# Electronic Supplementary Material (ESI) for CrystEngComm # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 Co2 N6 O15 S2' _chemical_formula_weight 1182.98 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' Co Co 0.3494 0.9721 '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' 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 12.1624(9) _cell_length_b 13.1051(13) _cell_length_c 17.8595(16) _cell_angle_alpha 106.905(5) _cell_angle_beta 94.129(2) _cell_angle_gamma 97.344(4) _cell_volume 2683.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.8934 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17467 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9126 _reflns_number_gt 6434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+1.3800P] 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 9126 _refine_ls_number_parameters 686 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Co1 Co 0.19482(4) -0.13232(4) 0.32631(3) 0.02358(17) Uani 1 1 d . . . Co2 Co 0.12843(4) 0.05867(4) 0.22784(3) 0.02338(17) Uani 1 1 d . . . S2 S 0.82991(8) 0.29968(8) 0.41725(7) 0.0304(3) Uani 1 1 d . . . S1 S 0.41353(10) -0.39734(9) -0.12952(6) 0.0356(3) Uani 1 1 d . . . O5 O 0.0954(2) -0.0144(2) 0.31907(16) 0.0263(6) Uani 1 1 d . . . H5A H 0.1161 0.0492 0.3552 0.032 Uiso 1 1 d R . . H5B H 0.0221 -0.0264 0.3156 0.032 Uiso 1 1 d R . . O4 O 0.2979(2) 0.0901(2) 0.26797(18) 0.0349(7) Uani 1 1 d . . . O3 O 0.3298(2) -0.0074(2) 0.34986(19) 0.0366(8) Uani 1 1 d . . . O15 O 0.8846(3) 0.7893(2) 0.68981(17) 0.0318(7) Uani 1 1 d . . . O10 O -0.0499(3) -0.7472(2) -0.30951(19) 0.0391(8) Uani 1 1 d . . . O6 O 0.1838(3) -0.0911(2) 0.44803(18) 0.0422(8) Uani 1 1 d . . . H6B H 0.2156 -0.0336 0.4797 0.051 Uiso 1 1 d R . . H6A H 0.1503 -0.1303 0.4721 0.051 Uiso 1 1 d R . . O1 O 0.2050(3) -0.1869(3) 0.20787(18) 0.0428(8) Uani 1 1 d . . . O13 O 0.8845(2) 0.2409(2) 0.4615(2) 0.0448(9) Uani 1 1 d . . . O11 O 0.0786(3) -0.8574(3) -0.3331(2) 0.0484(9) Uani 1 1 d . . . O2 O 0.1467(3) -0.0810(2) 0.14049(18) 0.0368(7) Uani 1 1 d . . . O14 O 0.8490(3) 0.8302(2) 0.57850(18) 0.0423(8) Uani 1 1 d . . . O12 O 0.8671(3) 0.3063(3) 0.3436(2) 0.0448(9) Uani 1 1 d . . . O9 O 0.5021(3) -0.4446(3) -0.1015(2) 0.0453(9) Uani 1 1 d . . . O8 O 0.4370(3) -0.3254(3) -0.1761(2) 0.0542(10) Uani 1 1 d . . . N5 N 0.3054(3) -0.2436(3) 0.3353(2) 0.0296(8) Uani 1 1 d . . . N1 N -0.0492(3) 0.0236(3) 0.1934(2) 0.0285(8) Uani 1 1 d . . . N3 N 0.1523(3) 0.1531(3) 0.1471(2) 0.0309(8) Uani 1 1 d . . . N6 N 0.5346(3) -0.4896(3) 0.4285(2) 0.0341(9) Uani 1 1 d . . . N2 N -0.4349(3) 0.0084(3) 0.0731(2) 0.0391(9) Uani 1 1 d . . . N4 N 