# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_110125-2 _database_code_depnum_ccdc_archive 'CCDC 813757' #TrackingRef '110125-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 N3 O9 Pb2 S3' _chemical_formula_weight 822.79 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' 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' Pb Pb -3.3944 10.1111 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.3190(12) _cell_length_b 16.4691(14) _cell_length_c 8.3323(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.735(13) _cell_angle_gamma 90.00 _cell_volume 1750.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3383 _cell_measurement_theta_min 2.4684 _cell_measurement_theta_max 28.6737 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1483 _exptl_absorpt_coefficient_mu 19.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.34179 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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_type 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7332 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0646 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2822 _reflns_number_gt 2104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^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_extinction_coef ? _refine_ls_number_reflns 2822 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.39204(3) 0.45111(2) 0.62531(4) 0.01998(11) Uani 1 1 d . . . Pb2 Pb 0.33418(3) 0.30603(2) 1.04892(4) 0.02072(11) Uani 1 1 d . . . S3 S 0.98568(18) 0.12058(15) 1.0126(3) 0.0265(6) Uani 1 1 d . . . S2 S 0.66680(18) 0.21100(14) 0.5296(3) 0.0237(6) Uani 1 1 d . . . S1 S 0.9013(2) 0.43250(15) 0.9362(3) 0.0310(6) Uani 1 1 d . . . O1 O 0.4932(5) 0.3156(4) 0.6062(9) 0.041(2) Uani 1 1 d . . . O2 O 0.5644(5) 0.4290(3) 0.5577(8) 0.0253(16) Uani 1 1 d . . . O9 O 0.5023(5) 0.5511(4) 0.8187(7) 0.0253(11) Uani 1 1 d . . . O3 O 0.4443(5) 0.4078(4) 0.9208(8) 0.0253(11) Uani 1 1 d . . . O6 O 0.2426(6) 0.5152(4) 0.7472(9) 0.046(2) Uani 1 1 d . . . O8 O 0.7144(6) 0.6107(4) 0.7044(8) 0.0376(18) Uani 1 1 d . . . O7 O 0.7714(5) 0.5730(4) 0.9727(7) 0.0280(16) Uani 1 1 d . . . O5 O 1.2668(4) 0.1871(4) 1.2439(7) 0.0241(16) Uani 1 1 d . . . O4 O 1.1673(5) 0.2374(4) 1.0083(8) 0.0349(18) Uani 1 1 d . . . N1 N 0.7924(6) 0.3201(4) 0.7252(10) 0.0192(18) Uani 1 1 d . . . N2 N 0.8277(6) 0.1792(4) 0.7819(9) 0.0188(18) Uani 1 1 d . . . N3 N 0.9318(6) 0.2776(5) 0.9632(10) 0.0238(19) Uani 1 1 d . . . C7 C 0.5553(7) 0.3536(5) 0.5469(11) 0.020(2) Uani 1 1 d . . . C6 C 0.6162(7) 0.3082(5) 0.4478(11) 0.024(2) Uani 1 1 d . . . H6A H 0.6745 0.3419 0.4408 0.029 Uiso 1 1 calc R . . H6B H 0.5710 0.3006 0.3346 0.029 Uiso 1 1 calc R . . C8 C 0.4843(7) 0.4587(5) 1.0306(11) 0.020(2) Uani 1 1 d . . . C2 C 0.7722(7) 0.2405(5) 0.6931(11) 0.017(2) Uani 1 1 d . . . C1 C 0.8718(7) 0.3335(6) 0.8663(13) 0.024(2) Uani 1 1 d . . . C9 C 1.1789(7) 0.1993(5) 1.1391(12) 0.022(2) Uani 1 1 d . . . C3 C 0.9101(6) 0.2025(5) 0.9126(11) 0.018(2) Uani 1 1 d . . . C4 C 0.8199(8) 0.4931(5) 0.7671(12) 0.033(3) Uani 1 1 d . . . H4A H 0.8636 0.5140 0.7014 0.040 Uiso 1 1 calc R . . H4B H 0.7680 0.4577 0.6947 0.040 Uiso 1 1 calc R . . C5 C 0.7635(8) 0.5634(6) 0.8169(12) 0.023(2) Uani 1 1 d . . . C10 C 1.0821(6) 0.1675(5) 1.1830(11) 0.022(2) Uani 1 1 d . . . H10A H 1.0494 0.2125 1.2244 0.026 Uiso 1 1 calc R . . H10B H 1.1046 0.1284 1.2733 0.026 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 Pb1 0.02153(19) 0.0219(2) 0.0159(2) -0.00102(17) 0.00452(17) 0.00003(17) Pb2 0.01827(18) 0.0211(2) 0.0226(2) 0.00577(18) 0.00554(17) 0.00298(17) S3 0.0240(12) 0.0205(13) 0.0312(16) 0.0030(12) 0.0019(13) 0.0001(11) S2 0.0223(12) 0.0243(13) 0.0213(15) -0.0040(12) 0.0013(12) 0.0011(11) S1 0.0358(14) 0.0190(14) 0.0328(17) -0.0074(12) 0.0012(14) -0.0005(12) O1 0.051(4) 0.029(4) 0.056(5) -0.001(4) 0.036(4) -0.011(4) O2 0.033(4) 0.017(4) 0.027(4) 0.012(3) 0.011(3) 0.010(3) O9 0.038(3) 0.025(3) 0.009(3) 0.000(2) 0.000(2) -0.011(2) O3 0.038(3) 0.025(3) 0.009(3) 0.000(2) 0.000(2) -0.011(2) O6 0.064(5) 0.034(4) 0.054(5) 0.013(4) 0.041(5) 0.018(4) O8 0.055(5) 0.034(4) 0.018(4) 0.001(4) 0.001(4) 0.012(4) O7 0.032(4) 0.031(4) 0.018(4) -0.001(3) 0.001(4) 0.009(3) O5 0.015(3) 0.041(4) 0.011(4) 0.006(3) -0.006(3) -0.001(3) O4 0.023(4) 0.054(5) 0.025(4) 0.017(4) 0.002(4) -0.004(4) N1 0.020(4) 0.017(4) 0.021(5) -0.004(4) 0.008(4) 0.000(4) N2 0.016(4) 0.022(5) 0.015(5) 0.001(4) 0.000(4) 0.001(4) N3 0.017(4) 0.027(5) 0.025(5) 0.001(4) 0.003(4) 0.001(4) C7 0.021(5) 0.021(5) 0.012(5) 0.000(5) -0.001(5) 0.008(5) C6 0.022(5) 0.029(6) 0.020(6) -0.001(5) 0.005(5) 0.000(5) C8 0.017(5) 0.023(5) 0.012(6) 0.002(5) -0.008(5) 0.000(4) C2 0.017(5) 0.022(5) 0.014(6) -0.007(5) 0.011(5) 0.002(4) C1 0.020(5) 0.023(6) 0.037(7) 0.004(5) 0.020(5) 0.004(5) C9 0.026(5) 0.018(5) 0.023(6) 0.007(5) 0.009(5) 0.002(5) C3 0.015(4) 0.019(5) 0.024(6) 0.000(5) 0.012(5) 0.002(5) C4 0.052(7) 0.016(5) 0.031(7) -0.002(5) 0.012(6) 0.005(5) C5 0.029(5) 0.022(5) 0.022(6) -0.006(5) 0.014(5) -0.013(5) C10 0.018(5) 0.025(5) 0.014(6) 0.003(5) -0.009(4) 0.001(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 Pb1 O3 2.464(6) . ? Pb1 O9 2.471(6) . ? Pb1 O2 2.542(6) . ? Pb1 O1 2.635(7) . ? Pb1 O2 2.659(5) 3_666 ? Pb1 O6 2.696(6) . ? Pb1 O8 2.890(7) 3_666 ? Pb1 C7 2.925(8) . ? Pb1 O5 3.145(6) 4_465 ? Pb1 Pb2 4.3187(6) 4_565 ? Pb1 Pb1 4.3225(7) 3_666 ? Pb2 O7 2.415(6) 3_667 ? Pb2 O4 2.429(6) 1_455 ? Pb2 O5 2.442(6) 4_465 ? Pb2 O3 2.646(6) . ? Pb2 O8 2.700(6) 3_667 ? Pb2 O5 2.850(6) 1_455 ? Pb2 O1 2.854(6) 4_566 ? Pb2 C5 2.899(9) 3_667 ? Pb2 C9 2.971(8) 1_455 ? Pb2 Pb1 4.3187(6) 4_566 ? S3 C3 1.745(9) . ? S3 