5566(3) 0.058(2) Uani 1 1 d D . . H3 H -0.1385 -0.3471 0.5483 0.070 Uiso 1 1 calc R . . C3S C 0.6991(19) -0.0822(12) 0.7847(8) 0.137(5) Uiso 1 1 d . . . H35A H 0.7898 -0.0466 0.7674 0.164 Uiso 1 1 calc R . . H35B H 0.7300 -0.1418 0.8155 0.164 Uiso 1 1 calc R . . C4 C -0.0426(8) -0.3697(5) 0.6715(3) 0.0517(19) Uani 1 1 d . . . H4A H 0.0029 -0.3481 0.7023 0.062 Uiso 1 1 calc R . . H4B H 0.0283 -0.4184 0.6598 0.062 Uiso 1 1 calc R . . C4S C 0.635(2) -0.1002(13) 0.7317(9) 0.166(7) Uiso 1 1 d . . . H3S1 H 0.7116 -0.1345 0.7095 0.250 Uiso 1 1 calc R . . H3S2 H 0.6039 -0.0411 0.7014 0.250 Uiso 1 1 calc R . . H3S3 H 0.5470 -0.1370 0.7491 0.250 Uiso 1 1 calc R . . C5 C -0.1939(8) -0.4118(5) 0.7040(3) 0.0459(17) Uani 1 1 d . . . C6 C -0.2314(8) -0.4971(5) 0.6999(4) 0.0500(17) Uani 1 1 d . . . H6 H -0.1605 -0.5312 0.6778 0.060 Uiso 1 1 calc R . . C7 C -0.3015(9) -0.3628(6) 0.7372(4) 0.059(2) Uani 1 1 d . . . H7 H -0.2786 -0.3047 0.7400 0.071 Uiso 1 1 calc R . . C8 C -0.3729(8) -0.5336(5) 0.7281(3) 0.0443(16) Uani 1 1 d . . . H8 H -0.3950 -0.5918 0.7250 0.053 Uiso 1 1 calc R . . C9 C -0.4417(9) -0.3973(5) 0.7660(4) 0.0545(19) Uani 1 1 d . . . H9 H -0.5103 -0.3633 0.7890 0.065 Uiso 1 1 calc R . . C10 C -0.4821(8) -0.4830(5) 0.7612(3) 0.0421(16) Uani 1 1 d . . . C11 C -0.6367(7) -0.5192(4) 0.7898(3) 0.0363(14) Uani 1 1 d . . . C12 C -0.6621(8) -0.6148(5) 0.8085(3) 0.0418(15) Uani 1 1 d . . . H12 H -0.5795 -0.6582 0.8038 0.050 Uiso 1 1 calc R . . C13 C -0.7651(8) -0.4570(5) 0.7983(3) 0.0466(17) Uani 1 1 d . . . H13 H -0.7529 -0.3923 0.7865 0.056 Uiso 1 1 calc R . . C14 C -0.8066(8) -0.6480(5) 0.8338(3) 0.0446(16) Uani 1 1 d . . . H14 H -0.8192 -0.7126 0.8455 0.054 Uiso 1 1 calc R . . C15 C -0.9073(8) -0.4890(4) 0.8234(3) 0.0439(16) Uani 1 1 d . . . H15 H -0.9896 -0.4456 0.8284 0.053 Uiso 1 1 calc R . . C16 C -0.9325(7) -0.5854(5) 0.8419(3) 0.0390(14) Uani 1 1 d . . . C17 C -0.0935(9) 0.3851(5) -0.1310(4) 0.0523(18) Uani 1 1 d . . . H17A H -0.1240 0.4027 -0.0910 0.063 Uiso 1 1 calc R . . H17B H -0.1643 0.4195 -0.1621 0.063 Uiso 1 1 calc R . . C18 C -0.0619(8) 0.2146(5) -0.0652(3) 0.0456(16) Uani 1 1 d D . . H18 H -0.0236 0.2262 -0.0307 0.055 Uiso 1 1 calc R . . C19 C -0.1572(8) 0.2379(5) -0.1563(3) 0.0511(18) Uani 1 1 d D . . H19 H -0.1956 0.2669 -0.1961 0.061 Uiso 1 1 calc R . . C20 C -0.1398(10) 0.1441(5) -0.1262(3) 0.055(2) Uani 1 1 d D . . H20 H -0.1658 0.0966 -0.1418 0.066 Uiso 1 1 calc R . . C21 C -0.0353(8) 0.0603(6) 0.6281(3) 0.060(2) Uani 1 1 d D . . H21 H -0.1357 0.0858 0.6222 0.072 Uiso 1 1 calc R . . C22 C 0.1848(8) -0.0161(5) 0.6189(3) 0.0545(19) Uani 1 1 d D . . H22 H 0.2659 -0.0537 0.6048 0.065 Uiso 1 1 calc R . . C23 C 0.1847(9) 0.0226(7) 0.6665(3) 0.067(2) Uani 1 1 d D . . H23 H 0.2654 0.0170 0.6912 0.080 Uiso 1 1 calc R . . C24 C 0.0037(10) 0.1363(9) 0.7135(4) 0.085(3) Uani 1 1 d . . . H24A H 0.0448 0.1089 0.7551 0.102 Uiso 1 1 calc R . . H24B H -0.1078 0.1443 0.7222 0.102 Uiso 1 1 calc R . . C25 C 0.0670(10) 0.2309(8) 0.6796(4) 0.075(3) Uani 1 1 d . . . C26 C 0.0047(9) 0.2942(9) 0.6256(5) 0.077(3) Uani 1 1 d . . . H26 H -0.0826 0.2790 0.6122 0.092 Uiso 1 1 calc R . . C27 C 0.1977(9) 0.2566(8) 0.6980(4) 0.072(3) Uani 1 1 d . . . H27 H 0.2428 0.2154 0.7335 0.087 Uiso 1 1 calc R . . C28 C 0.0673(9) 0.3770(8) 0.5921(4) 0.068(3) Uani 1 1 d . . . H28 H 0.0222 0.4169 0.5562 0.082 Uiso 1 1 calc R . . C29 C 0.2614(9) 0.3403(8) 0.6656(4) 0.070(3) Uani 1 1 d . . . H29 H 0.3469 0.3552 0.6803 0.084 Uiso 1 1 calc R . . C30 C 0.2017(9) 0.4049(7) 0.6104(4) 0.063(2) Uani 1 1 d . . . C31 C 0.2738(9) 0.4929(7) 0.5738(4) 0.066(2) Uani 1 1 d . . . C32 C 0.2819(10) 0.5269(8) 0.5052(4) 0.070(3) Uani 1 1 d . . . H32 H 0.2381 0.4941 0.4827 0.084 Uiso 1 1 calc R . . C33 C 0.3422(10) 0.5443(7) 0.6060(4) 0.069(2) Uani 1 1 d . . . H33 H 0.3382 0.5235 0.6513 0.083 Uiso 1 1 calc R . . C34 C 0.3534(11) 0.6077(8) 0.4712(5) 0.079(3) Uani 1 1 d . . . H34 H 0.3563 0.6294 0.4259 0.095 Uiso 1 1 calc R . . C35 C 0.4144(10) 0.6241(8) 0.5716(4) 0.071(3) Uani 1 1 d . . . H35 H 0.4595 0.6568 0.5938 0.086 Uiso 1 1 calc R . . C36 C 0.4220(10) -0.3420(8) 0.5033(5) 0.075(3) Uani 1 1 d . . . C37 C 0.5052(11) -0.2542(8) 0.4651(5) 0.089(3) Uani 1 1 d . . . H37A H 0.6017 -0.2569 0.4828 0.107 Uiso 1 1 calc R . . H37B H 0.5300 -0.2544 0.4200 0.107 Uiso 1 1 calc R . . C38 C 0.2726(9) -0.1510(6) 0.4923(4) 0.067(2) Uani 1 1 d D . . H38 H 0.2094 -0.1996 0.5150 0.080 Uiso 1 1 calc R . . C39 C 0.4653(12) -0.0821(10) 0.4369(10) 0.168(8) Uani 1 1 d D . . H39 H 0.5616 -0.0697 0.4130 0.202 Uiso 1 1 calc R . . C40 C 0.3473(11) -0.0136(7) 0.4469(8) 0.134(6) Uani 1 1 d D . . H40 H 0.3516 0.0518 0.4317 0.161 Uiso 1 1 calc R . . C41 C -0.3004(9) -0.0786(4) -0.0223(3) 0.0488(18) Uani 1 1 d D . . H41 H -0.2686 -0.0671 -0.0668 0.059 Uiso 1 1 calc R . . C42 C -0.3056(9) -0.0899(4) 0.0786(3) 0.0461(17) Uani 1 1 d D . . H42 H -0.2765 -0.0871 0.1176 0.055 Uiso 1 1 calc R . . C43 C -0.4360(8) -0.1238(4) 0.0725(3) 0.0474(17) Uani 1 1 d D . . H43 H -0.5132 -0.1476 0.1061 0.057 Uiso 1 1 calc R . . C44 C -0.5496(10) -0.1474(5) -0.0229(4) 0.0525(18) Uani 1 1 d . . . H44A H -0.5396 -0.1136 -0.0693 0.063 Uiso 1 1 calc R . . H44B H -0.6518 -0.1302 -0.0042 0.063 Uiso 1 1 calc R . . C45 C -0.5358(10) -0.2531(5) -0.0146(3) 0.055(2) Uani 1 1 d . . . C46 C -0.590(3) -0.2849(7) -0.0589(6) 0.192(10) Uani 1 1 d . . . H46 H -0.6375 -0.2427 -0.0933 0.230 Uiso 1 1 calc R . . C47 C -0.4955(10) -0.3198(5) 0.0395(4) 0.059(2) Uani 1 1 d . . . H47 H -0.4748 -0.3006 0.0744 0.070 Uiso 1 1 calc R . . C48 C -0.575(3) -0.3820(7) -0.0526(7) 0.236(14) Uani 1 1 d . . . H48 H -0.6125 -0.4025 -0.0836 0.284 Uiso 1 1 calc R . . C49 C -0.4834(10) -0.4154(5) 0.0455(4) 0.055(2) Uani 1 1 d . . . H49 H -0.4577 -0.4583 0.0846 0.067 Uiso 1 1 calc R . . C50 C -0.5075(14) -0.4485(5) -0.0030(4) 0.080(3) Uani 1 1 d . . . N1 N -0.0681(7) -0.1442(4) 0.5451(3) 0.0479(14) Uani 1 1 d D . . N2 N -0.0636(6) -0.2898(4) 0.6125(3) 0.0452(14) Uani 1 1 d D . . N3 N -0.0774(7) 0.1297(4) -0.0688(3) 0.0482(15) Uani 1 1 d D . . N4 N -0.1075(6) 0.2822(4) -0.1168(3) 0.0435(13) Uani 1 1 d D . . N5 N 0.0440(6) 0.0083(4) 0.5935(2) 0.0476(14) Uani 1 1 d D . . N6 N 0.0450(7) 0.0725(6) 0.6729(3) 0.066(2) Uani 1 1 d D . . N7 N 0.2290(6) -0.0606(5) 0.4822(3) 0.0507(15) Uani 1 1 d D . . N8 N 0.4161(7) -0.1654(5) 0.4668(4) 0.070(2) Uani 1 1 d D . . N9 N -0.2207(7) -0.0596(4) 0.0177(3) 0.0474(15) Uani 1 1 d D . . N10 N -0.4345(7) -0.1167(3) 0.0076(3) 0.0446(14) Uani 1 1 d D . . N100 N 1.147(2) -0.2181(7) 0.7553(6) 0.144(6) Uani 1 1 d . . . N200 N 0.5919(11) 0.1907(8) 0.7204(6) 0.090(3) Uani 1 1 d . . . O1S O -0.0269(10) -0.2294(6) -0.0850(4) 0.113(3) Uiso 1 1 d . . . H1S H 0.0221 -0.2223 -0.1212 0.170 Uiso 1 1 calc R . . O2S O 0.5811(11) -0.0271(7) 0.8189(5) 0.122(3) Uiso 1 1 d . . . H2S H 0.5523 0.0222 0.7924 0.183 Uiso 1 1 calc R . . O101 O 0.9919(15) -0.2172(11) 0.7720(10) 0.223(9) Uani 1 1 d . . . O102 O 1.2388(12) -0.2315(6) 0.6984(5) 0.117(3) Uani 1 1 d . . . O103 O 1.2472(14) -0.2083(6) 0.7890(6) 0.170(6) Uani 1 1 d . . . O201 O 0.5611(12) 0.1684(7) 0.7750(4) 0.126(3) Uani 1 1 d . . . O202 O 0.6338(11) 0.2739(8) 0.6934(5) 0.132(3) Uani 1 1 d . . . O203 O 0.6143(13) 0.1438(7) 0.6826(4) 0.131(3) Uani 1 1 d . . . Co1 Co 0.0000 0.0000 0.5000 0.0388(4) Uani 1 2 d S . . Co2 Co 0.0000 0.0000 0.0000 0.0495(4) Uani 1 2 d S . . O2W O 0.7180(9) 0.0477(5) 0.1773(3) 0.084(2) Uani 1 1 d . . . O1W O -0.0544(8) 0.0607(4) 0.0786(2) 0.0643(16) Uani 1 1 d D . . H2W H -0.038(9) 0.125(2) 0.071(4) 0.077 Uiso 1 1 d D . . H1W H -0.134(7) 0.045(5) 0.114(3) 0.077 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.052(4) 0.061(5) 0.033(4) -0.001(3) -0.006(3) -0.015(4) C2 0.056(5) 0.072(5) 0.038(4) -0.009(4) -0.005(3) -0.025(4) C3 0.071(5) 0.062(5) 0.042(4) -0.005(4) -0.007(4) -0.031(4) C4 0.038(4) 0.059(4) 0.044(4) 0.010(3) -0.008(3) -0.013(3) C5 0.040(4) 0.055(4) 0.034(3) 0.004(3) -0.005(3) -0.014(3) C6 0.045(4) 0.056(4) 0.046(4) -0.009(3) -0.007(3) -0.005(3) C7 0.064(5) 0.056(5) 0.056(5) -0.011(4) 0.002(4) -0.029(4) C8 0.042(4) 0.044(4) 0.045(4) -0.005(3) -0.010(3) -0.011(3) C9 0.062(5) 0.053(4) 0.045(4) -0.012(3) 0.010(3) -0.017(4) C10 0.046(4) 0.049(4) 0.027(3) 0.000(3) -0.008(3) -0.015(3) C11 0.046(4) 0.038(3) 0.022(3) 0.000(2) -0.008(3) -0.008(3) C12 0.044(4) 0.041(4) 0.038(3) -0.009(3) -0.003(3) -0.004(3) C13 0.052(4) 0.036(4) 0.044(4) 0.002(3) -0.004(3) -0.011(3) C14 0.047(4) 0.035(3) 0.050(4) -0.010(3) 0.000(3) -0.012(3) C15 0.045(4) 0.033(3) 0.048(4) -0.003(3) -0.006(3) -0.002(3) C16 0.041(4) 0.040(4) 0.035(3) -0.007(3) -0.005(3) -0.008(3) C17 0.052(4) 0.039(4) 0.063(5) -0.010(3) 0.000(4) -0.012(3) C18 0.050(4) 0.040(4) 0.047(4) -0.013(3) 0.007(3) -0.018(3) C19 0.053(4) 0.052(4) 0.045(4) -0.012(3) 0.010(3) -0.020(3) C20 0.081(5) 0.049(4) 0.039(4) -0.019(3) 0.015(4) -0.031(4) C21 0.042(4) 0.100(6) 0.037(4) -0.015(4) 0.002(3) -0.023(4) C22 0.041(4) 0.076(5) 0.040(4) -0.003(4) -0.013(3) -0.010(4) C23 0.052(5) 0.115(7) 0.033(4) -0.015(4) -0.006(3) -0.024(5) C24 0.054(5) 0.163(10) 0.052(5) -0.051(6) 0.010(4) -0.037(6) C25 0.046(5) 0.140(9) 0.056(5) -0.056(6) -0.004(4) -0.001(5) C26 0.036(4) 0.139(10) 0.076(6) -0.061(7) -0.012(4) -0.001(5) C27 0.041(4) 0.139(9) 0.039(4) -0.024(5) -0.003(3) -0.022(5) C28 0.040(4) 0.115(8) 0.066(5) -0.053(6) -0.027(4) 0.026(5) C29 0.039(4) 0.129(8) 0.047(4) -0.031(5) -0.020(4) 0.004(5) C30 0.039(4) 0.103(7) 0.058(5) -0.039(5) -0.015(4) 0.012(4) C31 0.040(4) 0.106(7) 0.059(5) -0.038(5) -0.027(4) 0.035(4) C32 0.060(5) 0.096(7) 0.059(5) -0.030(5) -0.030(4) 0.027(5) C33 0.055(5) 0.095(7) 