0.0674(3) 0.4184(3) 0.0022(2) 0.0399(10) Uani 1 1 d . . . C22 C 0.8404(3) 0.4342(3) 0.4787(2) 0.0261(9) Uani 1 1 d . . . C28 C 0.8657(3) 0.7649(3) 0.6160(3) 0.0271(9) Uani 1 1 d . . . C26 C 0.8409(4) 0.6197(3) 0.4877(3) 0.0302(10) Uani 1 1 d . . . H26 H 0.8360 0.6731 0.4633 0.036 Uiso 1 1 calc R . . C7 C 0.2304(4) -0.2000(4) 0.0053(3) 0.0338(10) Uani 1 1 d . . . H7 H 0.1848 -0.1504 -0.0007 0.041 Uiso 1 1 calc R . . C19 C 0.6869(3) 0.2422(3) 0.3955(3) 0.0272(9) Uani 1 1 d . . . C27 C 0.8292(4) 0.5130(3) 0.4423(3) 0.0320(10) Uani 1 1 d . . . H27 H 0.8139 0.4942 0.3878 0.038 Uiso 1 1 calc R . . C13 C 0.2104(4) -0.4823(4) -0.2190(3) 0.0357(11) Uani 1 1 d . . . H13 H 0.2015 -0.4115 -0.2149 0.043 Uiso 1 1 calc R . . C5 C 0.3485(4) -0.3282(3) -0.0484(2) 0.0310(10) Uani 1 1 d . . . C2 C 0.2468(3) -0.2201(3) 0.0784(2) 0.0257(9) Uani 1 1 d . . . C16 C 0.4715(3) 0.1310(3) 0.3479(2) 0.0265(9) Uani 1 1 d . . . C11 C 0.1415(4) -0.6721(3) -0.2694(2) 0.0301(10) Uani 1 1 d . . . C24 C 0.8716(4) 0.5688(3) 0.6035(3) 0.0316(10) Uani 1 1 d . . . H24 H 0.8855 0.5880 0.6581 0.038 Uiso 1 1 calc R . . C8 C 0.3075(4) -0.5043(3) -0.1850(2) 0.0322(10) Uani 1 1 d . . . C4 C 0.3657(4) -0.3505(3) 0.0227(2) 0.0312(10) Uani 1 1 d . . . H4 H 0.4105 -0.4009 0.0282 0.037 Uiso 1 1 calc R . . C18 C 0.6424(4) 0.1727(4) 0.4351(3) 0.0382(11) Uani 1 1 d . . . H18 H 0.6846 0.1628 0.4772 0.046 Uiso 1 1 calc R . . C15 C 0.3562(3) 0.0670(3) 0.3192(2) 0.0246(9) Uani 1 1 d . . . C21 C 0.5160(3) 0.2039(3) 0.3104(3) 0.0288(9) Uani 1 1 d . . . H21 H 0.4732 0.2151 0.2690 0.035 Uiso 1 1 calc R . . C20 C 0.6226(3) 0.2594(3) 0.3341(3) 0.0297(10) Uani 1 1 d . . . H20 H 0.6515 0.3083 0.3091 0.036 Uiso 1 1 calc R . . C14 C 0.0487(4) -0.7672(4) -0.3081(3) 0.0338(10) Uani 1 1 d . . . C1 C 0.1955(4) -0.1573(3) 0.1480(2) 0.0293(10) Uani 1 1 d . . . C49 C 0.2780(4) -0.3498(4) 0.3043(3) 0.0402(12) Uani 1 1 d . . . H49 H 0.2064 -0.3774 0.2786 0.048 Uiso 1 1 calc R . . C23 C 0.8636(3) 0.4603(3) 0.5593(3) 0.0291(9) Uani 1 1 d . . . H23 H 0.8736 0.4077 0.5835 0.035 Uiso 1 1 calc R . . C3 C 0.3130(4) -0.2941(4) 0.0859(3) 0.0333(10) Uani 1 1 d . . . H3 H 0.3234 -0.3075 0.1341 0.040 Uiso 1 1 calc R . . C40 C -0.2810(4) -0.0160(4) 0.1576(3) 0.0389(11) Uani 1 1 d . . . C25 C 0.8596(3) 0.6482(3) 0.5684(2) 0.0249(9) Uani 1 1 d . . . C6 C 0.2818(4) -0.2540(4) -0.0571(3) 0.0355(11) Uani 1 1 d . . . H6 H 0.2717 -0.2403 -0.1052 0.043 Uiso 1 1 calc R . . C12 C 0.1271(4) -0.5667(3) -0.2588(3) 0.0339(10) Uani 1 1 d . . . H12 H 0.0602 -0.5520 -0.2789 0.041 Uiso 1 1 calc R . . C10 C 0.2414(4) -0.6926(4) -0.2389(3) 0.0423(12) Uani 1 1 d . . . H10 H 0.2535 -0.7635 -0.2476 0.051 Uiso 1 1 calc R . . C32 C 0.0828(4) 0.2134(5) 0.0424(3) 0.0504(14) Uani 1 1 d . . . H32 H 0.0287 0.2028 0.0002 0.061 Uiso 1 1 calc R . . C17 C 0.5349(4) 0.1186(4) 0.4113(3) 0.0368(11) Uani 1 1 d . . . H17 H 0.5045 0.0729 0.4383 0.044 Uiso 1 1 calc R . . C31 C 0.1669(4) 0.3011(4) 0.0615(3) 0.0395(11) Uani 1 1 d . . . C47 C 0.4586(4) -0.3825(4) 0.3455(3) 0.0340(10) Uani 1 1 d . . . C48 C 0.3511(5) -0.4220(4) 0.3085(3) 0.0442(12) Uani 1 1 d . . . H48 H 0.3279 -0.4959 0.2867 0.053 Uiso 1 1 calc R . . C36 C 0.0709(5) 0.4728(5) -0.0589(3) 0.0493(14) Uani 1 1 d . . . H36A H 0.0888 0.4241 -0.1072 0.059 Uiso 1 1 calc R . . H36B H 0.1290 0.5354 -0.0422 0.059 Uiso 1 1 calc R . . C51 C 0.5559(4) -0.3987(4) 0.5007(3) 0.0361(11) Uani 1 1 d . . . H51A H 0.4945 -0.3576 0.5050 0.043 Uiso 1 1 calc R . . H51B H 0.6236 -0.3514 0.4998 0.043 Uiso 1 1 calc R . . C52 C 0.4318(4) -0.5581(4) 0.4296(3) 0.0360(11) Uani 1 1 d . . . H52A H 0.4158 -0.6176 0.3811 0.043 Uiso 1 1 calc R . . H52B H 0.3703 -0.5171 0.4340 0.043 Uiso 1 1 calc R . . C41 C -0.2238(4) 0.0873(4) 0.1936(3) 0.0398(11) Uani 1 1 d . . . H41 H -0.2626 0.1456 0.2063 0.048 Uiso 1 1 calc R . . C35 C 0.0383(5) 0.4927(4) 0.0739(3) 0.0462(13) Uani 1 1 d . . . H35A H 0.0959 0.5556 0.0924 0.055 Uiso 1 1 calc R . . H35B H 0.0345 0.4574 0.1146 0.055 Uiso 1 1 calc R . . C50 C 0.5410(4) -0.4567(4) 0.3573(3) 0.0419(12) Uani 1 1 d . . . H50A H 0.5285 -0.5210 0.3121 0.050 Uiso 1 1 calc R . . H50B H 0.6161 -0.4202 0.3587 0.050 Uiso 1 1 calc R . . C9 C 0.3225(4) -0.6095(4) -0.1961(3) 0.0426(12) Uani 1 1 d . . . H9 H 0.3881 -0.6244 -0.1744 0.051 Uiso 1 1 calc R . . C37 C -0.1094(4) 0.1038(4) 0.2107(3) 0.0358(11) Uani 1 1 d . . . H37 H -0.0727 0.1737 0.2353 0.043 Uiso 1 1 calc R . . C46 C 0.4889(4) -0.2720(4) 0.3742(3) 0.0469(13) Uani 1 1 d . . . H46 H 0.5613 -0.2420 0.3974 0.056 Uiso 1 1 calc R . . C42 C -0.4065(4) -0.0325(5) 0.1375(3) 0.0477(13) Uani 1 1 d . . . H42A H -0.4359 -0.1088 0.1231 0.057 Uiso 1 1 calc R . . H42B H -0.4402 0.0046 0.1833 0.057 Uiso 1 1 calc R . . C44 C -0.5521(4) 0.0269(5) 0.0702(3) 0.0496(13) Uani 1 1 d . . . H44A H -0.5626 0.0799 0.1189 0.059 Uiso 1 1 calc R . . H44B H -0.6006 -0.0399 0.0657 0.059 Uiso 1 1 calc R . . C43 C -0.4157(4) -0.0666(4) -0.0013(3) 0.0475(13) Uani 1 1 d . . . H43A H -0.4592 -0.1368 -0.0084 0.057 Uiso 1 1 calc R . . H43B H -0.3375 -0.0747 0.0002 0.057 Uiso 1 1 calc R . . C39 C -0.2181(4) -0.0982(4) 0.1407(3) 0.0490(14) Uani 1 1 d . . . H39 H -0.2533 -0.1689 0.1172 0.059 Uiso 1 1 calc R . . C29 C 0.2333(4) 0.2377(4) 0.1651(3) 0.0430(12) Uani 1 1 d . . . H29 H 0.2857 0.2476 0.2082 0.052 