C10 1.793(9) . ? S2 C2 1.721(9) . ? S2 C6 1.793(9) . ? S1 C1 1.738(10) . ? S1 C4 1.811(10) . ? O1 C7 1.246(10) . ? O1 Pb2 2.854(6) 4_565 ? O2 C7 1.250(10) . ? O2 Pb1 2.659(5) 3_666 ? O9 C8 1.227(10) 3_667 ? O3 C8 1.242(10) . ? O8 C5 1.249(11) . ? O8 Pb2 2.700(6) 3_667 ? O8 Pb1 2.890(7) 3_666 ? O7 C5 1.282(10) . ? O7 Pb2 2.415(6) 3_667 ? O5 C9 1.259(10) . ? O5 Pb2 2.442(6) 4_666 ? O5 Pb2 2.850(6) 1_655 ? O5 Pb1 3.145(6) 4_666 ? O4 C9 1.227(10) . ? O4 Pb2 2.429(6) 1_655 ? N1 C2 1.349(10) . ? N1 C1 1.354(11) . ? N2 C2 1.341(11) . ? N2 C3 1.359(11) . ? N3 C3 1.312(11) . ? N3 C1 1.329(11) . ? C7 C6 1.511(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 O9 1.227(10) 3_667 ? C8 C8 1.551(17) 3_667 ? C9 C10 1.530(11) . ? C9 Pb2 2.971(8) 1_655 ? C4 C5 1.501(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 Pb2 2.899(9) 3_667 ? C10 H10A 0.9700 . ? C10 H10B 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 O3 Pb1 O9 66.26(19) . . ? O3 Pb1 O2 99.6(2) . . ? O9 Pb1 O2 80.5(2) . . ? O3 Pb1 O1 79.2(2) . . ? O9 Pb1 O1 112.7(2) . . ? O2 Pb1 O1 49.86(18) . . ? O3 Pb1 O2 138.0(2) . 3_666 ? O9 Pb1 O2 72.06(19) . 3_666 ? O2 Pb1 O2 67.6(2) . 3_666 ? O1 Pb1 O2 113.19(18) . 3_666 ? O3 Pb1 O6 76.3(2) . . ? O9 Pb1 O6 81.8(2) . . ? O2 Pb1 O6 162.0(2) . . ? O1 Pb1 O6 143.13(19) . . ? O2 Pb1 O6 103.44(18) 3_666 . ? O3 Pb1 O8 140.2(2) . 3_666 ? O9 Pb1 O8 153.09(19) . 3_666 ? O2 Pb1 O8 88.1(2) . 3_666 ? O1 Pb1 O8 76.3(2) . 3_666 ? O2 Pb1 O8 81.07(19) 3_666 3_666 ? O6 Pb1 O8 106.4(2) . 3_666 ? O3 Pb1 C7 92.9(2) . . ? O9 Pb1 C7 99.9(2) . . ? O2 Pb1 C7 25.2(2) . . ? O1 Pb1 C7 25.2(2) . . ? O2 Pb1 C7 88.9(2) 3_666 . ? O6 Pb1 C7 167.4(2) . . ? O8 Pb1 C7 77.7(2) 3_666 . ? O3 Pb1 O5 59.95(18) . 4_465 ? O9 Pb1 O5 123.18(16) . 4_465 ? O2 Pb1 O5 124.10(17) . 4_465 ? O1 Pb1 O5 74.51(16) . 4_465 ? O2 Pb1 O5 160.19(18) 3_666 4_465 ? O6 Pb1 O5 69.45(17) . 4_465 ? O8 Pb1 O5 83.35(17) 3_666 4_465 ? C7 Pb1 O5 99.7(2) . 4_465 ? O3 Pb1 Pb2 81.41(15) . 4_565 ? O9 Pb1 Pb2 142.87(14) . 4_565 ? O2 Pb1 Pb2 87.78(13) . 4_565 ? O1 Pb1 Pb2 39.95(14) . 4_565 ? O2 Pb1 Pb2 134.63(13) 3_666 4_565 ? O6 Pb1 Pb2 108.63(15) . 4_565 ? O8 Pb1 Pb2 59.77(14) 3_666 4_565 ? C7 Pb1 Pb2 62.68(18) . 4_565 ? O5 Pb1 Pb2 41.26(10) 4_465 4_565 ? O3 Pb1 Pb1 123.71(14) . 3_666 ? O9 Pb1 Pb1 73.34(12) . 3_666 ? O2 Pb1 Pb1 34.66(13) . 3_666 ? O1 Pb1 Pb1 82.14(12) . 3_666 ? O2 Pb1 Pb1 32.93(12) 3_666 3_666 ? O6 Pb1 Pb1 134.60(14) . 3_666 ? O8 Pb1 Pb1 83.38(13) 3_666 3_666 ? C7 Pb1 Pb1 57.03(17) . 3_666 ? O5 Pb1 Pb1 155.28(11) 4_465 3_666 ? Pb2 Pb1 Pb1 114.169(12) 4_565 3_666 ? O7 Pb2 O4 83.3(2) 3_667 1_455 ? O7 Pb2 O5 81.5(2) 3_667 4_465 ? O4 Pb2 O5 80.2(2) 1_455 4_465 ? O7 Pb2 O3 80.0(2) 3_667 . ? O4 Pb2 O3 146.1(2) 1_455 . ? O5 Pb2 O3 68.4(2) 4_465 . ? O7 Pb2 O8 51.4(2) 3_667 3_667 ? O4 Pb2 O8 86.1(2) 1_455 3_667 ? O5 Pb2 O8 132.2(2) 4_465 3_667 ? O3 Pb2 O8 105.5(2) . 3_667 ? O7 Pb2 O5 109.71(18) 3_667 1_455 ? O4 Pb2 O5 48.21(19) 1_455 1_455 ? O5 Pb2 O5 122.91(18) 4_465 1_455 ? O3 Pb2 O5 165.36(18) . 1_455 ? O8 Pb2 O5 74.39(19) 3_667 1_455 ? O7 Pb2 O1 168.4(2) 3_667 4_566 ? O4 Pb2 O1 107.6(2) 1_455 4_566 ? O5 Pb2 O1 103.8(2) 4_465 4_566 ? O3 Pb2 O1 92.37(19) . 4_566 ? O8 Pb2 O1 123.9(2) 3_667 4_566 ? O5 Pb2 O1 76.28(17) 1_455 4_566 ? O7 Pb2 C5 25.9(2) 3_667 3_667 ? O4 Pb2 C5 84.5(2) 1_455 3_667 ? O5 Pb2 C5 107.2(3) 4_465 3_667 ? O3 Pb2 C5 92.7(2) . 3_667 ? O8 Pb2 C5 25.5(2) 3_667 3_667 ? O5 Pb2 C5 92.3(2) 1_455 3_667 ? O1 Pb2 C5 148.2(3) 4_566 3_667 ? O7 Pb2 C9 94.2(2) 3_667 1_455 ? O4 Pb2 C9 23.7(2) 1_455 1_455 ? O5 Pb2 C9 102.5(3) 4_465 1_455 ? O3 Pb2 C9 169.7(2) . 1_455 ? O8 Pb2 C9 76.7(2) 3_667 1_455 ? O5 Pb2 C9 24.9(2) 1_455 1_455 ? O1 Pb2 C9 94.6(2) 4_566 1_455 ? C5 Pb2 C9 85.4(2) 3_667 1_455 ? O7 Pb2 Pb1 153.55(15) 3_667 4_566 ? O4 Pb2 Pb1 71.41(16) 1_455 4_566 ? O5 Pb2 Pb1 101.25(15) 4_465 4_566 ? O3 Pb2 Pb1 125.77(14) . 4_566 ? O8 Pb2 Pb1 117.22(15) 3_667 4_566 ? O5 Pb2 Pb1 46.70(12) 1_455 4_566 ? O1 Pb2 Pb1 36.36(13) 4_566 4_566 ? C5 Pb2 Pb1 138.72(17) 3_667 4_566 ? C9 Pb2 Pb1 59.36(17) 1_455 4_566 ? C3 S3 C10 103.2(4) . . ? C2 S2 C6 100.4(4) . . ? C1 S1 C4 103.2(5) . . ? C7 O1 Pb1 90.5(5) . . ? C7 O1 Pb2 146.2(6) . 4_565 ? Pb1 O1 Pb2 103.7(2) . 4_565 ? C7 O2 Pb1 94.8(5) . . ? C7 O2 Pb1 136.8(6) . 3_666 ? Pb1 O2 Pb1 112.4(2) . 3_666 ? C8 O9 Pb1 117.6(6) 3_667 . ? C8 O3 Pb1 118.6(5) . . ? C8 O3 Pb2 107.5(5) . . ? Pb1 O3 Pb2 123.8(3) . . ? C5 O8 Pb2 86.2(5) . 3_667 ? C5 O8 Pb1 120.1(6) . 3_666 ? Pb2 O8 Pb1 138.0(3) 3_667 3_666 ? C5 O7 Pb2 98.6(6) . 3_667 ? C9 O5 Pb2 134.8(5) . 4_666 ? C9 O5 Pb2 83.0(5) . 1_655 ? Pb2 O5 Pb2 118.7(2) 4_666 1_655 ? C9 O5 Pb1 111.7(6) . 4_666 ? Pb2 O5 Pb1 106.9(2) 4_666 4_666 ? Pb2 O5 Pb1 92.04(15) 1_655 4_666 ? C9 O4 Pb2 103.8(6) . 1_655 ? C2 N1 C1 113.1(8) . . ? C2 N2 C3 114.8(8) . . ? C3 N3 C1 114.8(8) . . ? O1 C7 O2 122.1(8) . . ? O1 C7 C6 119.4(8) . . ? O2 C7 C6 118.4(8) . . ? O1 C7 Pb1 64.3(5) . . ? O2 C7 Pb1 60.0(4) . . ? C6 C7 Pb1 160.8(6) . . ? C7 C6 S2 115.8(6) . . ? C7 C6 H6A 108.3 . . ? S2 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? S2 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? O9 C8 O3 124.7(8) 3_667 . ? O9 C8 C8 118.6(11) 3_667 3_667 ? O3 C8 C8 116.6(10) . 3_667 ? N2 C2 N1 125.1(8) . . ? N2 C2 S2 114.8(7) . . ? N1 C2 S2 120.1(7) . . ? N3 C1 N1 126.7(9) . . ? N3 C1 S1 114.1(8) . . ? N1 C1 S1 119.3(7) . . ? O4 C9 O5 123.4(8) . . ? O4 C9 C10 119.2(9) . . ? O5 C9 C10 117.3(8) . . ? O4 C9 Pb2 52.6(4) . 1_655 ? O5 C9 Pb2 72.2(5) . 1_655 ? C10 C9 Pb2 163.5(6) . 