0.058(5) -0.025(5) -0.022(4) 0.018(5) C34 0.067(6) 0.114(8) 0.060(5) -0.037(6) -0.038(5) 0.049(6) C35 0.056(5) 0.105(8) 0.057(5) -0.029(5) -0.028(4) 0.021(5) C36 0.051(5) 0.097(7) 0.070(6) -0.023(5) -0.016(4) 0.031(5) C37 0.050(5) 0.126(9) 0.081(7) -0.026(6) -0.008(5) 0.029(6) C38 0.051(5) 0.080(6) 0.052(5) -0.005(4) 0.002(4) 0.014(4) C39 0.046(6) 0.110(10) 0.34(3) -0.090(13) 0.058(10) -0.024(7) C40 0.047(6) 0.104(9) 0.250(18) -0.074(10) 0.047(8) -0.028(6) C41 0.080(5) 0.031(3) 0.037(4) -0.011(3) 0.002(4) -0.020(3) C42 0.072(5) 0.032(3) 0.037(4) -0.013(3) 0.006(3) -0.021(3) C43 0.073(5) 0.028(3) 0.041(4) -0.012(3) 0.009(3) -0.015(3) C44 0.076(5) 0.039(4) 0.045(4) -0.010(3) -0.012(4) -0.017(4) C45 0.098(6) 0.030(3) 0.038(4) -0.001(3) -0.019(4) -0.019(4) C46 0.48(3) 0.030(5) 0.092(8) -0.009(5) -0.157(14) -0.001(10) C47 0.098(6) 0.042(4) 0.044(4) -0.017(3) -0.027(4) 0.000(4) C48 0.61(4) 0.034(5) 0.108(10) -0.013(6) -0.201(18) -0.015(12) C49 0.094(6) 0.034(4) 0.041(4) -0.009(3) -0.026(4) 0.000(4) C50 0.184(11) 0.024(4) 0.041(4) 0.000(3) -0.050(5) -0.016(5) N1 0.047(3) 0.057(4) 0.035(3) -0.002(3) -0.003(2) -0.016(3) N2 0.040(3) 0.050(3) 0.037(3) 0.000(3) 0.000(2) -0.016(3) N3 0.063(4) 0.046(3) 0.038(3) -0.016(3) 0.011(3) -0.028(3) N4 0.040(3) 0.037(3) 0.052(3) -0.014(3) 0.006(3) -0.010(2) N5 0.042(3) 0.061(4) 0.030(3) 0.004(3) -0.001(2) -0.015(3) N6 0.049(4) 0.121(6) 0.030(3) -0.021(3) 0.004(3) -0.029(4) N7 0.037(3) 0.073(4) 0.037(3) -0.008(3) -0.006(2) -0.004(3) N8 0.036(4) 0.093(6) 0.082(5) -0.026(4) -0.014(3) 0.004(4) N9 0.070(4) 0.031(3) 0.040(3) -0.012(2) 0.011(3) -0.021(3) N10 0.075(4) 0.022(3) 0.036(3) -0.006(2) 0.002(3) -0.019(3) N100 0.28(2) 0.065(6) 0.099(8) -0.029(6) -0.082(11) 0.022(9) N200 0.092(7) 0.093(7) 0.106(8) -0.061(7) -0.053(6) 0.048(6) O101 0.117(9) 0.209(14) 0.36(2) -0.070(14) -0.134(12) 0.027(9) O102 0.159(8) 0.079(5) 0.112(7) -0.018(5) -0.056(6) 0.024(5) O103 0.255(13) 0.083(6) 0.233(12) -0.081(7) -0.196(11) 0.053(7) O201 0.162(9) 0.154(8) 0.052(4) -0.021(5) 0.012(5) -0.029(7) O202 0.110(7) 0.137(8) 0.140(8) -0.045(7) -0.011(6) 0.042(6) O203 0.175(10) 0.130(7) 0.098(6) -0.054(6) -0.020(6) 0.006(7) Co1 0.0324(7) 0.0503(8) 0.0278(6) -0.0003(5) -0.0044(5) -0.0089(5) Co2 0.0797(10) 0.0372(7) 0.0343(7) -0.0136(5) 0.0122(6) -0.0312(7) O2W 0.130(6) 0.080(4) 0.046(3) -0.030(3) 0.025(3) -0.035(4) O1W 0.105(5) 0.049(3) 0.045(3) -0.022(2) 0.019(3) -0.038(3) _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 C1 N1 1.319(8) . ? C1 N2 1.333(9) . ? C1 H1 0.9300 . ? C1S C2S 1.76(4) . ? C1S O1S 1.81(4) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2 C3 1.353(10) . ? C2 N1 1.380(9) . ? C2 H2 0.9300 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3 N2 1.354(9) . ? C3 H3 0.9300 . ? C3S C4S 1.45(2) . ? C3S O2S 1.500(17) . ? C3S H35A 0.9700 . ? C3S H35B 0.9700 . ? C4 N2 1.472(8) . ? C4 C5 1.515(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4S H3S1 0.9600 . ? C4S H3S2 0.9600 . ? C4S H3S3 0.9600 . ? C5 C6 1.377(10) . ? C5 C7 1.379(11) . ? C6 C8 1.392(10) . ? C6 H6 0.9300 . ? C7 C9 1.375(10) . ? C7 H7 0.9300 . ? C8 C10 1.402(10) . ? C8 H8 0.9300 . ? C9 C10 1.396(10) . ? C9 H9 0.9300 . ? C10 C11 1.494(9) . ? C11 C12 1.388(9) . ? C11 C13 1.403(10) . ? C12 C14 1.388(9) . ? C12 H12 0.9300 . ? C13 C15 1.363(9) . ? C13 H13 0.9300 . ? C14 C16 1.389(10) . ? C14 H14 0.9300 . ? C15 C16 1.399(9) . ? C15 H15 0.9300 . ? C16 C17 1.509(9) 1_446 ? C17 N4 1.480(8) . ? C17 C16 1.509(9) 1_664 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N3 1.310(8) . ? C18 N4 1.330(9) . ? C18 H18 0.9300 . ? C19 C20 1.348(10) . ? C19 N4 1.368(9) . ? C19 H19 0.9300 . ? C20 N3 1.378(9) . ? C20 H20 0.9300 . ? C21 N5 1.313(10) . ? C21 N6 1.343(9) . ? C21 H21 0.9300 . ? C22 C23 1.322(11) . ? C22 N5 1.391(8) . ? C22 H22 0.9300 . ? C23 N6 1.372(11) . ? C23 H23 0.9300 . ? C24 N6 1.463(12) . ? C24 C25 1.501(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C27 1.394(12) . ? C25 C26 1.394(14) . ? C26 C28 1.354(14) . ? C26 H26 0.9300 . ? C27 C29 1.364(13) . ? C27 H27 0.9300 . ? C28 C30 1.437(11) . ? C28 H28 0.9300 . ? C29 C30 1.409(12) . ? C29 H29 0.9300 . ? C30 C31 1.465(13) . ? C31 C33 1.406(12) . ? C31 C32 1.405(12) . ? C32 C34 1.368(14) . ? C32 H32 0.9300 . ? C33 C35 1.362(14) . ? C33 H33 0.9300 . ? C34 C36 1.392(14) 1_565 ? C34 H34 0.9300 . ? C35 C36 1.401(13) 1_565 ? C35 H35 0.9300 . ? C36 C34 1.392(14) 1_545 ? C36 C35 1.401(13) 1_545 ? C36 C37 1.516(15) . ? C37 N8 1.464(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N7 1.315(10) . ? C38 N8 1.322(10) . ? C38 H38 0.9300 . ? C39 N8 1.299(14) . ? C39 C40 1.411(15) . ? C39 H39 0.9300 . ? C40 N7 1.325(11) . ? C40 H40 0.9300 . ? C41 N9 1.299(9) . ? C41 N10 1.354(8) . ? C41 H41 0.9300 . ? C42 C43 1.339(9) . ? C42 N9 1.385(8) . ? C42 H42 0.9300 . ? C43 N10 1.375(8) . ? C43 H43 0.9300 . ? C44 N10 1.464(9) . ? C44 C45 1.517(9) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C47 1.345(10) . ? C45 C46 1.354(12) . ? C46 C48 1.398(13) . ? C46 H46 0.9300 . ? C47 C49 1.381(10) . ? C47 H47 0.9300 . ? C48 C50 1.371(14) . ? C48 H48 0.9300 . ? C49 C50 1.337(10) . ? C49 H49 0.9300 . ? C50 C50 1.487(14) 2_445 ? N1 Co1 2.177(5) . ? N3 Co2 2.153(6) . ? N5 Co1 2.154(5) . ? N7 Co1 2.140(5) . ? N9 Co2 2.156(5) . ? N100 O103 1.268(15) . ? N100 O101 1.36(2) . ? N100 O102 1.427(16) . ? N200 O201 1.125(12) . ? N200 O203 1.209(11) . ? N200 O202 1.267(14) . ? O1S H1S 0.8200 . ? O2S H2S 0.8200 . ? Co1 N7 2.140(5) 2_556 ? Co1 N5 2.154(5) 2_556 ? Co1 N1 2.177(5) 2_556 ? Co2 O1W 2.130(5) . ? Co2 O1W 2.130(5) 2 ? Co2 N3 2.153(6) 2 ? Co2 N9 2.156(5) 2 ? O1W H2W 0.94(2) . ? O1W H1W 0.94(2) . ? 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 N1 C1 N2 112.7(6) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? C2S C1S O1S 75(2) . . ? C2S C1S H1S1 116.2 . . ? O1S C1S H1S1 116.1 . . ? C2S C1S H1S2 115.9 . . ? O1S C1S H1S2 115.9 . . ? H1S1 C1S H1S2 113.0 . . ? C3 C2 N1 109.0(6) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C1S C2S H2S1 109.3 . . ? C1S C2S H2S2 109.4 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.7 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C2 C3 N2 107.5(6) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C4S C3S O2S 109.9(14) . . ? C4S C3S H35A 109.7 . . ? O2S C3S H35A 109.7 . . ? C4S C3S H35B 109.7 . . ? O2S C3S H35B 109.7 . . ? H35A C3S H35B 108.2 . . ? N2 C4 C5 111.9(5) . . ? N2 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C3S C4S H3S1 109.5 . . ? C3S C4S H3S2 109.5 . . ? H3S1 C4S H3S2 109.5 . . ? C3S C4S H3S3 109.5 . . ? H3S1 C4S H3S3 109.5 . . ? H3S2 C4S H3S3 109.5 . . ? C6 C5 C7 117.8(7) . . ? C6 C5 C4 122.1(7) . . ? C7 C5 C4 120.1(7) . . ? C5 C6 C8 121.6(7) . . ? C5 C6 H6 119.2 . . ? C8 C6 H6 119.2 . . ? C9 C7 C5 122.1(7) . . ? C9 C7 H7 119.0 . . ? C5 C7 H7 119.0 . . ? C6 C8 C10 120.1(7) . . ? C6 C8 H8 119.9 . . ? C10 C8 H8 119.9 . . ? C7 C9 C10 120.6(7) . . ? C7 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C8 117.7(6) . . ? C9 C10 C11 121.2(6) . . ? C8 C10 C11 121.1(6) . . ? C12 C11 C13 116.5(6) . . ? C12 C11 C10 122.4(6) . . ? C13 C11 C10 121.1(6) . . ? C14 C12 C11 122.2(6) . . ? C14 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C15 C13 C11 121.6(6) . . ? C15 C13 H13 119.2 . . ? C11 C13 H13 119.2 . . ? C12 C14 C16 120.5(6) . . ? C12 C14 H14 119.7 . . ? C16 C14 H14 119.7 . . ? C13 C15 C16 121.7(6) . . ? C13 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C14 C16 C15 117.5(6) . . ? C14 C16 C17 124.2(6) . 1_446 ? C15 C16 C17 118.3(6) . 1_446 ? N4 C17 C16 113.2(6) . 1_664 ? N4 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 1_664 . ? N4 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 1_664 . ? H17A C17 H17B 107.7 . . ? N3 C18 N4 112.0(6) . . ? N3 C18 H18 124.0 . . ? N4 C18 H18 124.0 . . ? C20 C19 N4 106.6(6) . . ? C20 C19 H19 126.7 . . ? N4 C19 H19 126.7 . . ? C19 C20 N3 109.1(5) . . ? C19 C20 H20 125.5 . . ? N3 C20 H20 125.5 . . ? N5 C21 N6 112.3(6) . . ? N5 C21 H21 123.9 . . ? N6 C21 H21 123.9 . . ? C23 C22 N5 109.1(6) . . ? C23 C22 H22 125.5 . . ? N5 C22 H22 125.5 . . ? C22 C23 N6 108.2(6) . . ? C22 C23 H23 125.9 . . ? N6 C23 H23 125.9 . . ? N6 C24 C25 110.3(7) . . ? N6 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? N6 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C27 C25 C26 117.0(10) . . ? C27 C25 C24 121.2(9) . . ? C26 C25 C24 121.6(9) . . ? C28 C26 C25 122.1(8) . . ? C28 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C29 C27 C25 121.9(9) . . ? C29 C27 H27 119.0 . . ? C25 C27 H27 119.0 . . ? C26 C28 C30 121.8(9) . . ? C26 C28 H28 119.1 . . ? C30 C28 H28 119.1 . . ? C27 C29 C30 122.1(8) . . ? C27 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C29 C30 C28 115.1(9) . . ? C29 C30 C31 122.3(7) . . ? C28 C30 C31 122.6(8) . . ? C33 C31 C32 117.8(10) . . ? C33 C31 C30 120.9(8) . . ? C32 C31 C30 121.3(9) . . ? C34 C32 C31 121.0(9) . . ? C34 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C35 C33 C31 120.8(9) . . ? C35 C33 H33 119.6 . . ? C31 C33 H33 119.6 . . ? C32 C34 C36 121.0(9) . 1_565 ? C32 C34 H34 119.5 . . ? C36 C34 H34 119.5 1_565 . ? C33 C35 C36 121.3(9) . 