Uiso 1 1 calc R . . C34 C 0.1749(5) 0.3814(5) 0.0159(4) 0.0520(14) Uani 1 1 d . . . H34A H 0.2300 0.4434 0.0445 0.062 Uiso 1 1 calc R . . H34B H 0.2005 0.3487 -0.0345 0.062 Uiso 1 1 calc R . . C33 C 0.0787(4) 0.1423(4) 0.0849(3) 0.0443(13) Uani 1 1 d . . . H33 H 0.0218 0.0833 0.0700 0.053 Uiso 1 1 calc R . . C30 C 0.2438(4) 0.3112(4) 0.1239(3) 0.0477(13) Uani 1 1 d . . . H30 H 0.3033 0.3678 0.1384 0.057 Uiso 1 1 calc R . . C45 C 0.4108(4) -0.2064(4) 0.3683(3) 0.0428(12) Uani 1 1 d . . . H45 H 0.4325 -0.1320 0.3885 0.051 Uiso 1 1 calc R . . C38 C -0.1050(3) -0.0776(2) 0.15792(19) 0.0444(12) Uani 1 1 d . . . H38 H -0.0647 -0.1348 0.1450 0.053 Uiso 1 1 calc R . . O16 O 0.2334(3) 0.1148(2) 0.55115(19) 0.0616(11) Uiso 1 1 d R . . H16B H 0.1682 0.1339 0.5566 0.074 Uiso 1 1 d R . . H16A H 0.2689 0.1572 0.5297 0.074 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0241(3) 0.0197(3) 0.0262(3) 0.0073(2) -0.0008(2) 0.0022(2) Co2 0.0231(3) 0.0207(3) 0.0243(3) 0.0052(2) -0.0037(2) 0.0031(2) S2 0.0196(5) 0.0203(5) 0.0431(6) -0.0015(5) 0.0020(5) 0.0005(4) S1 0.0343(7) 0.0344(6) 0.0291(6) 0.0000(5) 0.0103(5) -0.0085(5) O5 0.0197(15) 0.0224(14) 0.0325(15) 0.0039(12) -0.0002(12) 0.0002(11) O4 0.0268(17) 0.0407(18) 0.0373(17) 0.0172(15) -0.0043(14) -0.0027(13) O3 0.0281(17) 0.0315(17) 0.0517(19) 0.0214(15) -0.0081(15) -0.0034(13) O15 0.0388(18) 0.0247(15) 0.0262(15) 0.0002(13) -0.0026(13) 0.0058(13) O10 0.0326(19) 0.0300(17) 0.0475(19) 0.0045(15) 0.0044(15) -0.0043(14) O6 0.065(2) 0.0303(17) 0.0283(16) 0.0081(14) -0.0014(16) 0.0031(15) O1 0.071(2) 0.0368(18) 0.0266(16) 0.0099(15) 0.0141(16) 0.0240(17) O13 0.0221(17) 0.0270(17) 0.079(3) 0.0097(17) -0.0114(16) 0.0045(13) O11 0.037(2) 0.0288(18) 0.066(2) -0.0042(16) 0.0108(17) -0.0046(14) O2 0.0433(19) 0.0331(17) 0.0317(16) 0.0044(14) -0.0011(14) 0.0134(15) O14 0.069(2) 0.0229(16) 0.0301(16) 0.0027(14) -0.0046(16) 0.0068(15) O12 0.0352(19) 0.0343(18) 0.050(2) -0.0096(15) 0.0180(16) -0.0033(14) O9 0.0256(18) 0.053(2) 0.046(2) -0.0016(17) 0.0028(15) 0.0045(15) O8 0.068(3) 0.046(2) 0.0395(19) 0.0077(16) 0.0203(18) -0.0213(18) N5 0.032(2) 0.0270(19) 0.0345(19) 0.0146(16) -0.0032(16) 0.0124(15) N1 0.0269(19) 0.0286(19) 0.0258(18) 0.0035(15) -0.0041(15) 0.0037(15) N3 0.033(2) 0.0301(19) 0.0307(19) 0.0118(16) -0.0020(16) 0.0058(15) N6 0.029(2) 0.039(2) 0.040(2) 0.0162(18) 0.0110(17) 0.0160(17) N2 0.0189(19) 0.049(2) 0.045(2) 0.010(2) -0.0065(17) 0.0026(17) N4 0.046(3) 0.048(2) 0.042(2) 0.031(2) 0.0152(19) 0.0180(19) C22 0.018(2) 0.022(2) 0.032(2) 0.0015(18) 0.0012(17) -0.0016(16) C28 0.025(2) 0.022(2) 0.034(2) 0.0067(18) -0.0015(18) 0.0075(17) C26 