1_655 ? N3 C3 N2 125.1(8) . . ? N3 C3 S3 122.2(7) . . ? N2 C3 S3 112.7(7) . . ? C5 C4 S1 116.4(7) . . ? C5 C4 H4A 108.2 . . ? S1 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? S1 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? O8 C5 O7 123.8(8) . . ? O8 C5 C4 117.9(8) . . ? O7 C5 C4 118.2(9) . . ? O8 C5 Pb2 68.3(5) . 3_667 ? O7 C5 Pb2 55.5(4) . 3_667 ? C4 C5 Pb2 173.7(7) . 3_667 ? C9 C10 S3 114.7(6) . . ? C9 C10 H10A 108.6 . . ? S3 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? S3 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.747 _refine_diff_density_min -1.584 _refine_diff_density_rms 0.212 data_110422-5 _database_code_depnum_ccdc_archive 'CCDC 918096' #TrackingRef '110125-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N6 O14 Pb3 S6' _chemical_formula_weight 1350.36 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' 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' Pb Pb -3.3944 10.1111 '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' H H 0.0000 0.0000 '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 8.2682(4) _cell_length_b 9.0948(4) _cell_length_c 10.6166(5) _cell_angle_alpha 85.777(4) _cell_angle_beta 78.575(4) _cell_angle_gamma 87.068(4) _cell_volume 779.85(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4573 _cell_measurement_theta_min 2.2425 _cell_measurement_theta_max 29.1110 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 16.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44975 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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_type 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6326 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2741 _reflns_number_gt 2330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^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_extinction_coef ? _refine_ls_number_reflns 2741 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.47937(4) 0.23489(3) 1.03387(3) 0.01939(12) Uani 1 1 d . . . Pb2A Pb 0.04035(8) 0.57903(7) 0.98105(7) 0.01786(17) Uani 0.48 1 d P . . Pb2B Pb 0.0517(16) 0.6441(14) 0.9062(14) 0.020(3) Uani 0.02 1 d P . . S3 S 0.1140(3) 0.1230(2) 0.2826(2) 0.0237(5) Uani 1 1 d . . . S2 S 0.3664(3) 0.0168(2) 0.6987(2) 0.0252(5) Uani 1 1 d . . . S1 S 0.2665(3) -0.4259(2) 0.4512(2) 0.0335(6) Uani 1 1 d . . . O3 O 0.3694(7) -0.0403(6) 0.0988(5) 0.0209(13) Uani 1 1 d . . . O5 O 0.4292(8) -0.3662(7) 0.1732(5) 0.0299(14) Uani 1 1 d . . . O6 O 0.2636(8) -0.5030(7) 0.0919(6) 0.0367(16) Uani 1 1 d . . . O1 O 0.1424(9) 0.3776(8) 0.8138(6) 0.0448(13) Uani 1 1 d . . . O2 O 0.2580(9) 0.2009(8) 0.9204(6) 0.0448(13) Uani 1 1 d . . . O4 O 0.2003(7) -0.1749(6) 0.0266(6) 0.0314(15) Uani 1 1 d . . . O7 O 0.3842(10) 0.6373(7) 0.7717(6) 0.0468(19) Uani 1 1 d . . . N1 N 0.3128(9) -0.1865(7) 0.5557(6) 0.0228(16) Uani 1 1 d . . . N2 N 0.1857(9) -0.1481(7) 0.3724(6) 0.0231(16) Uani 1 1 d . . . N3 N 0.2348(8) 0.0569(7) 0.4867(6) 0.0211(16) Uani 1 1 d . . . C9 C 0.3047(11) -0.4412(9) 0.1822(8) 0.0233(19) Uani 1 1 d . . . C8 C 0.1854(12) -0.4573(10) 0.3114(8) 0.029(2) Uani 1 1 d . . . H8A H 0.1440 -0.5562 0.3218 0.035 Uiso 1 1 calc R . . H8B H 0.0920 -0.3890 0.3084 0.035 Uiso 1 1 calc R . . C1 C 0.2530(10) -0.2324(8) 0.4574(8) 0.0199(18) Uani 1 1 d . . . C3 C 0.1853(10) -0.0054(9) 0.3916(8) 0.0211(18) Uani 1 1 d . . . C5 C 0.2341(10) 0.2669(9) 0.8179(9) 0.0229(19) Uani 1 1 d . . . C4 C 0.3113(13) 0.2135(9) 0.6918(9) 0.032(2) Uani 1 1 d . . . H4A H 0.4101 0.2680 0.6577 0.039 Uiso 1 1 calc R . . H4B H 0.2357 0.2334 0.6329 0.039 Uiso 1 1 calc R . . C2 C 0.2953(10) -0.0404(9) 0.5667(8) 0.0202(18) Uani 1 1 d . . . C7 C 0.2260(11) -0.0749(8) 0.0927(8) 0.0196(18) Uani 1 1 d . . . C6 C 0.0751(10) 0.0048(9) 0.1665(8) 0.0187(17) Uani 1 1 d . . . H6A H -0.0017 -0.0684 0.2101 0.022 Uiso 1 1 calc R . . H6B H 0.0214 0.0629 0.1052 0.022 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 Pb1 0.02048(19) 0.01939(17) 0.01969(19) -0.00572(12) -0.00609(14) 0.00100(12) Pb2A 0.0192(4) 0.0165(4) 0.0184(4) -0.0028(3) -0.0051(3) 0.0022(3) Pb2B 0.025(7) 0.011(6) 0.029(8) -0.010(6) -0.012(6) -0.002(5) S3 0.0279(12) 0.0191(10) 0.0236(11) -0.0036(9) -0.0050(10) 0.0057(9) S2 0.0315(13) 0.0249(11) 0.0210(11) -0.0111(9) -0.0076(10) 0.0036(9) S1 0.0664(18) 0.0160(10) 0.0198(11) -0.0022(9) -0.0118(12) -0.0023(11) O3 0.014(3) 0.022(3) 0.027(3) -0.007(3) -0.002(3) -0.002(2) O5 0.028(4) 0.041(4) 0.020(3) 0.003(3) -0.008(3) 0.003(3) O6 0.039(4) 0.048(4) 0.026(3) -0.015(3) -0.011(3) 0.015(3) O1 0.054(3) 0.046(3) 0.027(3) 0.004(2) 0.002(2) 0.015(2) O2 0.054(3) 0.046(3) 0.027(3) 0.004(2) 0.002(2) 0.015(2) O4 0.030(4) 0.026(3) 0.043(4) -0.017(3) -0.011(3) 0.002(3) O7 0.077(6) 0.033(4) 0.038(4) -0.004(3) -0.028(4) 0.000(4) N1 0.033(4) 0.019(3) 0.016(4) -0.007(3) -0.004(3) 0.004(3) N2 0.032(4) 0.018(3) 0.020(4) -0.003(3) -0.006(3) 0.001(3) N3 0.026(4) 0.022(4) 0.015(3) -0.005(3) -0.005(3) -0.001(3) C9 0.033(5) 0.020(4) 0.020(4) -0.004(4) -0.013(4) 0.012(4) C8 0.048(6) 0.025(5) 0.018(4) -0.009(4) -0.014(4) -0.008(4) C1 0.024(5) 0.017(4) 0.017(4) -0.005(3) 0.002(4) -0.002(3) C3 0.018(5) 0.025(4) 0.019(4) -0.001(4) 0.000(4) 0.001(3) C5 0.020(5) 0.015(4) 0.031(5) -0.007(4) 0.002(4) -0.001(3) C4 0.048(6) 0.024(5) 0.023(5) -0.004(4) -0.001(5) 0.001(4) C2 0.016(4) 0.025(4) 0.018(4) -0.009(4) 0.003(4) 0.000(3) C7 0.030(5) 0.012(4) 0.018(4) 0.002(3) -0.010(4) 0.002(3) C6 0.018(4) 0.024(4) 0.016(4) -0.003(3) -0.005(4) 0.002(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 Pb1 O5 2.424(6) 2_656 ? Pb1 O2 2.425(8) . ? Pb1 O3 2.474(5) 2_656 ? Pb1 O4 2.637(6) 2_656 ? Pb1 O3 2.701(5) 1_556 ? Pb1 O7 2.880(7) 2_667 ? Pb1 C7 2.913(8) 2_656 ? Pb1 O6 2.931(6) 1_566 ? Pb1 Pb2B 4.262(13) 2_667 ? Pb1 Pb2A 4.3655(8) 2_667 ? Pb1 Pb1 4.3698(6) 2_657 ? Pb1 Pb2B 4.405(13) 2_567 ? Pb2A Pb2B 0.947(16) . ? Pb2A Pb2A 1.6063(14) 2_567 ? Pb2A Pb2B 2.360(15) 2_567 ? Pb2A O6 2.437(6) 1_566 ? Pb2A O1 2.438(6) 2_567 ? Pb2A O1 2.636(7) . ? Pb2A O4 2.777(6) 1_566 ? Pb2A O6 2.902(7) 2_556 ? Pb2A C5 3.141(8) 2_567 ? Pb2A Pb1 4.3655(8) 2_667 ? Pb2B Pb2A 2.360(15) 2_567 ? Pb2B O4 2.645(12) 1_566 ? Pb2B O1 2.696(13) . ? Pb2B O7 2.835(16) . ? Pb2B O6 2.960(14) 2_556 ? Pb2B O6 3.080(16) 1_566 ? Pb2B O1 3.084(16) 2_567 ? Pb2B Pb2B 3.22(3) 2_567 ? Pb2B S3 3.247(15) 2_566 ? Pb2B Pb1 4.262(13) 2_667 ? Pb2B Pb1 4.405(13) 2_567 ? S3 C3 1.747(9) . ? S3 C6 1.779(8) . ? S3 Pb2B 3.247(15) 2_566 ? S2 C2 1.745(8) . ? S2 C4 1.824(9) . ? S1 C1 1.762(8) . ? S1 C8 1.791(8) . ? O3 C7 1.257(10) . ? O3 Pb1 2.474(5) 2_656 ? O3 Pb1 2.701(5) 1_554 ? O5 C9 1.248(10) . ? O5 Pb1 2.424(6) 2_656 ? O6 C9 1.256(10) . ? O6 Pb2A 2.437(6) 1_544 ? O6 Pb2A 2.902(7) 2_556 ? O6 Pb1 2.931(6) 1_544 ? O6 Pb2B 2.960(14) 2_556 ? O6 Pb2B 3.080(16) 1_544 ? O1 C5 1.233(10) . ? O1 Pb2A 2.438(6) 2_567 ? O1 Pb2B 3.084(16) 2_567 ? O2 C5 1.249(11) . ? O4 C7 1.239(9) . ? O4 Pb1 2.637(6) 2_656 ? O4 Pb2B 2.645(12) 1_544 ? O4 Pb2A 2.777(6) 1_544 ? O7 Pb1 2.880(7) 2_667 ? N1 C2 1.340(10) . ? N1 C1 1.342(10) . ? N2 C3 1.329(10) . ? N2 C1 1.329(10) . ? N3 C2 1.329(10) . ? N3 C3 1.334(10) . ? C9 C8 1.525(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C5 C4 1.470(12) . ? C5 Pb2A 3.141(8) 2_567 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C7 C6 1.516(11) . ? C7 Pb1 2.913(8) 2_656 ? C6 H6A 0.9700 . ? C6 H6B 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 O5 Pb1 O2 76.9(2) 2_656 . ? O5 Pb1 O3 77.1(2) 2_656 2_656 ? O2 Pb1 O3 85.2(2) . 2_656 ? O5 Pb1 O4 74.7(2) 2_656 2_656 ? O2 Pb1 O4 131.4(2) . 2_656 ? O3 Pb1 O4 50.51(17) 2_656 2_656 ? O5 Pb1 O3 131.96(19) 2_656 1_556 ? O2 Pb1 O3 72.0(2) . 1_556 ? O3 Pb1 O3 64.9(2) 2_656 1_556 ? O4 Pb1 O3 99.94(17) 2_656 1_556 ? O5 Pb1 O7 109.9(2) 2_656 2_667 ? O2 Pb1 O7 152.7(2) . 2_667 ? O3 Pb1 O7 121.98(19) 2_656 2_667 ? O4 Pb1 O7 75.08(19) 2_656 2_667 ? O3 Pb1 O7 114.69(18) 1_556 2_667 ? O5 Pb1 C7 73.5(2) 2_656 2_656 ? O2 Pb1 C7 108.4(2) . 2_656 ? O3 Pb1 C7 25.35(19) 2_656 2_656 ? O4 Pb1 C7 25.18(19) 2_656 2_656 ? O3 Pb1 C7 82.66(19) 1_556 2_656 ? O7 Pb1 C7 98.9(2) 2_667 2_656 ? O5 Pb1 O6 84.64(19) 2_656 1_566 ? O2 Pb1 O6 77.3(2) . 1_566 ? O3 Pb1 O6 157.11(18) 2_656 1_566 ? O4 Pb1 O6 136.82(19) 2_656 1_566 ? O3 Pb1 O6 121.61(18) 1_556 1_566 ? O7 Pb1 O6 77.10(19) 2_667 1_566 ? C7 Pb1 O6 155.1(2) 2_656 1_566 ? O5 Pb1 Pb2B 82.2(3) 2_656 2_667 ? O2 Pb1 Pb2B 158.8(3) . 2_667 ? O3 Pb1 Pb2B 86.7(2) 2_656 2_667 ? O4 Pb1 Pb2B 36.27(19) 2_656 2_667 ? O3 Pb1 Pb2B 121.6(2) 1_556 2_667 ? O7 Pb1 Pb2B 41.4(2) 2_667 2_667 ? C7 Pb1 Pb2B 61.4(2) 2_656 2_667 ? O6 Pb1 Pb2B 104.5(2) 1_566 2_667 ? O5 Pb1 Pb2A 69.89(15) 2_656 2_667 ? O2 Pb1 Pb2A 146.78(17) . 2_667 ? O3 Pb1 Pb2A 86.60(12) 2_656 2_667 ? O4 Pb1 Pb2A 37.35(12) 2_656 2_667 ? O3 Pb1 Pb2A 131.78(12) 1_556 2_667 ? O7 Pb1 Pb2A 48.77(15) 2_667 2_667 ? C7 Pb1 Pb2A 61.56(16) 2_656 2_667 ? O6 Pb1 Pb2A 100.03(14) 1_566 2_667 ? Pb2B Pb1 Pb2A 12.5(2) 2_667 2_667 ? O5 Pb1 Pb1 106.65(15) 2_656 2_657 ? O2 Pb1 Pb1 76.18(16) . 2_657 ? O3 Pb1 Pb1 34.03(13) 2_656 2_657 ? O4 Pb1 Pb1 75.32(12) 2_656 2_657 ? O3 Pb1 Pb1 30.84(11) 1_556 2_657 ? O7 Pb1 Pb1 123.92(13) 2_667 2_657 ? C7 Pb1 Pb1 53.80(15) 2_656 2_657 ? O6 Pb1 Pb1 147.74(14) 1_566 2_657 ? Pb2B Pb1 Pb1 106.96(16) 2_667 2_657 ? Pb2A Pb1 Pb1 112.227(14) 2_667 2_657 ? O5 Pb1 Pb2B 99.4(3) 2_656 2_567 ? O2 Pb1 Pb2B 44.6(2) . 2_567 ? O3 Pb1 Pb2B 127.81(19) 2_656 2_567 ? O4 Pb1 Pb2B 174.0(2) 2_656 2_567 ? O3 Pb1 Pb2B 83.2(2) 1_556 2_567 ? O7 Pb1 Pb2B 108.3(2) 2_667 2_567 ? C7 Pb1 Pb2B 152.6(2) 2_656 2_567 ? O6 Pb1 Pb2B 41.9(2) 1_566 2_567 ? Pb2B Pb1 Pb2B 145.1(3) 2_667 2_567 ? Pb2A Pb1 Pb2B 141.88(15) 2_667 2_567 ? Pb1 Pb1 Pb2B 105.89(15) 2_657 2_567 ? Pb2B Pb2A Pb2A 133.4(7) . 2_567 ? Pb2B Pb2A Pb2B 150.4(5) . 2_567 ? Pb2A Pb2A Pb2B 16.9(3) 2_567 2_567 ? Pb2B Pb2A O6 125.0(8) . 1_566 ? Pb2A Pb2A O6 89.28(17) 2_567 1_566 ? Pb2B Pb2A O6 76.2(4) 2_567 1_566 ? Pb2B Pb2A O1 125.3(7) . 2_567 ? Pb2A Pb2A O1 78.39(18) 2_567 2_567 ? Pb2B Pb2A O1 68.4(3) 2_567 2_567 ? O6 Pb2A O1 90.6(2) 1_566 2_567 ? Pb2B Pb2A O1 83.4(7) . . ? Pb2A Pb2A O1 64.96(16) 2_567 . ? Pb2B Pb2A O1 76.0(3) 2_567 . ? O6 Pb2A O1 89.0(2) 1_566 . ? O1 Pb2A O1 143.35(10) 2_567 . ? Pb2B Pb2A O4 72.2(7) . 1_566 ? Pb2A Pb2A O4 154.41(14) 2_567 1_566 ? Pb2B Pb2A O4 137.5(3) 2_567 1_566 ? O6 Pb2A O4 71.4(2) 1_566 1_566 ? O1 Pb2A O4 85.0(2) 2_567 1_566 ? O1 Pb2A O4 129.1(2) . 1_566 ? Pb2B Pb2A O6 84.2(8) . 2_556 ? Pb2A Pb2A O6 57.12(14) 2_567 2_556 ? Pb2B Pb2A O6 70.8(3) 2_567 2_556 ? O6 Pb2A O6 146.40(9) 1_566 2_556 ? O1 Pb2A O6 83.1(2) 2_567 2_556 ? O1 Pb2A O6 77.3(2) . 2_556 ? O4 Pb2A O6 140.05(18) 1_566 2_556 ? Pb2B Pb2A C5 104.3(8) . 2_567 ? Pb2A Pb2A C5 91.93(15) 2_567 2_567 ? Pb2B Pb2A C5 85.6(3) 2_567 2_567 ? O6 Pb2A C5 107.1(2) 1_566 2_567 ? O1 Pb2A C5 21.1(2) 2_567 2_567 ? O1 Pb2A C5 152.1(2) . 2_567 ? O4 Pb2A C5 78.45(19) 1_566 2_567 ? O6 Pb2A C5 76.8(2) 2_556 2_567 ? Pb2B Pb2A Pb1 77.5(8) . 2_667 ? Pb2A Pb2A Pb1 136.56(6) 2_567 2_667 ? Pb2B Pb2A Pb1 125.5(3) 2_567 2_667 ? O6 Pb2A Pb1 49.48(17) 1_566 2_667 ? O1 Pb2A Pb1 110.35(18) 2_567 2_667 ? O1 Pb2A Pb1 96.94(17) . 2_667 ? O4 Pb2A Pb1 35.19(12) 1_566 2_667 ? O6 Pb2A Pb1 161.36(13) 2_556 2_667 ? C5 Pb2A Pb1 110.89(15) 2_567 2_667 ? Pb2A Pb2B Pb2A 29.6(5) . 2_567 ? Pb2A Pb2B O4 87.9(8) . 1_566 ? Pb2A Pb2B O4 117.5(6) 2_567 1_566 ? Pb2A Pb2B O1 76.2(7) . . ? Pb2A Pb2B O1 57.2(3) 2_567 . ? O4 Pb2B O1 132.4(6) 1_566 . ? Pb2A Pb2B O7 110.1(9) . . ? Pb2A Pb2B O7 115.5(5) 2_567 . ? O4 Pb2B O7 75.7(4) 1_566 . ? O1 Pb2B O7 68.7(4) . . ? Pb2A Pb2B O6 77.3(8) . 