1_565 ? C33 C35 H35 119.4 . . ? C36 C35 H35 119.4 1_565 . ? C34 C36 C37 120.8(9) 1_545 . ? C35 C36 C37 121.0(10) 1_545 . ? N8 C37 C36 113.7(8) . . ? N8 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? N8 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? N7 C38 N8 112.8(7) . . ? N7 C38 H38 123.6 . . ? N8 C38 H38 123.6 . . ? N8 C39 C40 108.1(7) . . ? N8 C39 H39 126.0 . . ? C40 C39 H39 126.0 . . ? N7 C40 C39 106.8(8) . . ? N7 C40 H40 126.6 . . ? C39 C40 H40 126.6 . . ? N9 C41 N10 112.8(5) . . ? N9 C41 H41 123.6 . . ? N10 C41 H41 123.6 . . ? C43 C42 N9 109.5(5) . . ? C43 C42 H42 125.2 . . ? N9 C42 H42 125.2 . . ? C42 C43 N10 107.2(5) . . ? C42 C43 H43 126.4 . . ? N10 C43 H43 126.4 . . ? N10 C44 C45 113.9(6) . . ? N10 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? N10 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C47 C45 C46 115.9(7) . . ? C47 C45 C44 124.3(6) . . ? C46 C45 C44 119.0(7) . . ? C45 C46 C48 119.5(10) . . ? C45 C46 H46 120.3 . . ? C48 C46 H46 120.3 . . ? C45 C47 C49 122.8(7) . . ? C45 C47 H47 118.6 . . ? C49 C47 H47 118.6 . . ? C50 C48 C46 123.6(10) . . ? C50 C48 H48 118.2 . . ? C46 C48 H48 118.2 . . ? C50 C49 C47 122.2(7) . . ? C50 C49 H49 118.9 . . ? C47 C49 H49 118.9 . . ? C49 C50 C48 113.7(8) . . ? C49 C50 C50 122.3(8) . 2_445 ? C48 C50 C50 122.9(9) . 2_445 ? C1 N1 C2 104.6(5) . . ? C1 N1 Co1 125.9(5) . . ? C2 N1 Co1 127.9(4) . . ? C1 N2 C3 106.3(5) . . ? C1 N2 C4 126.8(6) . . ? C3 N2 C4 126.8(6) . . ? C18 N3 C20 105.4(5) . . ? C18 N3 Co2 124.4(5) . . ? C20 N3 Co2 130.0(4) . . ? C18 N4 C19 106.9(5) . . ? C18 N4 C17 126.0(6) . . ? C19 N4 C17 126.9(6) . . ? C21 N5 C22 104.9(5) . . ? C21 N5 Co1 127.1(5) . . ? C22 N5 Co1 125.4(5) . . ? C21 N6 C23 105.5(6) . . ? C21 N6 C24 127.7(8) . . ? C23 N6 C24 126.2(7) . . ? C38 N7 C40 106.0(6) . . ? C38 N7 Co1 127.0(5) . . ? C40 N7 Co1 125.7(6) . . ? C39 N8 C38 106.3(7) . . ? C39 N8 C37 123.7(8) . . ? C38 N8 C37 129.8(8) . . ? C41 N9 C42 105.0(5) . . ? C41 N9 Co2 130.2(4) . . ? C42 N9 Co2 124.7(4) . . ? C41 N10 C43 105.4(5) . . ? C41 N10 C44 126.9(6) . . ? C43 N10 C44 127.7(6) . . ? O103 N100 O101 127.0(15) . . ? O103 N100 O102 102.5(16) . . ? O101 N100 O102 130.6(14) . . ? O201 N200 O203 130.2(13) . . ? O201 N200 O202 117.5(10) . . ? O203 N200 O202 111.3(12) . . ? C1S O1S H1S 109.4 . . ? C3S O2S H2S 109.5 . . ? N7 Co1 N7 180.0(3) 2_556 . ? N7 Co1 N5 91.6(2) 2_556 2_556 ? N7 Co1 N5 88.4(2) . 2_556 ? N7 Co1 N5 88.4(2) 2_556 . ? N7 Co1 N5 91.6(2) . . ? N5 Co1 N5 180.000(1) 2_556 . ? N7 Co1 N1 92.8(2) 2_556 . ? N7 Co1 N1 87.2(2) . . ? N5 Co1 N1 89.6(2) 2_556 . ? N5 Co1 N1 90.4(2) . . ? N7 Co1 N1 87.2(2) 2_556 2_556 ? N7 Co1 N1 92.8(2) . 2_556 ? N5 Co1 N1 90.4(2) 2_556 2_556 ? N5 Co1 N1 89.6(2) . 2_556 ? N1 Co1 N1 180.0(4) . 2_556 ? O1W Co2 O1W 180.00(13) . 2 ? O1W Co2 N3 88.6(2) . 2 ? O1W Co2 N3 91.4(2) 2 2 ? O1W Co2 N3 91.4(2) . . ? O1W Co2 N3 88.6(2) 2 . ? N3 Co2 N3 180.0(4) 2 . ? O1W Co2 N9 92.8(2) . . ? O1W Co2 N9 87.2(2) 2 . ? N3 Co2 N9 86.3(2) 2 . ? N3 Co2 N9 93.7(2) . . ? O1W Co2 N9 87.2(2) . 2 ? O1W Co2 N9 92.8(2) 2 2 ? N3 Co2 N9 93.7(2) 2 2 ? N3 Co2 N9 86.3(2) . 2 ? N9 Co2 N9 180.0(3) . 2 ? Co2 O1W H2W 119(4) . . ? Co2 O1W H1W 127(5) . . ? H2W O1W H1W 107(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.835 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.109 data_7_lu669_[Cu(BIMB)2(H2O)2](H2O)2(acetone)2(SO4) _database_code_depnum_ccdc_archive 'CCDC 680074' _chemical_formula_sum 'C46 H56 Cu N8 O10 S' _chemical_formula_weight 976.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.1572(17) _cell_length_b 9.6534(12) _cell_length_c 17.317(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.729(2) _cell_angle_gamma 90.00 _cell_volume 2365.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3226 _cell_measurement_theta_min 3 _cell_measurement_theta_max 21 _exptl_crystal_description column _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 6 _diffrn_reflns_number 17518 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 22.53 _reflns_number_total 3104 _reflns_number_observed 2502 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The crystal is unstable in air, was collected under mineral oil. For technical problem the data were collected only up to 23. degree, but the quality of the measurement are enough to give reliable results. The two water molecules are refined without hydrogens. ; _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^)+(0.1156P)^2^+6.8203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3104 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_obs 0.0654 _refine_ls_wR_factor_all 0.1929 _refine_ls_wR_factor_obs 0.1777 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _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 C1 C -0.0802(4) 0.0462(6) 0.6545(3) 0.0257(12) Uani 1 1 d . . . H1 H -0.0873 -0.0486 0.6619 0.031 Uiso 1 1 calc R . . C2 C -0.0472(4) 0.2437(6) 0.6049(3) 0.0302(13) Uani 1 1 d . . . H2 H -0.0264 0.3108 0.5709 0.036 Uiso 1 1 calc R . . C3 C -0.0820(4) 0.2696(6) 0.6748(3) 0.0303(13) Uani 1 1 d . . . H3 H -0.0908 0.3560 0.6972 0.036 Uiso 1 1 calc R . . C4 C -0.1443(4) 0.1150(6) 0.7817(3) 0.0284(13) Uani 1 1 d . . . H4A H -0.1255 0.1870 0.8181 0.034 Uiso 1 1 calc R . . H4B H -0.1212 0.0271 0.8018 0.034 Uiso 1 1 calc R . . C5 C -0.2503(4) 0.1108(5) 0.7737(3) 0.0240(12) Uani 1 1 d . . . C6 C -0.2965(4) -0.0101(6) 0.7514(3) 0.0302(13) Uani 1 1 d . . . H6 H -0.2615 -0.0899 0.7426 0.036 Uiso 1 1 calc R . . C7 C -0.3037(4) 0.2283(6) 0.7871(3) 0.0282(13) Uani 1 1 d . . . H7 H -0.2737 0.3100 0.8024 0.034 Uiso 1 1 calc R . . C8 C -0.3932(4) -0.0137(5) 0.7422(3) 0.0296(13) Uani 1 1 d . . . H8 H -0.4228 -0.0959 0.7273 0.036 Uiso 1 1 calc R . . C9 C -0.4005(4) 0.2250(6) 0.7780(3) 0.0288(13) Uani 1 1 d . . . H9 H -0.4350 0.3049 0.7875 0.035 Uiso 1 1 calc R . . C10 C -0.4483(4) 0.1050(5) 0.7548(3) 0.0256(12) Uani 1 1 d . . . C11 C -0.1152(4) -0.2467(6) 0.5448(3) 0.0293(13) Uani 1 1 d . . . H11 H -0.0654 -0.2842 0.5741 0.035 Uiso 1 1 calc R . . C12 C -0.2533(4) -0.2208(6) 0.4898(3) 0.0351(14) Uani 1 1 d . . . H13 H -0.3159 -0.2347 0.4738 0.042 Uiso 1 1 calc R . . C13 C -0.1976(4) -0.1127(6) 0.4710(3) 0.0295(13) Uani 1 1 d . . . H12 H -0.2155 -0.0388 0.4393 0.035 Uiso 1 1 calc R . . C14 C -0.2268(4) -0.4396(6) 0.5680(4) 0.0361(14) Uani 1 1 d . . . H14A H -0.1728 -0.4792 0.5958 0.043 Uiso 1 1 calc R . . H14B H -0.2438 -0.5014 0.5257 0.043 Uiso 1 1 calc R . . C15 C -0.3089(4) -0.4295(6) 0.6219(3) 0.0327(14) Uani 1 1 d . . . C16 C -0.4002(4) -0.4588(6) 0.5964(4) 0.0366(14) Uani 1 1 d . . . H16 H -0.4116 -0.4841 0.5451 0.044 Uiso 1 1 calc R . . C17 C -0.2928(4) -0.3916(5) 0.6989(3) 0.0320(14) Uani 1 1 d . . . H17 H -0.2319 -0.3708 0.7171 0.038 Uiso 1 1 calc R . . C18 C -0.4749(4) -0.4511(6) 0.6459(3) 0.0332(14) Uani 1 1 d . . . H18 H -0.5358 -0.4701 0.6273 0.040 Uiso 1 1 calc R . . C19 C -0.3678(4) -0.3849(6) 0.7481(3) 0.0343(14) Uani 1 1 d . . . H19 H -0.3564 -0.3593 0.7993 0.041 Uiso 1 1 calc R . . C20 C -0.4602(4) -0.4154(5) 0.7234(3) 0.0285(13) Uani 1 1 d . . . C21 C 0.4244(7) -0.1383(10) 0.5498(7) 0.111(4) Uani 1 1 d . . . H21A H 0.4374 -0.1763 0.6003 0.166 Uiso 1 1 calc R . . H21B H 0.4116 -0.0410 0.5542 0.166 Uiso 1 1 calc R . . H21C H 0.4782 -0.1519 0.5182 0.166 Uiso 1 1 calc R . . C22 C 0.3435(6) -0.2069(8) 0.5151(5) 0.059(2) Uani 1 1 d . . . C23 C 0.3139(6) -0.1781(8) 0.4343(4) 0.065(2) Uani 1 1 d . . . H23A H 0.2558 -0.2258 0.4223 0.098 Uiso 1 1 calc R . . H23B H 0.3619 -0.2096 0.4005 0.098 Uiso 1 1 calc R . . H23C H 0.3047 -0.0803 0.4276 0.098 Uiso 1 1 calc R . . N1 N -0.0470(3) 0.1028(4) 0.5911(2) 0.0268(11) Uani 1 1 d . . . N2 N -0.1021(3) 0.1426(4) 0.7064(2) 0.0244(10) Uani 1 1 d . . . N3 N -0.1103(3) -0.1302(4) 0.5063(2) 0.0268(11) Uani 1 1 d . . . N4 N -0.2002(3) -0.3050(5) 0.5367(2) 0.0273(11) Uani 1 1 d . . . O1 O -0.0216(3) -0.4141(4) 0.6824(2) 0.0335(9) Uani 1 1 d . . . O2 O 0.0820(3) -0.2391(4) 0.7344(2) 0.0416(10) Uani 1 1 d . . . O3 O 0.2986(5) -0.2850(7) 0.5552(3) 0.092(2) Uani 1 1 d . . . O1W O 0.0985(3) -0.1635(4) 0.5846(2) 0.0379(10) Uani 1 1 d . . . O2W O 0.1327(9) -0.5045(9) 0.6062(8) 0.244(8) Uani 1 1 d . . . S S 0.0000 -0.32695(18) 0.7500 0.0245(5) Uani 1 2 d S . . Cu Cu 0.0000 0.0000 0.5000 0.0289(4) Uani 1 2 d S . . 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 C1 0.023(3) 0.024(3) 0.030(3) -0.002(3) 0.000(2) -0.004(2) C2 0.030(3) 0.025(3) 0.036(3) 0.007(3) 0.002(3) -0.006(2) C3 0.031(3) 0.027(3) 0.033(3) 0.001(3) 0.002(3) 0.003(2) C4 0.022(3) 0.036(3) 0.027(3) 0.002(3) 0.000(2) 0.000(2) C5 0.024(3) 0.029(3) 0.019(3) 0.001(2) 0.002(2) -0.002(2) C6 0.028(3) 0.025(3) 0.038(3) 0.001(3) 0.004(3) 0.006(2) C7 0.024(3) 0.026(3) 0.034(3) -0.003(2) -0.002(2) -0.002(2) C8 0.027(3) 0.021(3) 0.041(3) -0.006(2) 0.000(3) -0.002(2) C9 0.027(3) 0.022(3) 0.038(3) -0.001(2) 0.003(2) 0.002(2) C10 0.023(3) 0.024(3) 0.030(3) 0.002(2) 0.001(2) 0.000(2) C11 0.028(3) 0.029(3) 0.031(3) 0.004(3) 0.003(2) -0.005(2) C12 0.023(3) 0.037(4) 0.046(4) -0.001(3) -0.001(3) -0.007(3) C13 0.031(3) 0.030(3) 0.028(3) 0.004(3) 0.003(2) 0.000(2) C14 0.033(3) 0.025(3) 0.050(4) 0.006(3) 0.012(3) -0.004(3) C15 0.029(3) 0.021(3) 0.049(4) 0.011(3) 0.012(3) -0.005(2) C16 0.036(4) 0.034(3) 0.040(3) 0.008(3) 0.007(3) -0.005(3) C17 0.026(3) 0.022(3) 0.048(4) 0.000(3) 0.004(3) -0.004(2) C18 0.023(3) 0.031(3) 0.045(4) 0.010(3) 0.003(3) -0.003(2) C19 0.033(3) 0.025(3) 0.045(4) -0.004(3) 0.004(3) -0.003(2) C20 0.029(3) 0.015(3) 0.042(3) 0.006(2) 0.004(2) -0.001(2) C21 0.088(7) 0.080(7) 0.162(11) 0.047(7) -0.038(7) -0.025(6) C22 0.063(5) 0.054(5) 0.061(5) 0.000(4) -0.001(4) 0.008(4) C23 0.087(6) 0.065(5) 0.043(4) 0.003(4) -0.001(4) 0.013(4) N1 0.026(2) 0.025(3) 0.030(3) 0.006(2) 0.003(2) -0.004(2) N2 0.018(2) 0.026(3) 0.029(2) 0.002(2) 0.0013(18) -0.0012(19) N3 0.027(3) 0.029(3) 0.025(2) -0.003(2) 0.0046(19) -0.005(2) N4 0.023(2) 0.028(3) 0.031(3) 0.007(2) 0.005(2) -0.005(2) O1 0.047(2) 0.025(2) 0.027(2) -0.0077(17) -0.0018(17) -0.0036(18) O2 0.045(2) 0.040(2) 0.040(2) 0.0040(19) -0.0030(19) -0.016(2) O3 0.099(5) 0.116(5) 0.061(4) 