0.033(2) 0.024(2) 0.034(2) 0.0106(19) 0.0009(19) 0.0032(18) C7 0.043(3) 0.029(2) 0.028(2) 0.0073(19) -0.002(2) 0.0067(19) C19 0.019(2) 0.021(2) 0.036(2) 0.0019(18) 0.0016(18) 0.0006(16) C27 0.041(3) 0.025(2) 0.026(2) 0.0034(18) 0.0026(19) 0.0020(18) C13 0.047(3) 0.024(2) 0.034(2) 0.0063(19) 0.008(2) 0.000(2) C5 0.034(3) 0.027(2) 0.025(2) 0.0020(18) 0.0057(18) -0.0070(18) C2 0.028(2) 0.022(2) 0.024(2) 0.0051(17) -0.0008(17) 0.0000(17) C16 0.023(2) 0.023(2) 0.032(2) 0.0072(18) 0.0001(18) 0.0012(16) C11 0.027(2) 0.029(2) 0.029(2) 0.0041(19) 0.0031(18) -0.0044(18) C24 0.033(3) 0.030(2) 0.029(2) 0.0052(19) -0.0011(19) 0.0047(18) C8 0.031(3) 0.031(2) 0.027(2) 0.0010(19) 0.0094(19) -0.0065(19) C4 0.036(3) 0.028(2) 0.029(2) 0.0050(19) 0.0035(19) 0.0091(19) C18 0.031(3) 0.037(3) 0.046(3) 0.020(2) -0.012(2) -0.003(2) C15 0.019(2) 0.023(2) 0.031(2) 0.0077(18) -0.0032(17) 0.0036(16) C21 0.025(2) 0.030(2) 0.035(2) 0.0151(19) -0.0009(18) 0.0079(18) C20 0.027(2) 0.025(2) 0.036(2) 0.0100(19) 0.0037(19) -0.0031(17) C14 0.032(3) 0.029(2) 0.036(2) 0.006(2) 0.007(2) -0.0034(19) C1 0.029(2) 0.025(2) 0.028(2) 0.0031(18) 0.0013(18) -0.0009(18) C49 0.034(3) 0.037(3) 0.047(3) 0.014(2) -0.004(2) -0.001(2) C23 0.025(2) 0.024(2) 0.038(2) 0.0089(19) -0.0007(19) 0.0035(17) C3 0.040(3) 0.036(2) 0.024(2) 0.0099(19) 0.0051(19) 0.006(2) C40 0.027(3) 0.051(3) 0.040(3) 0.020(2) -0.006(2) 0.001(2) C25 0.019(2) 0.021(2) 0.030(2) 0.0023(17) -0.0005(17) 0.0012(16) C6 0.047(3) 0.035(2) 0.023(2) 0.0103(19) -0.003(2) 0.000(2) C12 0.031(3) 0.033(2) 0.033(2) 0.006(2) 0.0058(19) -0.0032(19) C10 0.041(3) 0.028(2) 0.056(3) 0.012(2) 0.003(2) 0.001(2) C32 0.041(3) 0.071(4) 0.049(3) 0.039(3) -0.006(2) -0.001(3) C17 0.030(3) 0.037(3) 0.046(3) 0.025(2) -0.008(2) -0.006(2) C31 0.029(3) 0.049(3) 0.052(3) 0.030(3) 0.011(2) 0.011(2) C47 0.037(3) 0.044(3) 0.033(2) 0.023(2) 0.010(2) 0.022(2) C48 0.064(4) 0.027(2) 0.042(3) 0.008(2) 0.001(3) 0.015(2) C36 0.060(4) 0.059(3) 0.047(3) 0.035(3) 0.022(3) 0.022(3) C51 0.030(3) 0.036(3) 0.046(3) 0.015(2) 0.008(2) 0.0120(19) C52 0.040(3) 0.033(2) 0.036(2) 0.007(2) 0.006(2) 0.016(2) C41 0.033(3) 0.041(3) 0.042(3) 0.007(2) -0.001(2) 0.011(2) C35 0.053(3) 0.055(3) 0.040(3) 0.029(3) 0.007(2) 0.009(3) C50 0.045(3) 0.055(3) 0.040(3) 0.024(2) 0.016(2) 0.030(2) C9 0.031(3) 0.038(3) 0.055(3) 0.012(2) 0.002(2) 0.000(2) C37 0.032(3) 0.032(2) 0.035(2) -0.001(2) -0.003(2) 0.0057(19) C46 0.037(3) 0.047(3) 0.062(3) 0.025(3) 0.000(2) 0.006(2) C42 0.026(3) 0.060(3) 0.055(3) 0.021(3) -0.008(2) -0.001(2) C44 0.026(3) 0.068(4) 0.047(3) 0.008(3) -0.006(2) 0.007(2) C43 0.036(3) 0.047(3) 0.048(3) 0.000(2) -0.011(2) 