2_556 ? Pb2A Pb2B O6 53.1(3) 2_567 2_556 ? O4 Pb2B O6 144.4(5) 1_566 2_556 ? O1 Pb2B O6 75.4(3) . 2_556 ? O7 Pb2B O6 139.8(5) . 2_556 ? Pb2A Pb2B O6 40.4(6) . 1_566 ? Pb2A Pb2B O6 62.9(4) 2_567 1_566 ? O4 Pb2B O6 64.0(3) 1_566 1_566 ? O1 Pb2B O6 75.7(4) . 1_566 ? O7 Pb2B O6 72.7(4) . 1_566 ? O6 Pb2B O6 115.7(5) 2_556 1_566 ? Pb2A Pb2B O1 40.2(6) . 2_567 ? Pb2A Pb2B O1 56.0(4) 2_567 2_567 ? O4 Pb2B O1 75.7(4) 1_566 2_567 ? O1 Pb2B O1 112.7(5) . 2_567 ? O7 Pb2B O1 138.9(5) . 2_567 ? O6 Pb2B O1 72.1(4) 2_556 2_567 ? O6 Pb2B O1 68.4(4) 1_566 2_567 ? Pb2A Pb2B Pb2B 21.3(4) . 2_567 ? Pb2A Pb2B Pb2B 8.37(14) 2_567 2_567 ? O4 Pb2B Pb2B 109.2(7) 1_566 2_567 ? O1 Pb2B Pb2B 62.1(4) . 2_567 ? O7 Pb2B Pb2B 114.7(6) . 2_567 ? O6 Pb2B Pb2B 59.6(4) 2_556 2_567 ? O6 Pb2B Pb2B 56.0(4) 1_566 2_567 ? O1 Pb2B Pb2B 50.6(4) 2_567 2_567 ? Pb2A Pb2B S3 149.6(10) . 2_566 ? Pb2A Pb2B S3 132.0(5) 2_567 2_566 ? O4 Pb2B S3 100.9(4) 1_566 2_566 ? O1 Pb2B S3 115.5(5) . 2_566 ? O7 Pb2B S3 100.3(5) . 2_566 ? O6 Pb2B S3 78.9(3) 2_556 2_566 ? O6 Pb2B S3 164.3(4) 1_566 2_566 ? O1 Pb2B S3 113.6(4) 2_567 2_566 ? Pb2B Pb2B S3 138.1(6) 2_567 2_566 ? Pb2A Pb2B Pb1 90.0(8) . 2_667 ? Pb2A Pb2B Pb1 113.7(5) 2_567 2_667 ? O4 Pb2B Pb1 36.1(2) 1_566 2_667 ? O1 Pb2B Pb1 98.4(4) . 2_667 ? O7 Pb2B Pb1 42.2(2) . 2_667 ? O6 Pb2B Pb1 166.8(5) 2_556 2_667 ? O6 Pb2B Pb1 51.1(2) 1_566 2_667 ? O1 Pb2B Pb1 100.4(4) 2_567 2_667 ? Pb2B Pb2B Pb1 107.1(6) 2_567 2_667 ? S3 Pb2B Pb1 114.3(4) 2_566 2_667 ? Pb2A Pb2B Pb1 93.7(8) . 2_567 ? Pb2A Pb2B Pb1 83.7(4) 2_567 2_567 ? O4 Pb2B Pb1 109.3(4) 1_566 2_567 ? O1 Pb2B Pb1 116.2(4) . 2_567 ? O7 Pb2B Pb1 156.0(5) . 2_567 ? O6 Pb2B Pb1 41.4(2) 2_556 2_567 ? O6 Pb2B Pb1 131.1(5) 1_566 2_567 ? O1 Pb2B Pb1 63.2(3) 2_567 2_567 ? Pb2B Pb2B Pb1 86.5(5) 2_567 2_567 ? S3 Pb2B Pb1 55.9(2) 2_566 2_567 ? Pb1 Pb2B Pb1 145.1(3) 2_667 2_567 ? C3 S3 C6 100.7(4) . . ? C3 S3 Pb2B 174.9(4) . 2_566 ? C6 S3 Pb2B 79.0(3) . 2_566 ? C2 S2 C4 101.8(4) . . ? C1 S1 C8 103.8(4) . . ? C7 O3 Pb1 97.2(5) . 2_656 ? C7 O3 Pb1 122.7(5) . 1_554 ? Pb1 O3 Pb1 115.1(2) 2_656 1_554 ? C9 O5 Pb1 115.7(5) . 2_656 ? C9 O6 Pb2A 126.1(5) . 1_544 ? C9 O6 Pb2A 137.3(6) . 2_556 ? Pb2A O6 Pb2A 33.60(9) 1_544 2_556 ? C9 O6 Pb1 109.2(5) . 1_544 ? Pb2A O6 Pb1 124.7(2) 1_544 1_544 ? Pb2A O6 Pb1 103.0(2) 2_556 1_544 ? C9 O6 Pb2B 127.6(6) . 2_556 ? Pb2A O6 Pb2B 50.7(3) 1_544 2_556 ? Pb2A O6 Pb2B 18.6(3) 2_556 2_556 ? Pb1 O6 Pb2B 96.8(3) 1_544 2_556 ? C9 O6 Pb2B 124.9(6) . 1_544 ? Pb2A O6 Pb2B 14.6(3) 1_544 1_544 ? Pb2A O6 Pb2B 46.3(3) 2_556 1_544 ? Pb1 O6 Pb2B 123.3(3) 1_544 1_544 ? Pb2B O6 Pb2B 64.3(5) 2_556 1_544 ? C5 O1 Pb2A 113.5(6) . 2_567 ? C5 O1 Pb2A 131.6(6) . . ? Pb2A O1 Pb2A 36.65(10) 2_567 . ? C5 O1 Pb2B 146.1(7) . . ? Pb2A O1 Pb2B 54.4(4) 2_567 . ? Pb2A O1 Pb2B 20.4(3) . . ? C5 O1 Pb2B 99.1(6) . 2_567 ? Pb2A O1 Pb2B 14.5(2) 2_567 2_567 ? Pb2A O1 Pb2B 48.0(2) . 2_567 ? Pb2B O1 Pb2B 67.3(5) . 2_567 ? C5 O2 Pb1 127.6(6) . . ? C7 O4 Pb1 90.0(5) . 2_656 ? C7 O4 Pb2B 162.4(6) . 1_544 ? Pb1 O4 Pb2B 107.6(3) 2_656 1_544 ? C7 O4 Pb2A 154.0(5) . 1_544 ? Pb1 O4 Pb2A 107.46(18) 2_656 1_544 ? Pb2B O4 Pb2A 19.9(3) 1_544 1_544 ? Pb2B O7 Pb1 96.4(3) . 2_667 ? C2 N1 C1 113.7(7) . . ? C3 N2 C1 112.6(7) . . ? C2 N3 C3 113.1(7) . . ? O5 C9 O6 125.7(8) . . ? O5 C9 C8 118.9(7) . . ? O6 C9 C8 115.3(8) . . ? C9 C8 S1 116.5(6) . . ? C9 C8 H8A 108.2 . . ? S1 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? S1 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? N2 C1 N1 126.6(7) . . ? N2 C1 S1 120.7(6) . . ? N1 C1 S1 112.7(6) . . ? N2 C3 N3 127.9(8) . . ? N2 C3 S3 119.0(6) . . ? N3 C3 S3 113.1(6) . . ? O1 C5 O2 123.5(8) . . ? O1 C5 C4 115.0(8) . . ? O2 C5 C4 121.5(7) . . ? O1 C5 Pb2A 45.4(4) . 2_567 ? O2 C5 Pb2A 79.3(5) . 2_567 ? C4 C5 Pb2A 156.3(7) . 2_567 ? C5 C4 S2 113.1(6) . . ? C5 C4 H4A 108.9 . . ? S2 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? S2 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? N3 C2 N1 126.0(7) . . ? N3 C2 S2 120.9(6) . . ? N1 C2 S2 113.2(6) . . ? O4 C7 O3 122.2(8) . . ? O4 C7 C6 116.7(7) . . ? O3 C7 C6 121.2(7) . . ? O4 C7 Pb1 64.9(4) . 2_656 ? O3 C7 Pb1 57.4(4) . 2_656 ? C6 C7 Pb1 176.5(5) . 2_656 ? C7 C6 S3 115.5(6) . . ? C7 C6 H6A 108.4 . . ? S3 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? S3 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.146 _refine_diff_density_min -2.007 _refine_diff_density_rms 0.244 data_111203g _database_code_depnum_ccdc_archive 'CCDC 918097' #TrackingRef '110125-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H134 N24 Ni6 O43 S12' _chemical_formula_weight 3193.37 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' Ni Ni 0.3393 1.1124 '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 31.068(3) _cell_length_b 13.5170(12) _cell_length_c 20.8591(18) _cell_angle_alpha 90.00 _cell_angle_beta 125.962(2) _cell_angle_gamma 90.00 _cell_volume 7090.