0.012(4) 0.005(3) -0.026(4) O1W 0.038(2) 0.036(2) 0.040(2) 0.0065(19) 0.0031(18) -0.0078(18) O2W 0.274(13) 0.118(7) 0.354(16) -0.154(9) 0.251(13) -0.090(8) S 0.0315(11) 0.0184(10) 0.0235(10) 0.000 -0.0001(8) 0.000 Cu 0.0282(6) 0.0296(6) 0.0292(6) -0.0014(4) 0.0071(4) -0.0118(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 C1 N1 1.325(7) . ? C1 N2 1.337(7) . ? C1 Cu 2.971(5) . ? C1 H1 0.9300 . ? C2 C3 1.343(8) . ? C2 N1 1.381(7) . ? C2 Cu 3.059(6) . ? C2 H2 0.9300 . ? C3 N2 1.376(7) . ? C3 H3 0.9300 . ? C4 N2 1.476(7) . ? C4 C5 1.503(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C7 1.386(7) . ? C5 C6 1.387(8) . ? C6 C8 1.375(8) . ? C6 H6 0.9300 . ? C7 C9 1.376(7) . ? C7 H7 0.9300 . ? C8 C10 1.407(7) . ? C8 H8 0.9300 . ? C9 C10 1.394(7) . ? C9 H9 0.9300 . ? C10 C10 1.468(10) 2_456 ? C11 N3 1.310(7) . ? C11 N4 1.333(7) . ? C11 Cu 3.001(5) . ? C11 H11 0.9300 . ? C12 C13 1.354(8) . ? C12 N4 1.359(7) . ? C12 H13 0.9300 . ? C13 N3 1.372(7) . ? C13 Cu 3.029(5) . ? C13 H12 0.9300 . ? C14 N4 1.461(7) . ? C14 C15 1.516(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.383(8) . ? C15 C17 1.395(8) . ? C16 C18 1.384(8) . ? C16 H16 0.9300 . ? C17 C19 1.383(8) . ? C17 H17 0.9300 . ? C18 C20 1.394(8) . ? C18 H18 0.9300 . ? C19 C20 1.395(8) . ? C19 H19 0.9300 . ? C20 C20 1.477(11) 2_456 ? C21 C22 1.439(12) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O3 1.218(9) . ? C22 C23 1.474(10) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 Cu 1.994(4) . ? N3 Cu 2.010(4) . ? O1 S 1.466(4) . ? O2 S 1.469(4) . ? O1W Cu 2.541(4) . ? S O1 1.466(4) 2_556 ? S O2 1.469(4) 2_556 ? Cu N1 1.994(4) 3_556 ? Cu N3 2.010(4) 3_556 ? Cu O1W 2.541(4) 3_556 ? 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 N1 C1 N2 111.4(5) . . ? N1 C1 Cu 33.0(2) . . ? N2 C1 Cu 144.4(4) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? Cu C1 H1 91.3 . . ? C3 C2 N1 110.1(5) . . ? C3 C2 Cu 140.4(4) . . ? N1 C2 Cu 30.4(2) . . ? C3 C2 H2 125.0 . . ? N1 C2 H2 125.0 . . ? Cu C2 H2 94.6 . . ? C2 C3 N2 106.1(5) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? N2 C4 C5 110.7(4) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C7 C5 C6 118.8(5) . . ? C7 C5 C4 120.6(5) . . ? C6 C5 C4 120.6(5) . . ? C8 C6 C5 120.8(5) . . ? C8 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C9 C7 C5 120.5(5) . . ? C9 C7 H7 119.7 . . ? C5 C7 H7 119.7 . . ? C6 C8 C10 121.1(5) . . ? C6 C8 H8 119.4 . . ? C10 C8 H8 119.4 . . ? C7 C9 C10 121.7(5) . . ? C7 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C8 117.1(5) . . ? C9 C10 C10 120.4(3) . 2_456 ? C8 C10 C10 122.5(3) . 2_456 ? N3 C11 N4 111.7(5) . . ? N3 C11 Cu 31.8(2) . . ? N4 C11 Cu 143.5(4) . . ? N3 C11 H11 124.1 . . ? N4 C11 H11 124.1 . . ? Cu C11 H11 92.3 . . ? C13 C12 N4 106.8(5) . . ? C13 C12 H13 126.6 . . ? N4 C12 H13 126.6 . . ? C12 C13 N3 108.7(5) . . ? C12 C13 Cu 141.2(4) . . ? N3 C13 Cu 32.4(2) . . ? C12 C13 H12 125.6 . . ? N3 C13 H12 125.6 . . ? Cu C13 H12 93.2 . . ? N4 C14 C15 112.5(5) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 C15 C17 119.0(5) . . ? C16 C15 C14 121.1(6) . . ? C17 C15 C14 120.0(5) . . ? C15 C16 C18 121.0(6) . . ? C15 C16 H16 119.5 . . ? C18 C16 H16 119.5 . . ? C19 C17 C15 119.6(5) . . ? C19 C17 H17 120.2 . . ? C15 C17 H17 120.2 . . ? C16 C18 C20 121.0(5) . . ? C16 C18 H18 119.5 . . ? C20 C18 H18 119.5 . . ? C17 C19 C20 122.1(6) . . ? C17 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C18 C20 C19 117.3(5) . . ? C18 C20 C20 120.4(6) . 2_456 ? C19 C20 C20 122.2(6) . 2_456 ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O3 C22 C21 117.9(8) . . ? O3 C22 C23 121.3(8) . . ? C21 C22 C23 120.7(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 N1 C2 105.0(4) . . ? C1 N1 Cu 125.8(4) . . ? C2 N1 Cu 129.1(4) . . ? C1 N2 C3 107.3(4) . . ? C1 N2 C4 125.3(4) . . ? C3 N2 C4 127.3(5) . . ? C11 N3 C13 105.8(4) . . ? C11 N3 Cu 128.1(4) . . ? C13 N3 Cu 126.1(4) . . ? C11 N4 C12 107.0(4) . . ? C11 N4 C14 125.3(5) . . ? C12 N4 C14 127.5(5) . . ? O1 S O1 110.0(3) 2_556 . ? O1 S O2 109.4(2) 2_556 2_556 ? O1 S O2 109.3(2) . 2_556 ? O1 S O2 109.3(2) 2_556 . ? O1 S O2 109.4(2) . . ? O2 S O2 109.5(4) 2_556 . ? N1 Cu N1 180.00(14) . 3_556 ? N1 Cu N3 89.41(17) . . ? N1 Cu N3 90.59(17) 3_556 . ? N1 Cu N3 90.59(17) . 3_556 ? N1 Cu N3 89.41(17) 3_556 3_556 ? N3 Cu N3 180.00(15) . 3_556 ? N1 Cu O1W 92.50(15) . . ? N1 Cu O1W 87.50(15) 3_556 . ? N3 Cu O1W 89.66(15) . . ? N3 Cu O1W 90.34(15) 3_556 . ? N1 Cu O1W 87.50(15) . 3_556 ? N1 Cu O1W 92.50(15) 3_556 3_556 ? N3 Cu O1W 90.34(15) . 3_556 ? N3 Cu O1W 89.66(15) 3_556 3_556 ? O1W Cu O1W 180.00(14) . 3_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.437 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.092 data_8_lu675_Cu(bimb)2(NO3)2 _database_code_depnum_ccdc_archive 'CCDC 680075' _chemical_formula_sum 'C40 H36 Cu N10 O6' _chemical_formula_weight 816.33 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8500(6) _cell_length_b 9.0910(7) _cell_length_c 13.2400(10) _cell_angle_alpha 71.503(3) _cell_angle_beta 83.998(3) _cell_angle_gamma 67.939(3) _cell_volume 936.11(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 778 _cell_measurement_theta_min 3 _cell_measurement_theta_max 17 _exptl_crystal_description blue _exptl_crystal_colour block _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 423 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 8341 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3301 _reflns_number_observed 1982 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The nitrate anion is modelled on two different position with two oxygen disordered with occupation 63%:37%. The two oxygen with the smaller occupation are refined isotropically. ; _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^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3301 _refine_ls_number_parameters 268 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_obs 0.0737 _refine_ls_wR_factor_all 0.1850 _refine_ls_wR_factor_obs 0.1587 _refine_ls_goodness_of_fit_all 1.005 _refine_ls_restrained_S_all 1.051 _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 C1 C -0.0103(7) -0.1727(6) 0.7329(4) 0.0530(14) Uani 1 1 d . . . H1 H -0.0879 -0.0773 0.7447 0.064 Uiso 1 1 calc R . . C2 C 0.0623(7) -0.3164(7) 0.8091(4) 0.0585(15) Uani 1 1 d . . . H2 H 0.0443 -0.3388 0.8820 0.070 Uiso 1 1 calc R . . C3 C 0.1545(7) -0.3419(7) 0.6555(4) 0.0573(15) Uani 1 1 d . . . H3 H 0.2137 -0.3877 0.6035 0.069 Uiso 1 1 calc R . . C4 C 0.2785(7) -0.5925(6) 0.8099(5) 0.0654(16) Uani 1 1 d . . . H4A H 0.3480 -0.5902 0.8609 0.078 Uiso 1 1 calc R . . H4B H 0.3478 -0.6356 0.7562 0.078 Uiso 1 1 calc R . . C5 C 0.1893(7) -0.7083(6) 0.8665(5) 0.0538(14) Uani 1 1 d . . . C6 C 0.0700(7) -0.7221(7) 0.8175(5) 0.0686(18) Uani 1 1 d . . . H6 H 0.0377 -0.6548 0.7482 0.082 Uiso 1 1 calc R . . C7 C 0.2328(8) -0.8075(7) 0.9683(4) 0.0641(16) Uani 1 1 d . . . H7 H 0.3134 -0.7987 1.0032 0.077 Uiso 1 1 calc R . . C8 C -0.0046(7) -0.8357(7) 0.8695(5) 0.0675(17) Uani 1 1 d . . . H8 H -0.0858 -0.8427 0.8340 0.081 Uiso 1 1 calc R . . C9 C 0.1594(8) -0.9221(7) 1.0217(4) 0.0629(16) Uani 1 1 d . . . H9 H 0.1920 -0.9884 1.0911 0.076 Uiso 1 1 calc R . . C10 C 0.0389(6) -0.9377(6) 0.9721(4) 0.0511(14) Uani 1 1 d . . . C11 C -0.1819(8) -0.2214(7) 0.4831(5) 0.0681(17) Uani 1 1 d . . . H11 H -0.1069 -0.3207 0.5241 0.082 Uiso 1 1 calc R . . C12 C -0.3198(8) -0.2060(7) 0.4393(5) 0.0666(17) Uani 1 1 d . . . H12 H -0.3576 -0.2910 0.4452 0.080 Uiso 1 1 calc R . . C13 C -0.3006(7) 0.0329(7) 0.4002(5) 0.0635(16) Uani 1 1 d . . . H13 H -0.3264 0.1473 0.3724 0.076 Uiso 1 1 calc R . . C14 C -0.5447(7) 0.0353(7) 0.3229(5) 0.0697(17) Uani 1 1 d . . . H14A H -0.6347 0.0786 0.3669 0.084 Uiso 1 1 calc R . . H14B H -0.5651 -0.0470 0.3000 0.084 Uiso 1 1 calc R . . C15 C -0.5351(6) 0.1757(7) 0.2263(4) 0.0525(14) Uani 1 1 d . . . C16 C -0.6313(8) 0.3369(8) 0.2118(5) 0.087(2) Uani 1 1 d . . . H16 H -0.7096 0.3632 0.2624 0.105 Uiso 1 1 calc R . . C17 C -0.4239(8) 0.1464(7) 0.1494(5) 0.081(2) Uani 1 1 d . . . H17 H -0.3544 0.0373 0.1565 0.097 Uiso 1 1 calc R . . C18 C -0.6179(8) 0.4628(8) 0.1257(6) 0.090(2) Uani 1 1 d . . . H18 H -0.6849 0.5721 0.1204 0.108 Uiso 1 1 calc R . . C19 C -0.4097(8) 0.2692(7) 0.0627(5) 0.079(2) Uani 1 1 d . . . H19 H -0.3309 0.2418 0.0126 0.094 Uiso 1 1 calc R . . C20 C -0.5080(6) 0.4318(6) 0.0470(4) 0.0487(13) Uani 1 1 d . . . N1 N 0.0469(5) -0.1883(5) 0.6361(3) 0.0495(11) Uani 1 1 d . . . N2 N 0.1670(5) -0.4220(5) 0.7588(3) 0.0518(11) Uani 1 1 d . . . N3 N -0.1689(6) -0.0672(5) 0.4577(3) 0.0543(12) Uani 1 1 d . . . N4 N -0.3927(6) -0.0432(6) 0.3852(3) 0.0554(12) Uani 1 1 d . . . Cu Cu 0.0000 0.0000 0.5000 0.0579(4) Uani 1 2 d S . . N5 N 0.2819(9) -0.2968(7) 0.3731(4) 0.092(2) Uani 1 1 d D . . O1 O 0.3342(7) -0.2546(7) 0.2831(4) 0.1159(19) Uani 1 1 d D A . O2 O 0.2426(10) -0.1939(8) 0.4236(6) 0.071(3) Uani 0.628(12) 1 d PD A 1 O3 O 0.2241(11) -0.4105(9) 0.4067(6) 0.104(4) Uani 0.628(12) 1 d PD A 1 O10 O 0.399(2) -0.420(2) 0.4327(12) 0.166(9) Uiso 0.372(12) 1 d PD A 2 O11 O 0.168(2) -0.213(3) 0.4080(14) 0.151(10) Uiso 0.372(12) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(4) 0.041(3) 0.047(3) -0.008(3) 0.004(3) -0.016(3) C2 0.076(4) 0.052(4) 0.042(3) -0.016(3) 0.014(3) -0.019(3) C3 0.080(4) 0.043(3) 0.054(3) -0.014(3) 0.017(3) -0.032(3) C4 0.062(4) 0.042(3) 0.078(4) -0.001(3) 0.005(3) -0.020(3) C5 0.050(3) 0.029(3) 0.077(4) -0.014(3) 0.016(3) -0.015(3) C6 0.053(3) 0.042(3) 0.084(4) 0.019(3) -0.010(3) -0.017(3) C7 0.091(5) 0.066(4) 0.055(4) -0.020(3) 0.014(3) -0.051(4) C8 0.051(3) 0.045(3) 0.087(4) 