0.007(2) C39 0.038(3) 0.034(3) 0.067(4) 0.011(3) -0.011(3) -0.007(2) C29 0.037(3) 0.044(3) 0.049(3) 0.021(2) -0.005(2) -0.003(2) C34 0.047(3) 0.061(4) 0.071(4) 0.048(3) 0.017(3) 0.021(3) C33 0.042(3) 0.053(3) 0.035(3) 0.019(2) -0.010(2) -0.011(2) C30 0.046(3) 0.041(3) 0.058(3) 0.023(3) 0.004(3) -0.005(2) C45 0.037(3) 0.030(2) 0.060(3) 0.017(2) -0.010(2) 0.001(2) C38 0.041(3) 0.027(2) 0.061(3) 0.010(2) -0.008(2) 0.006(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 Co1 O1 2.045(3) . ? Co1 O3 2.089(3) . ? Co1 O6 2.101(3) . ? Co1 O5 2.107(3) . ? Co1 N5 2.136(3) . ? Co1 O10 2.151(3) 2_545 ? Co2 O2 2.080(3) . ? Co2 O4 2.082(3) . ? Co2 O15 2.137(3) 2_666 ? Co2 O5 2.153(3) . ? Co2 N1 2.156(3) . ? Co2 N3 2.168(4) . ? S2 O13 1.438(3) . ? S2 O12 1.444(4) . ? S2 C22 1.768(4) . ? S2 C19 1.772(4) . ? S1 O9 1.438(4) . ? S1 O8 1.444(3) . ? S1 C5 1.769(4) . ? S1 C8 1.777(4) . ? O5 H5A 0.8856 . ? O5 H5B 0.8796 . ? O4 C15 1.246(5) . ? O3 C15 1.268(5) . ? O15 C28 1.259(5) . ? O15 Co2 2.137(3) 2_666 ? O10 C14 1.260(6) . ? O10 Co1 2.151(3) 2_545 ? O6 H6B 0.8273 . ? O6 H6A 0.8459 . ? O1 C1 1.242(5) . ? O11 C14 1.247(5) . ? O2 C1 1.260(5) . ? O14 C28 1.257(5) . ? N5 C49 1.328(6) . ? N5 C45 1.339(6) . ? N1 C37 1.332(6) . ? N1 C38 1.357(4) . ? N3 C29 1.331(6) . ? N3 C33 1.337(6) . ? N6 C52 1.449(6) . ? N6 C51 1.459(6) . ? N6 C50 1.460(6) . ? N2 C42 1.442(6) . ? N2 C43 1.459(6) . ? N2 C44 1.476(6) . ? N4 C35 1.462(7) . ? N4 C36 1.467(6) . ? N4 C34 1.480(6) . ? C22 C23 1.379(6) . ? C22 C27 1.387(6) . ? C28 C25 1.508(6) . ? C26 C25 1.373(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9300 . ? C7 C6 1.374(6) . ? C7 C2 1.411(6) . ? C7 H7 0.9300 . ? C19 C18 1.387(6) . ? C19 C20 1.390(6) . ? C27 H27 0.9300 . ? C13 C12 1.381(6) . ? C13 C8 1.390(7) . ? C13 H13 0.9300 . ? C5 C6 1.378(7) . ? C5 C4 1.392(6) . ? C2 C3 1.367(6) . ? C2 C1 1.503(6) . ? C16 C17 1.384(6) . ? C16 C21 1.396(6) . ? C16 C15 1.510(5) . ? C11 C12 1.374(6) . ? C11 C10 1.385(7) . ? C11 C14 1.526(6) . ? C24 C25 1.380(6) . ? C24 C23 1.398(6) . ? C24 H24 0.9300 . ? C8 C9 1.372(7) . ? C4 C3 1.403(6) . ? C4 H4 0.9300 . ? C18 C17 1.378(6) . ? C18 H18 0.9300 . ? C21 C20 1.374(6) . ? C21 H21 0.9300 . ? C20 H20 0.9300 . ? C49 C48 1.391(7) . ? C49 H49 0.9300 . ? C23 H23 0.9300 . ? C3 H3 0.9300 . ? C40 C39 1.376(7) . ? C40 C41 1.385(7) . ? C40 C42 1.515(7) . ? C6 H6 0.9300 . ? C12 H12 0.9300 . ? C10 C9 1.370(7) . ? C10 H10 0.9300 . ? C32 C33 1.361(7) . ? C32 C31 1.380(7) . ? C32 H32 0.9300 . ? C17 H17 0.9300 . ? C31 C30 1.367(7) . ? C31 C34 1.505(6) . ? C47 C46 1.380(7) . ? C47 C48 1.385(7) . ? C47 C50 1.527(6) . ? C48 H48 0.9300 . ? C36 C35 