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6274 _cell_measurement_theta_min 2.487 _cell_measurement_theta_max 27.4825 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3308 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17440 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0433 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6233 _reflns_number_gt 4704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+38.5853P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6233 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.08688(6) 0.2500 0.0335(2) Uani 1 2 d S . . Ni2 Ni 0.27480(2) 0.41331(4) 0.14005(3) 0.03210(18) Uani 1 1 d . . . N1 N 0.45881(17) 0.3544(3) -0.0803(2) 0.0409(10) Uani 1 1 d . . . N2 N 0.41769(16) 0.3000(3) -0.0195(2) 0.0376(9) Uani 1 1 d . . . N3 N 0.40988(16) 0.4690(3) -0.0592(2) 0.0377(9) Uani 1 1 d . . . N4 N 0.5000 0.2417(4) 0.2500 0.0314(12) Uani 1 2 d S . . N5 N 0.5000 0.9322(4) 0.2500 0.0531(18) Uani 1 2 d S . . N6 N 0.28075(15) 0.5661(3) 0.1303(2) 0.0358(9) Uani 1 1 d . . . N7 N 0.26069(15) 0.9332(3) 0.3018(2) 0.0350(9) Uani 1 1 d . . . O1 O 0.46597(14) 0.0849(2) 0.1294(2) 0.0406(8) Uani 1 1 d . . . O2 O 0.53510(16) 0.1127(4) 0.1265(2) 0.0728(14) Uani 1 1 d . . . O3 O 0.31120(14) 0.3840(3) 0.0833(2) 0.0442(8) Uani 1 1 d . . . O4 O 0.3178(2) 0.2183(3) 0.0883(3) 0.0795(16) Uani 1 1 d . . . O5 O 0.33989(16) 0.7210(3) -0.1990(2) 0.0644(12) Uani 1 1 d . . . O6 O 0.34932(13) 0.5889(2) -0.25405(19) 0.0398(8) Uani 1 1 d . . . O7 O 0.42304(14) 0.0836(2) 0.2210(2) 0.0471(9) Uani 1 1 d . . . H7D H 0.4211 0.1379 0.2397 0.057 Uiso 1 1 d R . . H7E H 0.4252 0.0391 0.2515 0.057 Uiso 1 1 d R . . O8 O 0.26386(14) 0.2614(2) 0.1463(2) 0.0421(8) Uani 1 1 d . . . H8B H 0.2843 0.2456 0.1949 0.051 Uiso 1 1 d R . . H8C H 0.2756 0.2321 0.1234 0.051 Uiso 1 1 d R . . O9 O 0.20216(14) 0.4145(3) 0.0292(2) 0.0462(9) Uani 1 1 d . . . H9E H 0.1973 0.3728 -0.0051 0.055 Uiso 1 1 d R . . H9F H 0.1778 0.4579 0.0057 0.055 Uiso 1 1 d R . . O10 O 0.1222(2) 0.4483(5) 0.4480(4) 0.0842(15) Uani 0.75 1 d P . . H10C H 0.0967 0.4893 0.4228 0.101 Uiso 0.75 1 d PR . . H10D H 0.1220 0.4243 0.4856 0.101 Uiso 0.75 1 d PR . . O11 O 0.1141(2) 0.3679(5) 0.5876(4) 0.0842(15) Uani 0.75 1 d P . . H11C H 0.0893 0.3819 0.5921 0.101 Uiso 0.75 1 d PR . . H11D H 0.1325 0.3214 0.6199 0.101 Uiso 0.75 1 d PR . . O12 O 0.0973(7) 0.2858(15) 0.4667(11) 0.080(6) Uani 0.25 1 d P . . H12C H 0.1042 0.3369 0.4503 0.096 Uiso 0.25 1 d PR . . H12D H 0.1007 0.3014 0.5089 0.096 Uiso 0.25 1 d PR . . S1 S 0.46915(6) 0.16731(10) -0.04661(8) 0.0444(3) Uani 1 1 d . . . S2 S 0.45928(5) 0.53462(11) -0.12101(8) 0.0469(3) Uani 1 1 d . . . S3 S 0.36438(5) 0.42479(10) 0.00982(8) 0.0430(3) Uani 1 1 d . . . C1 C 0.44593(18) 0.2862(4) -0.0483(3) 0.0347(11) Uani 1 1 d . . . C2 C 0.40056(19) 0.3934(4) -0.0272(3) 0.0371(11) Uani 1 1 d . . . C3 C 0.43957(18) 0.4454(4) -0.0834(3) 0.0378(11) Uani 1 1 d . . . C4 C 0.4872(2) 0.1000(3) 0.0946(3) 0.0383(11) Uani 1 1 d . . . C5 C 0.4488(2) 0.0969(4) 0.0044(3) 0.0425(12) Uani 1 1 d . . . H5A H 0.4145 0.1214 -0.0113 0.051 Uiso 1 1 calc R . . H5B H 0.4440 0.0285 -0.0126 0.051 Uiso 1 1 calc R . . C6 C 0.3244(2) 0.3034(4) 0.0701(3) 0.0462(13) Uani 1 1 d . . . C7 C 0.3526(2) 0.3026(4) 0.0306(3) 0.0453(13) Uani 1 1 d . . . H7A H 0.3313 0.2657 -0.0186 0.054 Uiso 1 1 calc R . . H7B H 0.3863 0.2686 0.0647 0.054 Uiso 1 1 calc R . . C8 C 0.3660(2) 0.6500(4) -0.1995(3) 0.0408(12) Uani 1 1 d . . . C9 C 0.4237(2) 0.6417(4) -0.1262(3) 0.0463(13) Uani 1 1 d . . . H9A H 0.4238 0.6428 -0.0796 0.056 Uiso 1 1 calc R . . H9B H 0.4428 0.6998 -0.1240 0.056 Uiso 1 1 calc R . . C10 C 0.4573(2) 0.2938(4) 0.2295(3) 0.0445(12) Uani 1 1 d . . . H10 H 0.4270 0.2596 0.2160 0.053 Uiso 1 1 calc R . . C11 C 0.4555(3) 0.3953(4) 0.2272(4) 0.0587(16) Uani 1 1 d . . . H11 H 0.4241 0.4278 0.2102 0.070 Uiso 1 1 calc R . . C12 C 0.5000 0.4493(5) 0.2500 0.067(3) Uani 1 2 d S . . C13 C 0.5164(4) 0.8810(4) 0.2133(4) 0.079(2) Uani 1 1 d . . . H13 H 0.5159 0.9140 0.1738 0.095 Uiso 1 1 calc R A 1 C14 C 0.5341(6) 0.7834(8) 0.2282(7) 0.045(3) Uani 0.50 1 d P . 1 H14 H 0.5523 0.7573 0.2092 0.054 Uiso 0.50 1 calc PR . 1 C14' C 0.4986(7) 0.7770(9) 0.1943(9) 0.057(3) Uani 0.50 1 d P . 2 H14' H 0.4765 0.7487 0.1442 0.068 Uiso 0.50 1 d PR . 2 C15 C 0.5231(4) 0.7267(6) 0.2729(6) 0.045(3) Uani 0.50 1 d P . . C16 C 0.4820(4) 0.5599(8) 0.2303(7) 0.048(3) Uani 0.50 1 d P . . H16A H 0.4661 0.5739 0.1750 0.058 Uiso 0.50 1 d PR . . H16B H 0.4564 0.5749 0.2413 0.058 Uiso 0.50 1 d PR . . C17 C 0.5331(5) 0.6168(8) 0.2846(8) 0.058(3) Uani 0.50 1 d P . . H17A H 0.5486 0.6001 0.3393 0.070 Uiso 0.50 1 d PR . . H17B H 0.5584 0.5985 0.2737 0.070 Uiso 0.50 1 d PR . . C18 C 0.3204(2) 0.6058(4) 0.1308(3) 0.0462(13) Uani 1 1 d . . . H18 H 0.3477 0.5647 0.1409 0.055 Uiso 1 1 calc R . . C19 C 0.3226(2) 0.7051(4) 0.1171(3) 0.0489(13) Uani 1 1 d . . . H19 H 0.3512 0.7293 0.1187 0.059 Uiso 1 1 calc R . . C20 C 0.2824(2) 0.7689(4) 0.1009(3) 0.0394(12) Uani 1 1 d . . . C21 C 0.2421(2) 0.7282(4) 0.1019(3) 0.0411(12) Uani 1 1 d . . . H21 H 0.2147 0.7681 0.0931 0.049 Uiso 1 1 calc R . . C22 C 0.2421(2) 0.6282(4) 0.1158(3) 0.0403(12) Uani 1 1 d . . . H22 H 0.2141 0.6026 0.1152 0.048 Uiso 1 1 calc R . . C28 C 0.2389(2) 0.9911(4) 0.2380(3) 0.0431(12) Uani 1 1 d . . . H28 H 0.2097 1.0296 0.2238 0.052 Uiso 1 1 calc R . . C29 C 0.2573(2) 0.9966(4) 0.1919(3) 0.0439(12) Uani 1 1 d . . . H29 H 0.2409 1.0384 0.1482 0.053 Uiso 1 1 calc R . . C25 C 0.30044(19) 0.9398(4) 0.2109(3) 0.0367(11) Uani 1 1 d . . . C26 C 0.32299(19) 0.8809(4) 0.2769(3) 0.0410(12) Uani 1 1 d . . . H26 H 0.3522 0.8416 0.2923 0.049 Uiso 1 1 calc R . . C27 C 0.30286(19) 0.8797(4) 0.3202(3) 0.0410(12) Uani 1 1 d . . . H27 H 0.3193 0.8395 0.3649 0.049 Uiso 1 1 calc R . . C23 C 0.2830(2) 0.8767(4) 0.0838(3) 0.0470(13) Uani 1 1 d . . . H23A H 0.2470 0.9024 0.0546 0.056 Uiso 1 1 calc R . . H23B H 0.2950 0.8832 0.0502 0.056 Uiso 1 1 calc R . . C24 C 0.3190(2) 0.9392(4) 0.1585(3) 0.0442(12) Uani 1 1 d . . . H24A H 0.3549 0.9132 0.1881 0.053 Uiso 1 1 calc R . . H24B H 0.3198 1.0065 0.1432 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0499(5) 0.0175(4) 0.0427(5) 0.000 0.0325(4) 0.000 Ni2 0.0355(3) 0.0304(3) 0.0342(3) -0.0027(2) 0.0226(3) -0.0042(2) N1 0.046(2) 0.043(2) 0.036(2) 0.0071(18) 0.025(2) 0.006(2) N2 0.040(2) 