0.007(3) -0.007(3) -0.017(3) C9 0.096(5) 0.058(4) 0.052(3) -0.024(3) 0.022(3) -0.046(4) C10 0.054(3) 0.031(3) 0.069(4) -0.022(3) 0.022(3) -0.016(3) C11 0.090(5) 0.042(3) 0.067(4) -0.004(3) -0.014(4) -0.025(3) C12 0.095(5) 0.043(3) 0.070(4) -0.014(3) 0.004(4) -0.037(3) C13 0.061(4) 0.048(3) 0.073(4) 0.004(3) -0.001(3) -0.028(3) C14 0.064(4) 0.072(4) 0.072(4) -0.006(3) 0.005(3) -0.037(3) C15 0.047(3) 0.059(4) 0.052(3) -0.011(3) 0.005(3) -0.026(3) C16 0.086(5) 0.061(4) 0.094(5) -0.018(4) 0.049(4) -0.021(4) C17 0.086(5) 0.040(3) 0.078(4) -0.003(3) 0.029(4) 0.000(3) C18 0.093(5) 0.043(4) 0.107(5) -0.018(4) 0.059(4) -0.013(4) C19 0.090(5) 0.043(4) 0.068(4) -0.013(3) 0.039(4) 0.000(3) C20 0.046(3) 0.046(3) 0.054(3) -0.015(2) 0.006(3) -0.016(3) N1 0.065(3) 0.044(3) 0.043(3) -0.008(2) 0.004(2) -0.029(3) N2 0.058(3) 0.039(3) 0.055(3) -0.003(2) 0.009(2) -0.026(2) N3 0.069(3) 0.046(3) 0.049(3) -0.006(2) 0.007(2) -0.030(3) N4 0.062(3) 0.056(3) 0.051(3) -0.010(2) 0.011(2) -0.033(3) Cu 0.0839(8) 0.0520(6) 0.0422(6) -0.0009(4) 0.0032(5) -0.0409(6) N5 0.150(7) 0.068(4) 0.052(3) -0.002(3) -0.009(4) -0.041(4) O1 0.140(5) 0.154(5) 0.089(4) -0.063(4) 0.038(4) -0.080(4) O2 0.075(5) 0.068(5) 0.083(5) -0.037(4) 0.040(4) -0.037(4) O3 0.147(9) 0.067(5) 0.117(7) -0.027(5) 0.026(6) -0.065(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.344(7) . ? C1 N1 1.358(6) . ? C1 H1 0.9300 . ? C2 N2 1.353(6) . ? C2 H2 0.9300 . ? C3 N1 1.322(6) . ? C3 N2 1.324(6) . ? C3 H3 0.9300 . ? C4 N2 1.469(6) . ? C4 C5 1.514(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.359(8) . ? C5 C7 1.362(7) . ? C6 C8 1.394(7) . ? C6 H6 0.9300 . ? C7 C9 1.397(7) . ? C7 H7 0.9300 . ? C8 C10 1.377(8) . ? C8 H8 0.9300 . ? C9 C10 1.381(8) . ? C9 H9 0.9300 . ? C10 C10 1.501(9) 2_537 ? C11 C12 1.347(8) . ? C11 N3 1.380(6) . ? C11 H11 0.9300 . ? C12 N4 1.352(7) . ? C12 H12 0.9300 . ? C13 N3 1.310(6) . ? C13 N4 1.314(7) . ? C13 H13 0.9300 . ? C14 N4 1.463(7) . ? C14 C15 1.515(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.353(8) . ? C15 C17 1.357(8) . ? C16 C18 1.367(8) . ? C16 H16 0.9300 . ? C17 C19 1.358(7) . ? C17 H17 0.9300 . ? C18 C20 1.371(7) . ? C18 H18 0.9300 . ? C19 C20 1.365(7) . ? C19 H19 0.9300 . ? C20 C20 1.491(10) 2_465 ? N1 Cu 2.004(4) . ? N3 Cu 2.000(4) . ? Cu N3 2.000(4) 2_556 ? Cu N1 2.004(4) 2_556 ? Cu O11 2.528(16) . ? Cu O2 2.565(7) . ? N5 O11 1.169(12) . ? N5 O1 1.229(6) . ? N5 O2 1.243(7) . ? N5 O3 1.259(7) . ? N5 O10 1.301(11) . ? 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 C2 C1 N1 109.6(5) . . ? C2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? C1 C2 N2 106.4(5) . . ? C1 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? N1 C3 N2 111.1(5) . . ? N1 C3 H3 124.5 . . ? N2 C3 H3 124.5 . . ? N2 C4 C5 112.6(4) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C7 118.1(5) . . ? C6 C5 C4 122.1(5) . . ? C7 C5 C4 119.8(5) . . ? C5 C6 C8 121.0(5) . . ? C5 C6 H6 119.5 . . ? C8 C6 H6 119.5 . . ? C5 C7 C9 121.7(6) . . ? C5 C7 H7 119.1 . . ? C9 C7 H7 119.1 . . ? C10 C8 C6 121.6(6) . . ? C10 C8 H8 119.2 . . ? C6 C8 H8 119.2 . . ? C10 C9 C7 120.5(5) . . ? C10 C9 H9 119.7 . . ? C7 C9 H9 119.7 . . ? C8 C10 C9 117.1(5) . . ? C8 C10 C10 121.9(7) . 2_537 ? C9 C10 C10 121.0(6) . 2_537 ? C12 C11 N3 109.6(5) . . ? C12 C11 H11 125.2 . . ? N3 C11 H11 125.2 . . ? C11 C12 N4 106.7(5) . . ? C11 C12 H12 126.6 . . ? N4 C12 H12 126.6 . . ? N3 C13 N4 113.8(5) . . ? N3 C13 H13 123.1 . . ? N4 C13 H13 123.1 . . ? N4 C14 C15 110.6(4) . . ? N4 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C17 115.6(5) . . ? C16 C15 C14 123.2(5) . . ? C17 C15 C14 121.2(5) . . ? C15 C16 C18 122.5(6) . . ? C15 C16 H16 118.7 . . ? C18 C16 H16 118.7 . . ? C15 C17 C19 122.9(6) . . ? C15 C17 H17 118.6 . . ? C19 C17 H17 118.6 . . ? C16 C18 C20 121.6(6) . . ? C16 C18 H18 119.2 . . ? C20 C18 H18 119.2 . . ? C17 C19 C20 121.7(5) . . ? C17 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C18 115.7(5) . . ? C19 C20 C20 122.3(6) . 2_465 ? C18 C20 C20 122.0(6) . 2_465 ? C3 N1 C1 105.4(4) . . ? C3 N1 Cu 129.1(4) . . ? C1 N1 Cu 124.7(4) . . ? C3 N2 C2 107.6(4) . . ? C3 N2 C4 126.2(5) . . ? C2 N2 C4 126.2(5) . . ? C13 N3 C11 103.5(5) . . ? C13 N3 Cu 126.0(4) . . ? C11 N3 Cu 130.5(4) . . ? C13 N4 C12 106.5(5) . . ? C13 N4 C14 126.1(5) . . ? C12 N4 C14 127.4(5) . . ? N3 Cu N3 180.000(1) . 2_556 ? N3 Cu N1 91.00(16) . . ? N3 Cu N1 89.00(16) 2_556 . ? N3 Cu N1 89.00(16) . 2_556 ? N3 Cu N1 91.00(16) 2_556 2_556 ? N1 Cu N1 180.0 . 2_556 ? N3 Cu O11 77.7(6) . . ? N3 Cu O11 102.3(6) 2_556 . ? N1 Cu O11 87.1(4) . . ? N1 Cu O11 92.9(4) 2_556 . ? N3 Cu O2 95.9(2) . . ? N3 Cu O2 84.1(2) 2_556 . ? N1 Cu O2 86.3(2) . . ? N1 Cu O2 93.7(2) 2_556 . ? O11 Cu O2 18.2(5) . . ? O11 N5 O1 125.0(10) . . ? O11 N5 O2 38.9(11) . . ? O1 N5 O2 116.5(6) . . ? O11 N5 O3 87.5(14) . . ? O1 N5 O3 125.0(7) . . ? O2 N5 O3 115.6(7) . . ? O11 N5 O10 122.9(11) . . ? O1 N5 O10 108.4(9) . . ? O2 N5 O10 101.8(10) . . ? O3 N5 O10 76.6(10) . . ? N5 O2 Cu 143.8(7) . . ? N5 O11 Cu 159.0(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.396 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.066 data_9_Lu673_[Zn(bimb)3(SO4)2](bimb) _database_code_depnum_ccdc_archive 'CCDC 680076' _chemical_formula_sum 'C80 H72 N16 O8 S2 Zn2' _chemical_formula_weight 1580.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 14.862(5) _cell_length_b 16.693(6) _cell_length_c 34.116(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.453(5) _cell_angle_gamma 90.00 _cell_volume 8411(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2306 _cell_measurement_theta_min 2 _cell_measurement_theta_max 18 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6564 _exptl_absorpt_correction_T_max 0.7459 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 106415 _diffrn_reflns_av_R_equivalents 0.2210 _diffrn_reflns_av_sigmaI/netI 0.2947 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 29.42 _reflns_number_total 21768 _reflns_number_observed 4309 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. Empirical Absorption correction with SADABS: Sheldrick, G. M. (1996). University of Gottingen, Germany. The structure contains disordered solvents Methanol and water and all the crystals tested showed weak diffraction, hence the high R(int) Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.1291 for 4738 Fo > 4sig(Fo) and 0.4170 for all 21768 data 1048 parameters refined using 30 restraints One bimb molecule is chlatrate with no H-bond to the framework, hence it is acceptable to find high Ueq as compared to neighbors for all his atoms. One sulphate anion (S2a,b) is refined over two positions with two pivot Oxygens, with refined occupancy 86%:14%. All the atoms were refined isotropically and with constrains. ; _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^)+(0.1515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 21768 _refine_ls_number_parameters 961 _refine_ls_number_restraints 171 _refine_ls_R_factor_all 0.3186 _refine_ls_R_factor_obs 0.0993 _refine_ls_wR_factor_all 0.3126 _refine_ls_wR_factor_obs 0.2438 _refine_ls_goodness_of_fit_all 0.719 _refine_ls_restrained_S_all 0.723 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.004 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 C7 C 0.4222(6) 0.8814(6) 0.2165(3) 0.081(3) Uani 1 1 d . . . H7 H 0.4099 0.8447 0.1961 0.097 Uiso 1 1 calc R . . C16 C 1.0320(6) 0.8824(5) 0.1199(2) 0.069(2) Uani 1 1 d . . . C17 C 1.2115(6) 0.7472(6) 0.0142(4) 0.089(3) Uani 1 1 d . . . H17 H 1.1490 0.7512 0.0081 0.106 Uiso 1 1 calc R . . C21 C 0.8772(5) 0.9272(5) 0.1357(3) 0.095(3) Uani 1 1 d . . . H21 H 0.8561 0.8756 0.1299 0.115 Uiso 1 1 calc R . . C22 C 0.9666(5) 0.9434(5) 0.1334(2) 0.064(2) Uani 1 1 d . . . C24 C 0.4601(6) 0.9553(6) 0.2141(3) 0.084(3) Uani 1 1 d . . . H24 H 0.4789 0.9778 0.1914 0.101 Uiso 1 1 calc R . . C26 C 0.6549(6) 1.1104(5) 0.2068(3) 0.078(3) Uani 1 1 d . . . H26 H 0.6100 1.1231 0.1866 0.093 Uiso 1 1 calc R . . C27 C 0.3641(5) 0.8012(5) 0.2693(3) 0.087(3) Uani 1 1 d . . . H27A H 0.3860 0.7939 0.2969 0.104 Uiso 1 1 calc R . . H27B H 0.3818 0.7545 0.2550 0.104 Uiso 1 1 calc R . . C28 C 0.2621(5) 0.8069(5) 0.2649(3) 0.068(2) Uani 1 1 d . . . C31 C 1.2090(7) 0.6996(5) 0.0827(3) 0.104(3) Uani 1 1 d . . . H31A H 1.2551 0.6871 0.1043 0.125 Uiso 1 1 calc R . . H31B H 1.1744 0.6513 0.0761 0.125 Uiso 1 1 calc R . . C32 C 1.3420(6) 0.7271(5) 0.0446(3) 0.073(2) Uani 1 1 d . . . H32 H 1.3864 0.7135 0.0649 0.088 Uiso 1 1 calc R . . C33 C 1.2743(6) 0.7623(5) -0.0110(3) 0.081(3) Uani 1 1 d . . . H33 H 1.2626 0.7786 -0.0372 0.097 Uiso 1 1 calc R . . C34 C -0.0274(6) 0.8277(5) 0.2519(3) 0.079(3) Uani 1 1 d . . . C35 C 0.9009(7) 0.8889(7) 0.6541(4) 0.112(4) Uani 1 1 d . . . H35 H 0.9529 0.8835 0.6415 0.134 Uiso 1 1 calc R . . C36 C 0.4319(5) 0.9381(6) 0.2738(3) 0.073(2) Uani 1 1 d . . . H36 H 0.4272 0.9469 0.3004 0.088 Uiso 1 1 calc R . . C37 C 0.9962(6) 1.0190(6) 0.1418(3) 0.086(3) Uani 1 1 d . . . H37 H 1.0565 1.0319 0.1402 0.103 Uiso 1 1 calc R . . C38 C 1.5801(5) 0.9052(6) -0.0177(3) 0.062(2) Uani 1 1 d . . . H38 H 1.5858 0.8977 -0.0443 0.074 Uiso 1 1 calc R . . C39 C 0.8551(6) 0.8548(6) 0.5672(4) 0.093(3) Uani 1 1 d . . . H39 H 0.8923 0.8990 0.5729 0.112 Uiso 1 1 calc R . . C40 C 1.1212(6) 0.8864(6) 0.1301(3) 0.098(3) Uani 1 1 d . . . H40 H 1.1455 0.9286 0.1456 0.118 Uiso 1 1 calc R . . C41 C 0.8484(6) 1.0591(6) 0.1557(3) 0.086(3) Uani 1 1 d . . . C42 C 1.7617(5) 1.0233(5) -0.0078(4) 0.075(3) Uani 1 1 d . . . C43 C 0.8146(7) 0.8605(6) 0.6349(4) 0.096(3) Uani 1 1 d . . . C44 C 0.4259(6) 1.2134(7) 0.2068(3) 0.085(3) Uani 1 1 d . . . H44 H 0.4413 1.1878 