1.489(7) 2_565 ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C51 C52 1.515(6) 2_646 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C51 1.515(6) 2_646 ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C41 C37 1.378(7) . ? C41 H41 0.9300 . ? C35 C36 1.489(7) 2_565 ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C9 H9 0.9300 . ? C37 H37 0.9300 . ? C46 C45 1.379(7) . ? C46 H46 0.9300 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C44 C43 1.514(7) 2_455 ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C43 C44 1.514(7) 2_455 ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C39 C38 1.363(6) . ? C39 H39 0.9300 . ? C29 C30 1.372(7) . ? C29 H29 0.9300 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C33 H33 0.9300 . ? C30 H30 0.9300 . ? C45 H45 0.9300 . ? C38 H38 0.9300 . ? O16 H16B 0.8650 . ? O16 H16A 0.8541 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O3 95.28(14) . . ? O1 Co1 O6 174.70(12) . . ? O3 Co1 O6 88.19(13) . . ? O1 Co1 O5 95.01(12) . . ? O3 Co1 O5 85.53(11) . . ? O6 Co1 O5 89.25(12) . . ? O1 Co1 N5 85.33(13) . . ? O3 Co1 N5 90.56(13) . . ? O6 Co1 N5 90.63(13) . . ? O5 Co1 N5 176.10(12) . . ? O1 Co1 O10 88.56(14) . 2_545 ? O3 Co1 O10 175.44(13) . 2_545 ? O6 Co1 O10 88.16(13) . 2_545 ? O5 Co1 O10 91.68(12) . 2_545 ? N5 Co1 O10 92.21(13) . 2_545 ? O2 Co2 O4 92.04(13) . . ? O2 Co2 O15 174.47(12) . 2_666 ? O4 Co2 O15 87.05(12) . 2_666 ? O2 Co2 O5 97.49(12) . . ? O4 Co2 O5 89.97(11) . . ? O15 Co2 O5 87.97(11) 2_666 . ? O2 Co2 N1 89.23(13) . . ? O4 Co2 N1 176.20(13) . . ? O15 Co2 N1 92.02(12) 2_666 . ? O5 Co2 N1 86.31(12) . . ? O2 Co2 N3 90.87(13) . . ? O4 Co2 N3 91.94(13) . . ? O15 Co2 N3 83.72(13) 2_666 . ? O5 Co2 N3 171.36(12) . . ? N1 Co2 N3 91.62(13) . . ? O13 S2 O12 120.2(2) . . ? O13 S2 C22 107.5(2) . . ? O12 S2 C22 106.24(19) . . ? O13 S2 C19 107.9(2) . . ? O12 S2 C19 106.1(2) . . ? C22 S2 C19 108.44(19) . . ? O9 S1 O8 119.8(2) . . ? O9 S1 C5 109.1(2) . . ? O8 S1 C5 107.5(2) . . ? O9 S1 C8 107.7(2) . . ? O8 S1 C8 107.7(2) . . ? C5 S1 C8 103.8(2) . . ? Co1 O5 Co2 114.80(13) . . ? Co1 O5 H5A 114.6 . . ? Co2 O5 H5A 90.0 . . ? Co1 O5 H5B 122.8 . . ? Co2 O5 H5B 103.8 . . ? H5A O5 H5B 105.5 . . ? C15 O4 Co2 134.4(3) . . ? C15 O3 Co1 133.3(3) . . ? C28 O15 Co2 125.9(3) . 2_666 ? C14 O10 Co1 123.8(3) . 