0.038(2) 0.042(2) 0.0044(18) 0.028(2) 0.0008(18) N3 0.038(2) 0.038(2) 0.038(2) 0.0051(18) 0.0223(19) 0.0014(18) N4 0.033(3) 0.021(3) 0.035(3) 0.000 0.017(2) 0.000 N5 0.105(6) 0.018(3) 0.067(4) 0.000 0.068(4) 0.000 N6 0.037(2) 0.037(2) 0.032(2) -0.0015(17) 0.0194(18) -0.0053(18) N7 0.036(2) 0.037(2) 0.034(2) 0.0037(17) 0.0220(18) 0.0040(17) O1 0.054(2) 0.0307(18) 0.0437(19) -0.0023(15) 0.0323(18) -0.0065(15) O2 0.046(2) 0.125(4) 0.044(2) 0.013(2) 0.024(2) -0.010(2) O3 0.050(2) 0.043(2) 0.052(2) -0.0066(17) 0.0372(19) -0.0066(17) O4 0.144(5) 0.042(2) 0.121(4) -0.033(2) 0.116(4) -0.035(3) O5 0.055(2) 0.057(3) 0.059(3) -0.017(2) 0.021(2) 0.007(2) O6 0.0371(18) 0.0388(19) 0.0383(19) -0.0035(15) 0.0193(16) 0.0019(15) O7 0.058(2) 0.0326(19) 0.056(2) -0.0094(16) 0.037(2) -0.0169(16) O8 0.050(2) 0.0376(19) 0.047(2) -0.0064(16) 0.0334(17) -0.0075(16) O9 0.047(2) 0.044(2) 0.0372(19) -0.0100(16) 0.0188(17) -0.0004(16) O10 0.045(2) 0.067(3) 0.130(4) 0.010(3) 0.046(3) 0.011(2) O11 0.045(2) 0.067(3) 0.130(4) 0.010(3) 0.046(3) 0.011(2) O12 0.070(12) 0.103(15) 0.075(12) 0.021(11) 0.048(11) 0.017(11) S1 0.0563(8) 0.0434(7) 0.0435(7) 0.0059(6) 0.0348(7) 0.0100(6) S2 0.0436(7) 0.0508(8) 0.0476(8) 0.0138(6) 0.0275(6) 0.0014(6) S3 0.0508(8) 0.0405(7) 0.0515(8) 0.0002(6) 0.0377(7) 0.0023(6) C1 0.034(3) 0.042(3) 0.024(2) 0.000(2) 0.015(2) -0.002(2) C2 0.035(3) 0.039(3) 0.034(3) -0.006(2) 0.018(2) -0.005(2) C3 0.030(2) 0.046(3) 0.030(2) 0.003(2) 0.014(2) 0.000(2) C4 0.046(3) 0.028(2) 0.043(3) 0.009(2) 0.027(3) 0.003(2) C5 0.051(3) 0.034(3) 0.043(3) -0.003(2) 0.028(3) -0.005(2) C6 0.057(3) 0.044(3) 0.048(3) -0.017(2) 0.037(3) -0.016(3) C7 0.058(3) 0.041(3) 0.054(3) -0.013(2) 0.042(3) -0.012(2) C8 0.041(3) 0.035(3) 0.041(3) 0.000(2) 0.021(2) -0.004(2) C9 0.048(3) 0.038(3) 0.044(3) -0.001(2) 0.023(3) -0.008(2) C10 0.045(3) 0.032(3) 0.052(3) 0.002(2) 0.025(3) 0.004(2) C11 0.086(5) 0.032(3) 0.071(4) 0.014(3) 0.053(4) 0.026(3) C12 0.138(9) 0.017(4) 0.088(7) 0.000 0.091(7) 0.000 C13 0.178(8) 0.025(3) 0.096(5) 0.011(3) 0.115(6) 0.019(4) C14 0.068(8) 0.024(6) 0.052(8) -0.002(5) 0.041(7) 0.002(6) C14' 0.088(10) 0.030(6) 0.067(9) -0.009(6) 0.054(9) 0.003(7) C15 0.064(6) 0.015(4) 0.056(7) -0.005(4) 0.035(6) -0.005(4) C16 0.049(8) 0.020(5) 0.064(9) 0.006(5) 0.028(7) 0.006(4) C17 0.065(8) 0.024(6) 0.066(8) -0.011(6) 0.027(7) -0.008(6) C18 0.041(3) 0.044(3) 0.058(3) -0.001(2) 0.031(3) -0.002(2) C19 0.050(3) 0.048(3) 0.060(3) -0.004(3) 0.038(3) -0.012(3) C20 0.054(3) 0.035(3) 0.033(3) -0.003(2) 0.028(2) -0.009(2) C21 0.049(3) 0.035(3) 0.048(3) -0.001(2) 0.034(3) 0.002(2) C22 0.042(3) 0.039(3) 0.047(3) 0.001(2) 0.030(2) -0.003(2) C28 0.045(3) 0.041(3) 0.045(3) 0.011(2) 0.028(3) 0.013(2) C29 0.051(3) 0.046(3) 0.039(3) 0.009(2) 0.029(3) 0.005(2) C25 0.040(3) 0.036(3) 0.039(3) -0.010(2) 0.026(2) -0.014(2) C26 0.032(3) 0.049(3) 0.042(3) 0.003(2) 0.021(2) 0.004(2) C27 0.035(3) 0.047(3) 0.036(3) 0.007(2) 0.018(2) 0.008(2) C23 0.073(4) 0.037(3) 0.042(3) -0.004(2) 0.040(3) -0.012(3) C24 0.057(3) 0.038(3) 0.051(3) -0.007(2) 0.039(3) -0.014(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 Ni1 O1 2.078(3) . ? Ni1 O1 2.078(3) 2_655 ? Ni1 N5 2.091(5) 1_545 ? Ni1 N4 2.093(5) . ? Ni1 O7 2.094(4) 2_655 ? Ni1 O7 2.094(4) . ? Ni2 O6 2.058(3) 6_566 ? Ni2 O9 2.077(3) . ? Ni2 N7 2.081(4) 4_545 ? Ni2 N6 2.094(4) . ? Ni2 O8 2.097(3) . ? Ni2 O3 2.100(3) . ? N1 C1 1.331(6) . ? N1 C3 1.352(6) . ? N2 C1 1.336(6) . ? N2 C2 1.342(6) . ? N3 C3 1.324(6) . ? N3 C2 1.343(6) . ? N4 C10 1.331(6) 2_655 ? N4 C10 1.331(6) . ? N5 C13 1.334(6) . ? N5 C13 1.334(6) 2_655 ? N5 Ni1 2.091(5) 1_565 ? N6 C18 1.338(6) . ? N6 C22 1.345(6) . ? N7 C28 1.336(6) . ? N7 C27 1.340(6) . ? N7 Ni2 2.081(4) 4 ? O1 C4 1.253(6) . ? O2 C4 1.234(6) . ? O3 C6 1.250(6) . ? O4 C6 1.265(7) . ? O5 C8 1.262(6) . ? O6 C8 1.246(6) . ? O6 Ni2 2.058(3) 6_565 ? O7 H7D 0.8500 . ? O7 H7E 0.8499 . ? O8 H8B 0.8501 . ? O8 H8C 0.8502 . ? O9 H9E 0.8499 . ? O9 H9F 0.8500 . ? O10 H10C 0.8500 . ? O10 H10D 0.8503 . ? O11 H11C 0.8500 . ? O11 H11D 0.8499 . ? O12 H12C 0.8499 . ? O12 H12D 0.8499 . ? S1 C1 1.753(5) . ? S1 C5 1.798(5) . ? S2 C3 1.735(5) . ? S2 C9 1.786(6) . ? S3 C2 1.750(5) . ? S3 C7 1.799(5) . ? C4 C5 1.525(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.516(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.530(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.372(7) . ? C10 H10 0.9300 . ? C11 C12 1.377(8) . ? C11 H11 0.9300 . ? C12 C11 1.377(8) 2_655 ? C12 C16 1.564(12) 2_655 ? C12 C16 1.564(12) . ? C13 C14 1.393(13) . ? C13 C14' 1.478(15) . ? C13 H13 0.9300 . ? C14 C15 1.395(16) . ? C14 C15 1.924(17) 2_655 ? C14 H14 0.9300 . ? C14' C15 1.388(17) 2_655 ? C14' C15 1.504(18) . ? C14' H14' 0.9300 . ? C15 C15 1.17(2) 2_655 ? C15 C14' 1.388(17) 2_655 ? C15 C17 1.508(14) . ? C15 C14 1.924(17) 2_655 ? C16 C17 0.859(12) 2_655 ? C16 C16 0.92(2) 2_655 ? C16 C17 1.511(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C16 0.859(12) 2_655 ? C17 C17 1.68(2) 2_655 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.382(7) . ? C18 H18 0.9300 . ? C19 C20 1.387(8) . ? C19 H19 0.9300 . ? C20 C21 1.378(7) . ? C20 C23 1.503(7) . ? C21 C22 1.382(7) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C28 C29 1.381(7) . ? C28 H28 0.9300 . ? C29 C25 1.384(7) . ? C29 H29 0.9300 . ? C25 C26 1.374(7) . ? C25 C24 1.506(7) . ? C26 C27 1.367(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C23 C24 1.531(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 O1 Ni1 O1 178.54(18) . 2_655 ? O1 Ni1 N5 89.27(9) . 1_545 ? O1 Ni1 N5 89.27(9) 2_655 1_545 ? O1 Ni1 N4 90.73(9) . . ? O1 Ni1 N4 90.73(9) 2_655 . ? N5 Ni1 N4 180.000(1) 1_545 . ? O1 Ni1 O7 91.87(14) . 