0.1843 0.102 Uiso 1 1 calc R . . C45 C -0.0801(6) 0.7968(6) 0.2197(3) 0.093(3) Uani 1 1 d . . . H45 H -0.0542 0.7684 0.2003 0.112 Uiso 1 1 calc R . . C46 C 0.0715(6) 0.8187(5) 0.2571(3) 0.070(2) Uani 1 1 d . . . C47 C 1.5768(5) 0.6025(5) -0.0201(3) 0.066(2) Uani 1 1 d . . . H47 H 1.5707 0.6077 -0.0474 0.079 Uiso 1 1 calc R . . C48 C 1.5684(5) 0.6241(6) 0.0404(3) 0.075(2) Uani 1 1 d . . . H48 H 1.5548 0.6476 0.0638 0.090 Uiso 1 1 calc R . . C49 C 0.8494(7) 0.8211(6) 0.5301(4) 0.101(3) Uani 1 1 d . . . H49 H 0.8801 0.8430 0.5104 0.121 Uiso 1 1 calc R . . C50 C 1.1778(6) 0.8283(8) 0.1177(3) 0.113(4) Uani 1 1 d . . . H50 H 1.2399 0.8331 0.1246 0.135 Uiso 1 1 calc R . . C52 C 1.9509(5) 0.4949(5) -0.0029(3) 0.075(3) Uani 1 1 d . . . C53 C 0.7835(7) 1.1237(5) 0.1657(3) 0.105(3) Uani 1 1 d . . . H53A H 0.8156 1.1743 0.1691 0.126 Uiso 1 1 calc R . . H53B H 0.7360 1.1296 0.1440 0.126 Uiso 1 1 calc R . . C54 C 0.0704(6) 1.3712(6) 0.2200(3) 0.102(3) Uani 1 1 d . . . H54 H 0.0362 1.3922 0.1979 0.122 Uiso 1 1 calc R . . C55 C 0.7484(7) 0.7237(7) 0.5511(5) 0.103(4) Uani 1 1 d . . . H55 H 0.7113 0.6795 0.5452 0.123 Uiso 1 1 calc R . . C56 C 0.1164(6) 0.7986(5) 0.2258(3) 0.083(3) Uani 1 1 d . . . H56 H 0.0837 0.7889 0.2014 0.100 Uiso 1 1 calc R . . C58 C 0.8162(6) 0.9844(6) 0.1464(3) 0.103(3) Uani 1 1 d . . . H58 H 0.7554 0.9719 0.1471 0.123 Uiso 1 1 calc R . . C59 C 0.1217(6) 0.8302(6) 0.2926(3) 0.091(3) Uani 1 1 d . . . H59 H 0.0919 0.8420 0.3144 0.109 Uiso 1 1 calc R . . C60 C 0.7866(7) 1.0865(6) 0.2379(4) 0.102(3) Uani 1 1 d . . . H60 H 0.8486 1.0786 0.2437 0.122 Uiso 1 1 calc R . . C61 C 1.1462(7) 0.7647(6) 0.0958(3) 0.085(3) Uani 1 1 d . . . C62 C 1.6579(5) 0.4726(5) -0.0188(3) 0.090(3) Uani 1 1 d . . . H62A H 1.6357 0.4696 -0.0466 0.108 Uiso 1 1 calc R . . H62B H 1.6399 0.4239 -0.0063 0.108 Uiso 1 1 calc R . . C63 C 0.2096(6) 0.7926(5) 0.2296(3) 0.083(3) Uani 1 1 d . . . H63 H 0.2379 0.7784 0.2077 0.100 Uiso 1 1 calc R . . C65 C 1.6583(5) 1.0360(5) -0.0124(3) 0.098(3) Uani 1 1 d . . . H65A H 1.6444 1.0845 0.0014 0.118 Uiso 1 1 calc R . . H65B H 1.6370 1.0430 -0.0401 0.118 Uiso 1 1 calc R . . C66 C 0.1770(8) 1.3097(7) 0.2833(4) 0.114(4) Uani 1 1 d . . . H66 H 0.2136 1.2879 0.3046 0.137 Uiso 1 1 calc R . . C67 C 1.5471(5) 0.8886(6) 0.0408(3) 0.073(2) Uani 1 1 d . . . H67 H 1.5239 0.8672 0.0627 0.088 Uiso 1 1 calc R . . C68 C 0.3187(5) 1.3655(6) 0.2619(4) 0.125(4) Uani 1 1 d . . . H68A H 0.3333 1.4150 0.2491 0.150 Uiso 1 1 calc R . . H68B H 0.3391 1.3704 0.2898 0.150 Uiso 1 1 calc R . . C69 C 0.8352(10) 0.9348(6) 0.7117(4) 0.106(4) Uani 1 1 d . . . C70 C 1.5918(6) 0.9574(6) 0.0406(3) 0.080(3) Uani 1 1 d . . . H70 H 1.6070 0.9914 0.0619 0.096 Uiso 1 1 calc R . . C71 C 0.7241(7) 1.0817(5) 0.2629(3) 0.099(3) Uani 1 1 d . . . H71 H 0.7355 1.0704 0.2897 0.119 Uiso 1 1 calc R . . C72 C 0.8060(7) 0.8239(7) 0.5966(4) 0.089(3) Uani 1 1 d . . . C73 C 1.8112(7) 1.0255(7) 0.0264(3) 0.112(4) Uani 1 1 d . . . H73 H 1.7825 1.0337 0.0489 0.134 Uiso 1 1 calc R . . C74 C 1.9053(7) 0.4572(6) 0.0240(3) 0.098(3) Uani 1 1 d . . . H74 H 1.9370 0.4372 0.0470 0.117 Uiso 1 1 calc R . . C75 C 0.9370(7) 1.0778(6) 0.1528(3) 0.102(3) Uani 1 1 d . . . H75 H 0.9578 1.1297 0.1581 0.123 Uiso 1 1 calc R . . C77 C 0.9997(6) 0.8193(6) 0.0981(3) 0.110(4) Uani 1 1 d . . . H77 H 0.9378 0.8161 0.0903 0.132 Uiso 1 1 calc R . . C78 C 0.4065(6) 1.2403(5) 0.2672(3) 0.078(3) Uani 1 1 d . . . H78 H 0.4080 1.2364 0.2945 0.093 Uiso 1 1 calc R . . C79 C 1.9061(7) 1.0158(7) 0.0308(3) 0.117(4) Uani 1 1 d . . . H79 H 1.9386 1.0161 0.0557 0.141 Uiso 1 1 calc R . . C80 C 0.9066(9) 0.9245(7) 0.6915(4) 0.123(4) Uani 1 1 d . . . H80 H 0.9629 0.9419 0.7030 0.147 Uiso 1 1 calc R . . C81 C 0.7629(8) 0.9509(9) 0.8081(5) 0.125(5) Uani 1 1 d . . . H81 H 0.7317 0.9993 0.8060 0.151 Uiso 1 1 calc R . . C82 C 1.8986(6) 1.0034(7) -0.0365(4) 0.117(4) Uani 1 1 d . . . H82 H 1.9272 0.9957 -0.0591 0.141 Uiso 1 1 calc R . . C83 C 1.7607(6) 0.4781(5) -0.0143(3) 0.080(3) Uani 1 1 d . . . C84 C 0.3786(7) 1.2859(7) 0.2082(4) 0.098(3) Uani 1 1 d . . . H84 H 0.3598 1.3188 0.1869 0.118 Uiso 1 1 calc R . . C86 C 0.2168(6) 0.8251(6) 0.2975(3) 0.101(3) Uani 1 1 d . . . H86 H 0.2490 0.8337 0.3221 0.121 Uiso 1 1 calc R . . C87 C 0.7533(6) 0.7571(7) 0.5872(4) 0.094(3) Uani 1 1 d . . . H87 H 0.7207 0.7346 0.6061 0.112 Uiso 1 1 calc R . . C88 C 0.7499(8) 0.9076(7) 0.6933(5) 0.124(4) Uani 1 1 d . . . H88 H 0.6983 0.9149 0.7060 0.148 Uiso 1 1 calc R . . C89 C 0.8440(10) 0.9752(7) 0.7504(5) 0.155(5) Uani 1 1 d . . . H89A H 0.9068 0.9909 0.7569 0.187 Uiso 1 1 calc R . . H89B H 0.8081 1.0238 0.7480 0.187 Uiso 1 1 calc R . . C90 C 1.9487(5) 1.0061(5) -0.0013(4) 0.078(3) Uani 1 1 d . . . C91 C 1.8116(7) 0.4478(5) 0.0177(3) 0.094(3) Uani 1 1 d . . . H91 H 1.7828 0.4196 0.0362 0.113 Uiso 1 1 calc R . . C92 C 0.7428(9) 0.8699(7) 0.6563(4) 0.115(4) Uani 1 1 d . . . H92 H 0.6865 0.8504 0.6459 0.138 Uiso 1 1 calc R . . C93 C 1.8048(7) 1.0116(7) -0.0401(4) 0.118(4) Uani 1 1 d . . . H93 H 1.7717 1.0091 -0.0649 0.142 Uiso 1 1 calc R . . C94 C 1.6125(6) 0.5542(6) 0.0376(3) 0.085(3) Uani 1 1 d . . . H94 H 1.6355 0.5211 0.0583 0.102 Uiso 1 1 calc R . . C95 C 1.8055(7) 0.5141(7) -0.0417(3) 0.115(4) Uani 1 1 d . . . H95 H 1.7736 0.5344 -0.0646 0.138 Uiso 1 1 calc R . . C96 C 1.8985(6) 0.5210(7) -0.0360(3) 0.102(3) Uani 1 1 d . . . H96 H 1.9273 0.5447 -0.0558 0.123 Uiso 1 1 calc R . . N13 N 0.9344(18) 0.7804(14) 0.4119(6) 0.209(9) Uani 1 1 d . . . C100 C 0.2156(7) 1.3523(6) 0.2562(4) 0.090(3) Uani 1 1 d . . . C102 C 0.7968(7) 0.7542(7) 0.5234(4) 0.095(3) Uani 1 1 d . . . C103 C 1.0562(6) 0.7583(6) 0.0868(4) 0.118(4) Uani 1 1 d . . . H103 H 1.0316 0.7137 0.0733 0.142 Uiso 1 1 calc R . . C105 C 0.8487(8) 0.8558(7) 0.7939(5) 0.129(5) Uani 1 1 d . . . H105 H 0.8888 0.8234 0.7821 0.154 Uiso 1 1 calc R . . C106 C 0.7869(9) 0.7148(8) 0.4832(5) 0.138(5) Uani 1 1 d . . . H10A H 0.7856 0.6572 0.4868 0.166 Uiso 1 1 calc R . . H10B H 0.7291 0.7305 0.4693 0.166 Uiso 1 1 calc R . . C110 C 0.942(2) 0.7116(10) 0.4642(6) 0.172(8) Uani 1 1 d . . . H110 H 0.9651 0.6789 0.4850 0.206 Uiso 1 1 calc R . . C112 C 0.8550(17) 0.7785(12) 0.4269(7) 0.173(8) Uani 1 1 d . . . H112 H 0.8036 0.8057 0.4160 0.207 Uiso 1 1 calc R . . C117 C 0.1626(7) 1.3826(6) 0.2253(4) 0.115(4) Uani 1 1 d . . . H117 H 0.1893 1.4125 0.2067 0.138 Uiso 1 1 calc R . . C202 C 0.8074(12) 0.8412(11) 0.8265(5) 0.160(7) Uani 1 1 d . . . H202 H 0.8154 0.7935 0.8406 0.192 Uiso 1 1 calc R . . N1 N 0.6396(5) 1.0960(4) 0.2429(2) 0.0672(19) Uani 1 1 d . . . N2 N 0.7421(5) 1.1050(4) 0.2024(3) 0.075(2) Uani 1 1 d . . . N3 N 1.2529(5) 0.7264(4) 0.0481(3) 0.076(2) Uani 1 1 d . . . N4 N 1.3591(4) 0.7489(3) 0.0096(2) 0.0619(17) Uani 1 1 d . . . N5 N 0.4450(4) 1.1879(4) 0.2446(2) 0.0662(18) Uani 1 1 d . . . N6 N 0.3656(4) 1.2988(4) 0.2454(3) 0.082(2) Uani 1 1 d . . . N7 N 0.4657(4) 0.9905(4) 0.2498(2) 0.071(2) Uani 1 1 d . . . N8 N 0.4061(4) 0.8720(4) 0.2545(3) 0.0665(19) Uani 1 1 d . . . N9 N 1.5469(4) 0.6549(4) 0.0035(2) 0.0627(18) Uani 1 1 d . . . N10 N 1.6164(4) 0.5419(4) -0.0012(3) 0.0654(18) Uani 1 1 d . . . N11 N 1.5399(4) 0.8540(4) 0.0049(2) 0.0592(17) Uani 1 1 d . . . N12 N 1.6107(4) 0.9681(4) 0.0032(3) 0.077(2) Uani 1 1 d . . . C98 C 0.9903(14) 0.7398(16) 0.4374(10) 0.188(11) Uani 1 1 d . . . H98 H 1.0521 0.7326 0.4366 0.226 Uiso 1 1 calc R . . N14 N 0.8576(10) 0.7340(8) 0.4589(5) 0.127(4) Uani 1 1 d . . . N15 N 0.8171(6) 0.9294(6) 0.7826(3) 0.091(2) Uani 1 1 d . . . N16 N 0.7547(11) 0.9000(14) 0.8370(5) 0.204(9) Uani 1 1 d . . . O11 O 0.5064(4) 1.1011(3) 0.32238(16) 0.145(3) Uani 1 1 d D . . O12 O 0.6165(4) 1.2012(4) 0.32831(18) 0.162(3) Uani 1 1 d D . . O13 O 0.6149(4) 1.1033(4) 0.37760(17) 0.175(4) Uani 1 1 d D . . O14 O 0.5020(4) 1.2014(4) 0.36997(19) 0.183(4) Uani 1 1 d D . . S1 S 0.5606(2) 1.15180(18) 0.34974(8) 0.1034(9) Uani 1 1 d D . . Zn1 Zn 0.52108(6) 1.09706(6) 0.26589(3) 0.0702(3) Uani 1 1 d . . . Zn2 Zn 1.47674(6) 0.75282(5) -0.01277(3) 0.0613(3) Uani 1 1 d . A . O21 O 1.4668(6) 0.7437(4) -0.0684(2) 0.221(3) Uiso 1 1 d D . . O23 O 1.5019(5) 0.8228(6) -0.1215(2) 0.221(3) Uiso 1 1 d D . . S2A S 1.4324(2) 0.7950(2) -0.09983(9) 0.1113(14) Uani 0.863(4) 1 d PD A 1 O22A O 1.3658(5) 0.7527(5) -0.1257(2) 0.221(3) Uiso 0.863(4) 1 d PD A 1 O24A O 1.3936(7) 0.8653(4) -0.0851(3) 0.221(3) Uiso 0.863(4) 1 d PD A 1 S2B S 1.5380(6) 0.7760(9) -0.0885(4) 0.131(9) Uiso 0.137(4) 1 d PD A 2 O24B O 1.591(2) 0.831(2) -0.0636(8) 0.221(3) Uiso 0.137(4) 1 d PD A 2 O22B O 1.5933(19) 0.7133(16) -0.1007(9) 0.221(3) Uiso 0.137(4) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C7 0.075(6) 0.073(7) 0.096(8) -0.004(6) 0.012(6) -0.006(5) C16 0.055(5) 0.076(6) 0.079(6) -0.006(5) 0.023(5) 0.009(5) C17 0.042(5) 0.102(8) 0.125(9) -0.024(7) 0.021(6) 0.003(5) C21 0.048(5) 0.078(6) 0.166(10) -0.020(6) 0.039(6) -0.024(5) C22 0.051(5) 0.074(6) 0.066(6) -0.004(5) 0.011(4) 0.013(5) C24 0.099(7) 0.098(8) 0.060(6) -0.022(6) 0.029(5) -0.010(6) C26 0.052(6) 0.065(6) 0.116(9) -0.011(6) 0.013(5) 0.016(4) C27 0.061(6) 0.053(6) 0.147(9) 0.010(6) 0.014(5) 0.004(5) C28 0.049(5) 0.058(5) 0.098(7) 0.016(5) 0.013(6) -0.003(4) C31 0.107(8) 0.083(7) 0.137(9) 0.028(6) 0.075(7) 0.034(6) C32 0.062(6) 0.065(6) 0.090(7) -0.011(5) 0.000(5) 0.025(4) C33 0.066(6) 0.083(7) 0.092(7) 0.004(5) -0.002(6) 0.024(5) C34 0.059(6) 0.053(5) 0.125(8) -0.005(5) 0.015(6) -0.009(5) C35 0.080(8) 0.123(9) 0.126(10) 0.025(8) -0.011(7) -0.029(7) C36 0.058(6) 0.060(6) 0.099(7) -0.005(6) 0.002(5) 0.007(5) C37 0.058(6) 0.081(7) 0.121(8) -0.027(6) 0.019(5) 0.000(5) C38 0.040(5) 0.067(6) 0.077(6) 0.008(6) 0.003(4) 0.020(4) C39 0.089(7) 0.077(7) 0.115(9) 0.018(7) 0.012(7) -0.015(6) C40 0.062(6) 0.122(8) 0.109(8) -0.048(6) 0.009(6) 0.023(6) C41 0.066(6) 0.074(7) 0.120(8) -0.013(6) 0.018(6) 0.006(5) C42 0.031(5) 0.068(6) 0.124(9) 0.026(6) -0.007(6) -0.009(4) C43 0.064(7) 0.091(8) 0.133(11) 0.045(7) 0.010(8) -0.004(6) C44 0.058(6) 0.122(9) 0.073(7) -0.001(6) 0.002(5) 0.017(6) C45 0.051(6) 0.112(8) 0.114(8) -0.012(7) -0.004(6) 0.003(6) C46 0.049(5) 0.059(5) 0.104(8) 0.013(5) 0.013(6) -0.003(4) C47 0.055(5) 0.063(6) 0.080(6) -0.004(6) 0.005(5) -0.001(5) C48 0.063(6) 0.076(6) 0.087(7) 0.002(6) 0.009(5) 0.003(5) C49 0.116(9) 0.060(7) 0.123(10) 0.017(7) -0.007(7) -0.019(6) C50 0.060(6) 0.170(12) 0.109(9) -0.030(8) 0.009(6) 0.026(7) C52 0.057(5) 0.068(6) 0.099(7) -0.004(5) 0.000(7) 0.026(5) C53 0.106(8) 0.068(6) 0.152(10) 0.003(6) 0.066(7) 0.028(6) C54 0.050(6) 0.098(8) 0.153(10) 0.023(7) -0.007(6) 0.003(5) C55 0.063(7) 0.084(8) 0.157(12) 0.023(9) -0.005(8) -0.011(5) C56 0.054(6) 0.090(7) 0.104(8) -0.011(6) 0.005(5) -0.018(5) C58 0.067(6) 0.080(7) 0.168(10) -0.020(7) 0.046(6) 0.012(6) C59 0.048(6) 0.130(9) 0.095(8) 0.006(6) 0.014(5) -0.011(5) C60 0.047(6) 0.105(8) 0.156(11) 0.002(8) 0.024(7) 0.017(5) C61 0.069(7) 0.089(7) 0.104(8) 0.011(6) 0.041(6) 0.028(6) C62 0.059(6) 0.054(5) 0.154(9) -0.029(6) -0.003(6) 0.015(4) C63 0.068(6) 0.087(7) 0.098(8) 0.006(6) 0.025(6) -0.004(5) C65 0.044(5) 0.055(5) 0.192(11) 0.028(6) -0.001(6) -0.001(4) C66 0.090(9) 0.110(9) 0.138(11) -0.002(8) -0.008(7) 0.024(7) C67 0.044(5) 0.087(7) 0.088(8) -0.011(6) 0.005(5) 0.008(5) C68 0.033(5) 0.090(7) 0.252(14) -0.043(8) 0.010(6) 0.008(5) C69 0.138(12) 0.059(6) 0.123(11) 0.000(7) 0.018(9) -0.021(7) C70 0.046(5) 0.097(8) 0.095(8) -0.034(7) 0.003(5) 0.001(5) C71 0.060(6) 0.088(7) 0.150(10) -0.006(6) 0.018(7) 0.014(5) C72 0.083(7) 0.082(7) 0.096(9) 0.022(7) -0.018(7) 0.005(6) C73 0.059(7) 0.151(10) 0.122(10) -0.014(8) -0.007(7) -0.013(6) C74 0.074(8) 0.074(7) 0.143(10) 0.015(7) 0.003(7) 0.023(6) C75 0.082(7) 0.089(7) 0.142(9) -0.041(6) 0.040(7) -0.012(6) C77 0.053(6) 0.105(8) 0.178(11) -0.052(8) 0.033(6) 0.000(6) C78 0.059(5) 0.059(6) 0.115(8) -0.012(6) 0.013(5) 0.000(5) C79 0.058(7) 0.188(12) 0.103(9) 0.004(8) -0.005(6) -0.018(7) C80 0.119(11) 0.122(10) 0.123(11) 0.027(9) -0.006(9) -0.039(8) C81 0.053(7) 0.146(13) 0.175(15) -0.069(11) 0.002(8) -0.003(8) C82 0.038(6) 0.181(12) 0.129(10) 0.040(8) -0.003(6) 0.000(6) C83 0.075(7) 0.053(6) 0.112(9) -0.020(5) 0.013(7) 0.031(5) C84 0.067(7) 0.118(9) 0.106(9) 0.034(8) -0.004(7) 0.004(6) C86 0.058(6) 0.125(9) 0.113(9) 0.014(7) -0.022(6) -0.016(6) C87 0.048(6) 0.093(8) 0.139(11) 0.014(8) 0.007(6) -0.002(6) C88 0.097(9) 0.092(8) 0.184(14) 0.008(9) 0.023(9) -0.021(7) C89 0.221(16) 0.083(9) 0.166(14) -0.004(10) 0.038(12) -0.027(9) C90 0.048(5) 0.067(6) 0.115(8) 0.021(6) -0.008(7) -0.007(5) C91 0.082(8) 0.064(6) 0.140(9) 0.024(6) 0.031(7) 0.023(6) C92 0.139(12) 0.084(8) 0.123(10) 0.001(7) 0.011(9) -0.019(7) C93 0.059(7) 0.162(11) 0.129(10) 0.043(8) -0.013(7) -0.001(7) C94 0.073(6) 0.084(7) 0.101(9) 0.015(6) 0.021(6) 0.015(5) C95 0.071(8) 0.179(12) 0.091(8) 0.016(8) -0.011(6) 0.045(8) C96 0.055(6) 0.162(10) 0.091(8) 0.000(7) 0.014(6) 0.018(6) N13 0.172(18) 0.30(2) 0.168(16) -0.078(15) 0.069(14) -0.056(16) C100 0.081(8) 0.050(6) 0.136(10) -0.010(6) 0.001(7) 0.011(5) C102 0.072(7) 0.089(8) 0.121(10) -0.006(8) -0.001(7) 0.006(6) C103 0.050(6) 0.112(9) 0.199(12) -0.045(8) 0.037(7) 0.008(6) C105 0.119(10) 0.067(8) 0.192(15) -0.002(9) -0.014(10) 0.007(7) C106 0.107(10) 0.124(10) 0.188(15) 0.005(10) 0.030(10) -0.043(8) C110 0.17(2) 0.115(12) 0.24(2) -0.043(12) 0.06(2) -0.021(14) C112 0.22(3) 0.148(15) 0.137(16) -0.013(12) -0.039(15) 0.042(14) C117 0.062(7) 0.086(8) 0.197(13) 0.035(8) 0.010(7) -0.009(6) C202 0.158(17) 0.201(19) 0.123(13) 0.007(13) 0.024(11) -0.086(14) N1 0.068(5) 0.053(4) 0.086(5) -0.006(4) 0.034(5) 0.003(4) N2 0.059(5) 0.060(4) 0.113(7) -0.006(4) 0.037(5) 0.009(4) N3 0.054(5) 0.066(5) 0.111(7) 0.009(4) 0.022(5) 0.013(4) N4 0.057(4) 0.051(4) 0.078(5) 0.006(4) 0.010(4) 0.015(3) N5 0.040(4) 0.066(5) 0.095(6) 0.000(4) 0.017(4) 0.003(3) N6 0.033(4) 0.061(5) 0.149(8) -0.001(6) -0.001(5) -0.002(4) N7 0.054(4) 0.048(4) 0.116(7) 0.011(5) 0.027(4) -0.008(3) N8 0.039(4) 0.056(5) 0.105(6) 0.011(5) 0.010(4) 0.003(3) N9 0.042(4) 0.072(5) 0.076(5) 0.001(4) 0.013(4) 0.010(3) N10 0.046(4) 0.051(4) 0.096(6) -0.002(4) -0.001(4) 0.007(3) N11 0.041(4) 0.065(4) 0.071(5) -0.003(4) 0.003(3) 0.003(3) N12 0.031(4) 0.067(5) 0.130(8) -0.008(5) 0.001(4) 0.002(4) C98 0.114(15) 0.21(2) 0.24(3) -0.14(2) 0.022(17) -0.032(15) N14 0.089(9) 0.112(9) 0.176(13) -0.032(9) -0.012(9) 0.005(7) N15 0.079(6) 0.082(7) 0.108(7) 0.002(6) -0.003(5) -0.011(5) N16 0.141(13) 0.30(2) 0.186(15) -0.076(15) 0.077(11) -0.123(14) O11 0.203(8) 0.114(6) 0.107(6) 0.003(5) -0.031(5) -0.035(6) O12 0.133(7) 0.208(9) 0.147(7) 0.052(7) 0.021(5) -0.041(6) O13 0.237(10) 0.133(7) 0.136(7) 0.032(6) -0.063(7) -0.005(7) O14 0.182(9) 0.221(10) 0.154(8) -0.056(7) 0.049(6) 0.032(8) S1 0.107(2) 0.115(2) 0.086(2) -0.0080(19) 0.0023(18) -0.0097(19) Zn1 0.0583(6) 0.0641(6) 0.0898(8) -0.0035(6) 0.0155(5) -0.0024(5) Zn2 0.0483(5) 0.0601(6) 0.0762(7) -0.0030(5) 0.0097(4) 0.0049(4) S2A 0.120(3) 0.123(3) 0.088(2) -0.002(2) -0.002(2) -0.009(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 C7 N8 1.354(10) . ? C7 C24 1.363(11) . ? C7 H7 0.9300 . ? C16 C40 1.334(10) . ? C16 C77 1.347(11) . ? C16 C22 1.516(10) . ? C17 N3 1.295(11) . ? C17 C33 1.364(11) . ? C17 H17 0.9300 . ? C21 C22 1.367(10) . ? C21 C58 1.392(11) . ? C21 H21 0.9300 . ? C22 C37 1.356(11) . ? C24 N7 1.346(9) . ? C24 H24 0.9300 . ? C26 N1 1.297(10) . ? C26 N2 1.325(9) . ? C26 H26 0.9300 . ? C27 N8 1.453(9) . ? C27 C28 1.510(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C63 1.380(11) . ? C28 C86 1.396(12) . ? C31 N3 1.480(10) . ? C31 C61 1.531(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N4 1.301(9) . ? C32 N3 1.343(9) . ? C32 H32 0.9300 . ? C33 N4 1.391(9) . ? C33 H33 0.9300 . ? C34 C45 1.375(11) . ? C34 C54 1.413(12) 2_545 ? C34 C46 1.469(11) . ? C35 C80 1.401(15) . ? C35 C43 1.453(13) . ? C35 H35 0.9300 . ? C36 N8 1.320(9) . ? C36 N7 1.336(9) . ? C36 H36 0.9300 . ? C37 C75 1.398(11) . ? C37 H37 0.9300 . ? C38 N12 1.320(9) . ? C38 N11 1.336(9) . ? C38 H38 0.9300 . ? C39 C49 1.379(12) . ? C39 C72 1.403(12) . ? C39 H39 0.9300 . ? C40 C50 1.381(12) . ? C40 H40 0.9300 . ? C41 C58 1.362(11) . ? C41 C75 1.367(11) . ? C41 C53 1.511(11) . ? C42 C73 1.308(12) . ? C42 C93 1.350(13) . ? C42 C65 1.542(10) . ? C43 C92 1.369(13) . ? C43 C72 1.433(14) . ? C44 N5 1.358(10) . ? C44 C84 1.403(13) . ? C44 H44 0.9300 . ? C45 C66 1.449(13) 2_545 ? C45 H45 0.9300 . ? C46 C59 1.363(11) . ? C46 C56 1.363(11) . ? C47 N9 1.300(9) . ? C47 N10 1.304(9) . ? C47 H47 0.9300 . ? C48 C94 1.347(11) . ? C48 N9 1.365(9) . ? C48 H48 0.9300 . ? C49 C102 1.367(13) . ? C49 H49 0.9300 . ? C50 C61 1.350(12) . ? C50 H50 0.9300 . ? C52 C74 1.358(12) . ? C52 C96 1.367(11) . ? C52 C52 1.460(16) 3_965 ? C53 N2 1.487(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C117 1.376(12) . ? C54 C34 1.413(12) 2 ? C54 H54 0.9300 . ? C55 C87 1.344(13) . ? C55 C102 1.352(13) . ? C55 H55 0.9300 . ? C56 C63 1.380(11) . ? C56 H56 0.9300 . ? C58 H58 0.9300 . ? C59 C86 1.406(11) . ? C59 H59 0.9300 . ? C60 C71 1.333(12) . ? C60 N2 1.350(11) . ? C60 H60 0.9300 . ? C61 C103 1.343(12) . ? C62 N10 1.471(9) . ? C62 C83 1.521(11) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63 0.9300 . ? C65 N12 1.469(10) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C100 1.346(13) . ? C66 C45 1.449(13) 2 ? C66 H66 0.9300 . ? C67 C70 1.327(11) . ? C67 N11 1.347(9) . ? C67 H67 0.9300 . ? C68 N6 1.460(11) . ? C68 C100 1.539(12) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C80 1.338(14) . ? C69 C88 1.423(15) . ? C69 C89 1.477(15) . ? C70 N12 1.348(10) . ? C70 H70 0.9300 . ? C71 N1 1.381(11) . ? C71 H71 0.9300 . ? C72 C87 1.381(13) . ? C73 C79 1.410(12) . ? C73 H73 0.9300 . ? C74 C91 1.394(12) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C77 C103 1.400(11) . ? C77 H77 0.9300 . ? C78 N6 1.334(10) . ? C78 N5 1.336(9) . ? C78 H78 0.9300 . ? C79 C90 1.334(12) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? C81 N15 1.300(14) . ? C81 N16 1.32(2) . ? C81 C202 2.02(3) . ? C81 H81 0.9300 . ? C82 C90 1.341(12) . ? C82 C93 1.392(12) . ? C82 H82 0.9300 . ? C83 C95 1.350(12) . ? C83 C91 1.353(12) . ? C84 N6 1.321(11) . ? C84 H84 0.9300 . ? C86 H86 0.9300 . ? C87 H87 0.9300 . ? C88 C92 1.404(14) . ? C88 H88 0.9300 . ? C89 N15 1.432(13) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C90 1.530(16) 3_975 ? C91 H91 0.9300 . ? C92 H92 0.9300 . ? C93 H93 0.9300 . ? C94 N10 1.347(10) . ? C94 H94 0.9300 . ? C95 C96 1.378(12) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? N13 C98 1.32(3) . ? N13 C112 1.34(2) . ? C100 C117 1.342(13) . ? C102 C106 1.511(15) . ? C103 H103 0.9300 . ? C105 C202 1.352(17) . ? C105 N15 1.356(12) . ? C105 H105 0.9300 . ? C106 N14 1.447(15) . ? C106 H10A 0.9700 . ? C106 H10B 0.9700 . ? C110 N14 1.30(2) . ? C110 C98 1.32(3) . ? C110 C112 2.04(3) . ? C110 H110 0.9300 . ? C112 N14 1.32(2) . ? C112 H112 0.9300 . ? C117 H117 0.9300 . ? C202 N16 1.33(2) . ? C202 H202 0.9300 . ? N1 Zn1 2.008(6) . ? N4 Zn2 1.986(6) . ? N5 Zn1 1.980(7) . ? N7 Zn1 2.011(7) . ? N9 Zn2 1.984(6) . ? N11 Zn2 1.992(6) . ? C98 H98 0.9300 . ? O11 S1 1.438(4) . ? O11 Zn1 1.965(6) . ? O12 S1 1.428(4) . ? O13 S1 1.427(4) . ? O14 S1 1.433(4) . ? Zn2 O21 1.894(7) . ? O21 S2A 1.421(4) . ? O21 S2B 1.428(5) . ? O23 S2A 1.414(4) . ? O23 S2B 1.425(5) . ? S2A O24A 1.423(5) . ? S2A O22A 1.434(4) . ? S2B O24B 1.423(5) . ? S2B O22B 1.423(5) . ? 