2_655 ? O1 Ni1 O7 88.10(14) 2_655 2_655 ? N5 Ni1 O7 88.79(9) 1_545 2_655 ? N4 Ni1 O7 91.21(9) . 2_655 ? O1 Ni1 O7 88.10(14) . . ? O1 Ni1 O7 91.87(14) 2_655 . ? N5 Ni1 O7 88.79(9) 1_545 . ? N4 Ni1 O7 91.21(9) . . ? O7 Ni1 O7 177.59(19) 2_655 . ? O6 Ni2 O9 175.96(14) 6_566 . ? O6 Ni2 N7 91.35(14) 6_566 4_545 ? O9 Ni2 N7 92.69(15) . 4_545 ? O6 Ni2 N6 90.62(14) 6_566 . ? O9 Ni2 N6 89.12(14) . . ? N7 Ni2 N6 92.08(16) 4_545 . ? O6 Ni2 O8 92.30(13) 6_566 . ? O9 Ni2 O8 88.10(14) . . ? N7 Ni2 O8 85.96(14) 4_545 . ? N6 Ni2 O8 176.52(15) . . ? O6 Ni2 O3 87.92(14) 6_566 . ? O9 Ni2 O3 88.06(14) . . ? N7 Ni2 O3 176.48(15) 4_545 . ? N6 Ni2 O3 91.37(15) . . ? O8 Ni2 O3 90.63(14) . . ? C1 N1 C3 113.5(4) . . ? C1 N2 C2 113.4(4) . . ? C3 N3 C2 114.0(4) . . ? C10 N4 C10 116.1(6) 2_655 . ? C10 N4 Ni1 121.9(3) 2_655 . ? C10 N4 Ni1 121.9(3) . . ? C13 N5 C13 117.6(7) . 2_655 ? C13 N5 Ni1 121.2(3) . 1_565 ? C13 N5 Ni1 121.2(3) 2_655 1_565 ? C18 N6 C22 116.5(4) . . ? C18 N6 Ni2 121.9(3) . . ? C22 N6 Ni2 121.3(3) . . ? C28 N7 C27 116.1(4) . . ? C28 N7 Ni2 121.6(3) . 4 ? C27 N7 Ni2 121.8(3) . 4 ? C4 O1 Ni1 129.3(3) . . ? C6 O3 Ni2 129.9(3) . . ? C8 O6 Ni2 126.4(3) . 6_565 ? Ni1 O7 H7D 103.1 . . ? Ni1 O7 H7E 103.0 . . ? H7D O7 H7E 105.2 . . ? Ni2 O8 H8B 106.6 . . ? Ni2 O8 H8C 106.5 . . ? H8B O8 H8C 106.6 . . ? Ni2 O9 H9E 118.2 . . ? Ni2 O9 H9F 131.7 . . ? H9E O9 H9F 108.3 . . ? H10C O10 H10D 108.2 . . ? H11C O11 H11D 108.0 . . ? H12C O12 H12D 107.9 . . ? C1 S1 C5 102.3(2) . . ? C3 S2 C9 102.7(3) . . ? C2 S3 C7 99.1(2) . . ? N1 C1 N2 126.8(5) . . ? N1 C1 S1 113.8(4) . . ? N2 C1 S1 119.4(4) . . ? N2 C2 N3 126.1(5) . . ? N2 C2 S3 119.2(4) . . ? N3 C2 S3 114.6(4) . . ? N3 C3 N1 126.1(5) . . ? N3 C3 S2 120.9(4) . . ? N1 C3 S2 112.9(4) . . ? O2 C4 O1 126.1(5) . . ? O2 C4 C5 119.5(5) . . ? O1 C4 C5 114.3(4) . . ? C4 C5 S1 115.0(4) . . ? C4 C5 H5A 108.5 . . ? S1 C5 H5A 108.5 . . ? C4 C5 H5B 108.5 . . ? S1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? O3 C6 O4 126.5(5) . . ? O3 C6 C7 119.6(5) . . ? O4 C6 C7 113.8(5) . . ? C6 C7 S3 112.9(4) . . ? C6 C7 H7A 109.0 . . ? S3 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? S3 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O6 C8 O5 125.9(5) . . ? O6 C8 C9 118.7(5) . . ? O5 C8 C9 115.4(5) . . ? C8 C9 S2 116.1(4) . . ? C8 C9 H9A 108.3 . . ? S2 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? S2 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N4 C10 C11 123.5(5) . . ? N4 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 120.4(6) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C11 116.0(7) . 2_655 ? C11 C12 C16 136.8(6) . 2_655 ? C11 C12 C16 106.5(5) 2_655 2_655 ? C11 C12 C16 106.5(5) . . ? C11 C12 C16 136.8(6) 2_655 . ? C16 C12 C16 34.2(7) 2_655 . ? N5 C13 C14 126.7(7) . . ? N5 C13 C14' 116.0(8) . . ? C14 C13 C14' 36.4(6) . . ? N5 C13 H13 116.7 . . ? C14 C13 H13 116.7 . . ? C14' C13 H13 114.1 . . ? C13 C14 C15 116.7(11) . . ? C13 C14 C15 97.6(9) . 2_655 ? C15 C14 C15 37.1(8) . 2_655 ? C13 C14 H14 121.7 . . ? C15 C14 H14 121.7 . . ? C15 C14 H14 129.3 2_655 . ? C15 C14' C13 123.1(10) 2_655 . ? C15 C14' C15 47.4(9) 2_655 . ? C13 C14' C15 105.4(11) . . ? C15 C14' H14' 95.8 2_655 . ? C13 C14' H14' 127.3 . . ? C15 C14' H14' 127.3 . . ? C15 C15 C14' 71.5(12) 2_655 2_655 ? C15 C15 C14 96.9(12) 2_655 . ? C14' C15 C14 116.2(8) 2_655 . ? C15 C15 C14' 61.0(10) 2_655 . ? C14' C15 C14' 103.6(11) 2_655 . ? C14 C15 C14' 35.9(7) . . ? C15 C15 C17 99.8(6) 2_655 . ? C14' C15 C17 121.0(11) 2_655 . ? C14 C15 C17 122.7(11) . . ? C14' C15 C17 123.0(10) . . ? C15 C15 C14 46.1(9) 2_655 2_655 ? C14' C15 C14 25.5(7) 2_655 2_655 ? C14 C15 C14 111.2(10) . 2_655 ? C14' C15 C14 86.2(7) . 2_655 ? C17 C15 C14 119.7(9) . 2_655 ? C17 C16 C16 116.3(11) 2_655 2_655 ? C17 C16 C17 85.7(15) 2_655 . ? C16 C16 C17 30.6(5) 2_655 . ? C17 C16 C12 170.5(14) 2_655 . ? C16 C16 C12 72.9(4) 2_655 . ? C17 C16 C12 103.5(7) . . ? C17 C16 H16A 66.8 2_655 . ? C16 C16 H16A 124.4 2_655 . ? C17 C16 H16A 111.6 . . ? C12 C16 H16A 110.7 . . ? C17 C16 H16B 63.1 2_655 . ? C16 C16 H16B 121.6 2_655 . ? C17 C16 H16B 111.3 . . ? C12 C16 H16B 110.7 . . ? H16A C16 H16B 108.9 . . ? C16 C17 C15 143.8(16) 2_655 . ? C16 C17 C16 33.1(10) 2_655 . ? C15 C17 C16 110.8(9) . . ? C16 C17 C17 63.7(11) 2_655 2_655 ? C15 C17 C17 80.2(6) . 2_655 ? C16 C17 C17 30.6(5) . 2_655 ? C16 C17 H17A 90.3 2_655 . ? C15 C17 H17A 109.4 . . ? C16 C17 H17A 109.8 . . ? C17 C17 H17A 121.3 2_655 . ? C16 C17 H17B 91.9 2_655 . ? C15 C17 H17B 109.3 . . ? C16 C17 H17B 109.6 . . ? C17 C17 H17B 123.5 2_655 . ? H17A C17 H17B 107.9 . . ? N6 C18 C19 123.1(5) . . ? N6 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C18 C19 C20 120.5(5) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 116.3(5) . . ? C21 C20 C23 122.0(5) . . ? C19 C20 C23 121.6(5) . . ? C20 C21 C22 120.3(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? N6 C22 C21 123.2(5) . . ? N6 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N7 C28 C29 123.4(5) . . ? N7 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C28 C29 C25 119.9(5) . . ? C28 C29 H29 120.0 . . ? C25 C29 H29 120.0 . . ? C26 C25 C29 116.4(5) . . ? C26 C25 C24 122.5(5) . . ? C29 C25 C24 120.9(5) . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N7 C27 C26 123.6(5) . . ? N7 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C20 C23 C24 113.3(4) . . ? C20 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C20 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 112.3(4) . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.699 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.085 #===END