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 N8 C7 C24 106.4(8) . . ? N8 C7 H7 126.8 . . ? C24 C7 H7 126.8 . . ? C40 C16 C77 117.7(8) . . ? C40 C16 C22 122.7(8) . . ? C77 C16 C22 119.5(8) . . ? N3 C17 C33 108.9(8) . . ? N3 C17 H17 125.6 . . ? C33 C17 H17 125.6 . . ? C22 C21 C58 123.0(9) . . ? C22 C21 H21 118.5 . . ? C58 C21 H21 118.5 . . ? C37 C22 C21 117.8(8) . . ? C37 C22 C16 119.1(8) . . ? C21 C22 C16 123.1(8) . . ? N7 C24 C7 108.9(8) . . ? N7 C24 H24 125.5 . . ? C7 C24 H24 125.5 . . ? N1 C26 N2 112.0(9) . . ? N1 C26 H26 124.0 . . ? N2 C26 H26 124.0 . . ? N8 C27 C28 112.3(6) . . ? N8 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N8 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C63 C28 C86 117.1(8) . . ? C63 C28 C27 122.5(9) . . ? C86 C28 C27 120.3(9) . . ? N3 C31 C61 110.9(7) . . ? N3 C31 H31A 109.5 . . ? C61 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? C61 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N4 C32 N3 112.4(8) . . ? N4 C32 H32 123.8 . . ? N3 C32 H32 123.8 . . ? C17 C33 N4 107.2(8) . . ? C17 C33 H33 126.4 . . ? N4 C33 H33 126.4 . . ? C45 C34 C54 118.4(9) . 2_545 ? C45 C34 C46 122.1(9) . . ? C54 C34 C46 119.5(9) 2_545 . ? C80 C35 C43 120.6(12) . . ? C80 C35 H35 119.7 . . ? C43 C35 H35 119.7 . . ? N8 C36 N7 110.5(8) . . ? N8 C36 H36 124.8 . . ? N7 C36 H36 124.8 . . ? C22 C37 C75 120.7(8) . . ? C22 C37 H37 119.6 . . ? C75 C37 H37 119.6 . . ? N12 C38 N11 110.3(8) . . ? N12 C38 H38 124.9 . . ? N11 C38 H38 124.9 . . ? C49 C39 C72 121.6(10) . . ? C49 C39 H39 119.2 . . ? C72 C39 H39 119.2 . . ? C16 C40 C50 120.5(9) . . ? C16 C40 H40 119.8 . . ? C50 C40 H40 119.8 . . ? C58 C41 C75 120.6(9) . . ? C58 C41 C53 119.3(9) . . ? C75 C41 C53 119.9(9) . . ? C73 C42 C93 117.5(9) . . ? C73 C42 C65 122.8(11) . . ? C93 C42 C65 119.7(10) . . ? C92 C43 C72 122.7(11) . . ? C92 C43 C35 115.0(13) . . ? C72 C43 C35 122.3(12) . . ? N5 C44 C84 106.8(9) . . ? N5 C44 H44 126.6 . . ? C84 C44 H44 126.6 . . ? C34 C45 C66 118.3(10) . 2_545 ? C34 C45 H45 120.9 . . ? C66 C45 H45 120.9 2_545 . ? C59 C46 C56 117.6(8) . . ? C59 C46 C34 122.3(9) . . ? C56 C46 C34 120.1(10) . . ? N9 C47 N10 112.5(8) . . ? N9 C47 H47 123.8 . . ? N10 C47 H47 123.8 . . ? C94 C48 N9 109.0(9) . . ? C94 C48 H48 125.5 . . ? N9 C48 H48 125.5 . . ? C102 C49 C39 117.6(11) . . ? C102 C49 H49 121.2 . . ? C39 C49 H49 121.2 . . ? C61 C50 C40 122.3(9) . . ? C61 C50 H50 118.8 . . ? C40 C50 H50 118.8 . . ? C74 C52 C96 115.1(9) . . ? C74 C52 C52 121.9(13) . 3_965 ? C96 C52 C52 123.0(13) . 3_965 ? N2 C53 C41 112.0(8) . . ? N2 C53 H53A 109.2 . . ? C41 C53 H53A 109.2 . . ? N2 C53 H53B 109.2 . . ? C41 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C117 C54 C34 120.2(10) . 2 ? C117 C54 H54 119.9 . . ? C34 C54 H54 119.9 2 . ? C87 C55 C102 120.5(11) . . ? C87 C55 H55 119.8 . . ? C102 C55 H55 119.8 . . ? C46 C56 C63 121.1(9) . . ? C46 C56 H56 119.4 . . ? C63 C56 H56 119.4 . . ? C41 C58 C21 117.8(9) . . ? C41 C58 H58 121.1 . . ? C21 C58 H58 121.1 . . ? C46 C59 C86 122.7(9) . . ? C46 C59 H59 118.7 . . ? C86 C59 H59 118.7 . . ? C71 C60 N2 106.4(9) . . ? C71 C60 H60 126.8 . . ? N2 C60 H60 126.8 . . ? C103 C61 C50 117.7(9) . . ? C103 C61 C31 120.1(10) . . ? C50 C61 C31 122.2(10) . . ? N10 C62 C83 111.9(6) . . ? N10 C62 H62A 109.2 . . ? C83 C62 H62A 109.2 . . ? N10 C62 H62B 109.2 . . ? C83 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? C28 C63 C56 122.3(9) . . ? C28 C63 H63 118.9 . . ? C56 C63 H63 118.9 . . ? N12 C65 C42 111.9(6) . . ? N12 C65 H65A 109.2 . . ? C42 C65 H65A 109.2 . . ? N12 C65 H65B 109.2 . . ? C42 C65 H65B 109.2 . . ? H65A C65 H65B 107.9 . . ? C100 C66 C45 121.8(11) . 2 ? C100 C66 H66 119.1 . . ? C45 C66 H66 119.1 2 . ? C70 C67 N11 110.9(9) . . ? C70 C67 H67 124.5 . . ? N11 C67 H67 124.5 . . ? N6 C68 C100 110.7(7) . . ? N6 C68 H68A 109.5 . . ? C100 C68 H68A 109.5 . . ? N6 C68 H68B 109.5 . . ? C100 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? C80 C69 C88 116.8(13) . . ? C80 C69 C89 121.5(14) . . ? C88 C69 C89 121.6(15) . . ? C67 C70 N12 106.0(8) . . ? C67 C70 H70 127.0 . . ? N12 C70 H70 127.0 . . ? C60 C71 N1 109.4(10) . . ? C60 C71 H71 125.3 . . ? N1 C71 H71 125.3 . . ? C87 C72 C39 117.1(11) . . ? C87 C72 C43 123.2(12) . . ? C39 C72 C43 119.7(11) . . ? C42 C73 C79 123.1(10) . . ? C42 C73 H73 118.5 . . ? C79 C73 H73 118.5 . . ? C52 C74 C91 120.8(10) . . ? C52 C74 H74 119.6 . . ? C91 C74 H74 119.6 . . ? C41 C75 C37 120.0(9) . . ? C41 C75 H75 120.0 . . ? C37 C75 H75 120.0 . . ? C16 C77 C103 122.1(9) . . ? C16 C77 H77 118.9 . . ? C103 C77 H77 118.9 . . ? N6 C78 N5 110.7(9) . . ? N6 C78 H78 124.6 . . ? N5 C78 H78 124.6 . . ? C90 C79 C73 119.3(10) . . ? C90 C79 H79 120.4 . . ? C73 C79 H79 120.4 . . ? C69 C80 C35 123.5(12) . . ? C69 C80 H80 118.2 . . ? C35 C80 H80 118.2 . . ? N15 C81 N16 116.1(16) . . ? N15 C81 C202 75.7(9) . . ? N16 C81 C202 40.4(9) . . ? N15 C81 H81 122.0 . . ? N16 C81 H81 122.0 . . ? C202 C81 H81 162.3 . . ? C90 C82 C93 121.8(11) . . ? C90 C82 H82 119.1 . . ? C93 C82 H82 119.1 . . ? C95 C83 C91 116.8(9) . . ? C95 C83 C62 121.7(10) . . ? C91 C83 C62 121.5(10) . . ? N6 C84 C44 107.6(9) . . ? N6 C84 H84 126.2 . . ? C44 C84 H84 126.2 . . ? C28 C86 C59 119.1(9) . . ? C28 C86 H86 120.5 . . ? C59 C86 H86 120.5 . . ? C55 C87 C72 121.3(11) . . ? C55 C87 H87 119.3 . . ? C72 C87 H87 119.3 . . ? C92 C88 C69 120.8(12) . . ? C92 C88 H88 119.6 . . ? C69 C88 H88 119.6 . . ? N15 C89 C69 116.0(10) . . ? N15 C89 H89A 108.3 . . ? C69 C89 H89A 108.3 . . ? N15 C89 H89B 108.3 . . ? C69 C89 H89B 108.3 . . ? H89A C89 H89B 107.4 . . ? C79 C90 C82 118.1(9) . . ? C79 C90 C90 122.0(13) . 3_975 ? C82 C90 C90 119.8(13) . 3_975 ? C83 C91 C74 122.8(10) . . ? C83 C91 H91 118.6 . . ? C74 C91 H91 118.6 . . ? C43 C92 C88 123.2(13) . . ? C43 C92 H92 118.4 . . ? C88 C92 H92 118.4 . . ? C42 C93 C82 120.2(10) . . ? C42 C93 H93 119.9 . . ? C82 C93 H93 119.9 . . ? C48 C94 N10 106.0(9) . . ? C48 C94 H94 127.0 . . ? N10 C94 H94 127.0 . . ? C83 C95 C96 120.2(10) . . ? C83 C95 H95 119.9 . . ? C96 C95 H95 119.9 . . ? C52 C96 C95 124.1(10) . . ? C52 C96 H96 117.9 . . ? C95 C96 H96 117.9 . . ? C98 N13 C112 104(2) . . ? C117 C100 C66 118.8(11) . . ? C117 C100 C68 122.3(11) . . ? C66 C100 C68 118.9(11) . . ? C55 C102 C49 121.9(12) . . ? C55 C102 C106 117.8(12) . . ? C49 C102 C106 120.2(12) . . ? C61 C103 C77 119.5(10) . . ? C61 C103 H103 120.3 . . ? C77 C103 H103 120.3 . . ? C202 C105 N15 102.9(14) . . ? C202 C105 H105 128.6 . . ? N15 C105 H105 128.6 . . ? N14 C106 C102 114.8(10) . . ? N14 C106 H10A 108.6 . . ? C102 C106 H10A 108.6 . . ? N14 C106 H10B 108.6 . . ? C102 C106 H10B 108.6 . . ? H10A C106 H10B 107.5 . . ? N14 C110 C98 113(3) . . ? N14 C110 C112 39.1(13) . . ? C98 C110 C112 74.2(16) . . ? N14 C110 H110 123.4 . . ? C98 C110 H110 123.4 . . ? C112 C110 H110 162.5 . . ? N14 C112 N13 112.8(19) . . ? N14 C112 C110 38.4(9) . . ? N13 C112 C110 74.4(13) . . ? N14 C112 H112 123.6 . . ? N13 C112 H112 123.6 . . ? C110 C112 H112 161.9 . . ? C100 C117 C54 122.6(11) . . ? C100 C117 H117 118.7 . . ? C54 C117 H117 118.7 . . ? N16 C202 C105 115(2) . . ? N16 C202 C81 40.0(11) . . ? C105 C202 C81 75.1(11) . . ? N16 C202 H202 122.5 . . ? C105 C202 H202 122.5 . . ? C81 C202 H202 162.4 . . ? C26 N1 C71 104.8(8) . . ? C26 N1 Zn1 128.6(7) . . ? C71 N1 Zn1 126.6(7) . . ? C26 N2 C60 107.4(8) . . ? C26 N2 C53 125.8(9) . . ? C60 N2 C53 126.5(9) . . ? C17 N3 C32 107.0(8) . . ? C17 N3 C31 125.8(9) . . ? C32 N3 C31 126.9(9) . . ? C32 N4 C33 104.5(7) . . ? C32 N4 Zn2 129.3(6) . . ? C33 N4 Zn2 125.9(6) . . ? C78 N5 C44 106.6(8) . . ? C78 N5 Zn1 123.6(7) . . ? C44 N5 Zn1 129.6(7) . . ? C84 N6 C78 108.1(9) . . ? C84 N6 C68 128.6(11) . . ? C78 N6 C68 123.3(10) . . ? C36 N7 C24 106.3(7) . . ? C36 N7 Zn1 125.6(7) . . ? C24 N7 Zn1 128.0(7) . . ? C36 N8 C7 108.0(7) . . ? C36 N8 C27 128.2(9) . . ? C7 N8 C27 123.8(9) . . ? C47 N9 C48 104.9(7) . . ? C47 N9 Zn2 125.9(7) . . ? C48 N9 Zn2 129.0(6) . . ? C47 N10 C94 107.6(7) . . ? C47 N10 C62 126.4(9) . . ? C94 N10 C62 126.0(8) . . ? C38 N11 C67 104.7(7) . . ? C38 N11 Zn2 126.5(7) . . ? C67 N11 Zn2 128.7(7) . . ? C38 N12 C70 108.1(8) . . ? C38 N12 C65 124.6(10) . . ? C70 N12 C65 127.3(10) . . ? C110 C98 N13 107(2) . . ? C110 C98 H98 126.6 . . ? N13 C98 H98 126.6 . . ? C110 N14 C112 102.5(17) . . ? C110 N14 C106 127.3(19) . . ? C112 N14 C106 130(2) . . ? C81 N15 C105 106.3(12) . . ? C81 N15 C89 127.8(13) . . ? C105 N15 C89 125.7(13) . . ? C81 N16 C202 99.6(15) . . ? S1 O11 Zn1 122.7(4) . . ? O13 S1 O12 110.5(3) . . ? O13 S1 O14 109.6(3) . . ? O12 S1 O14 109.4(3) . . ? O13 S1 O11 109.4(3) . . ? O12 S1 O11 108.9(3) . . ? O14 S1 O11 109.0(3) . . ? O11 Zn1 N5 102.2(3) . . ? O11 Zn1 N1 125.7(3) . . ? N5 Zn1 N1 110.7(3) . . ? O11 Zn1 N7 102.2(3) . . ? N5 Zn1 N7 112.2(3) . . ? N1 Zn1 N7 103.6(3) . . ? O21 Zn2 N9 101.2(3) . . ? O21 Zn2 N4 114.2(3) . . ? N9 Zn2 N4 108.8(3) . . ? O21 Zn2 N11 110.6(3) . . ? N9 Zn2 N11 113.5(2) . . ? N4 Zn2 N11 108.5(3) . . ? S2A O21 S2B 68.6(3) . . ? S2A O21 Zn2 133.5(5) . . ? S2B O21 Zn2 118.1(8) . . ? S2A O23 S2B 68.9(3) . . ? O23 S2A O21 111.6(3) . . ? O23 S2A O24A 105.2(7) . . ? O21 S2A O24A 110.9(3) . . ? O23 S2A O22A 109.5(3) . . ? O21 S2A O22A 109.4(3) . . ? O24A S2A O22A 110.2(3) . . ? O24B S2B O22B 110.5(4) . . ? O24B S2B O23 104.6(14) . . ? O22B S2B O23 110.5(4) . . ? O24B S2B O21 110.3(4) . . ? O22B S2B O21 110.3(4) . . ? O23 S2B O21 110.6(4) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.114 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.094 # * END