2_545 ? Co1 O6 H6B 123.2 . . ? Co1 O6 H6A 126.5 . . ? H6B O6 H6A 110.2 . . ? C1 O1 Co1 140.6(3) . . ? C1 O2 Co2 127.7(3) . . ? C49 N5 C45 116.7(4) . . ? C49 N5 Co1 123.4(3) . . ? C45 N5 Co1 119.7(3) . . ? C37 N1 C38 117.4(4) . . ? C37 N1 Co2 119.2(3) . . ? C38 N1 Co2 123.3(3) . . ? C29 N3 C33 116.0(4) . . ? C29 N3 Co2 120.0(3) . . ? C33 N3 Co2 123.1(3) . . ? C52 N6 C51 109.4(4) . . ? C52 N6 C50 114.7(4) . . ? C51 N6 C50 113.1(4) . . ? C42 N2 C43 110.2(4) . . ? C42 N2 C44 110.9(4) . . ? C43 N2 C44 110.3(4) . . ? C35 N4 C36 108.5(4) . . ? C35 N4 C34 111.9(4) . . ? C36 N4 C34 110.9(4) . . ? C23 C22 C27 121.3(4) . . ? C23 C22 S2 121.4(3) . . ? C27 C22 S2 117.3(3) . . ? O14 C28 O15 125.0(4) . . ? O14 C28 C25 116.9(4) . . ? O15 C28 C25 118.1(4) . . ? C25 C26 C27 120.9(4) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C6 C7 C2 119.9(4) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 S2 119.9(3) . . ? C20 C19 S2 119.6(3) . . ? C26 C27 C22 119.3(4) . . ? C26 C27 H27 120.3 . . ? C22 C27 H27 120.3 . . ? C12 C13 C8 119.3(4) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? C6 C5 C4 121.5(4) . . ? C6 C5 S1 119.4(3) . . ? C4 C5 S1 119.0(3) . . ? C3 C2 C7 119.3(4) . . ? C3 C2 C1 120.6(4) . . ? C7 C2 C1 120.1(4) . . ? C17 C16 C21 118.9(4) . . ? C17 C16 C15 121.0(4) . . ? C21 C16 C15 120.1(4) . . ? C12 C11 C10 118.7(4) . . ? C12 C11 C14 122.6(4) . . ? C10 C11 C14 118.5(4) . . ? C25 C24 C23 121.8(4) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C9 C8 C13 119.6(4) . . ? C9 C8 S1 119.9(4) . . ? C13 C8 S1 120.4(3) . . ? C5 C4 C3 117.6(4) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? O4 C15 O3 126.8(4) . . ? O4 C15 C16 118.2(4) . . ? O3 C15 C16 115.0(3) . . ? C20 C21 C16 120.5(4) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? O11 C14 O10 126.8(4) . . ? O11 C14 C11 116.2(4) . . ? O10 C14 C11 117.0(4) . . ? O1 C1 O2 126.2(4) . . ? O1 C1 C2 115.9(4) . . ? O2 C1 C2 117.9(4) . . ? N5 C49 C48 123.3(4) . . ? N5 C49 H49 118.4 . . ? C48 C49 H49 118.4 . . ? C22 C23 C24 117.7(4) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? C2 C3 C4 121.7(4) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C39 C40 C41 116.7(4) . . ? C39 C40 C42 123.8(5) . . ? C41 C40 C42 119.5(5) . . ? C26 C25 C24 118.9(4) . . ? C26 C25 C28 119.2(4) . . ? C24 C25 C28 121.9(4) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C11 C12 C13 121.1(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C30 C31 C32 116.6(4) . . ? C30 C31 C34 121.3(5) . . ? C32 C31 C34 122.2(5) . . ? C46 C47 C48 117.5(4) . . ? C46 C47 C50 120.1(4) . . ? C48 C47 C50 122.4(4) . . ? C47 C48 C49 119.3(4) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? N4 C36 C35 110.7(4) . 2_565 ? N4 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 2_565 . ? N4 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 2_565 . ? H36A C36 H36B 108.1 . . ? N6 C51 C52 108.8(4) . 2_646 ? N6 C51 H51A 109.9 . . ? C52 C51 H51A 109.9 2_646 . ? N6 C51 H51B 109.9 . . ? C52 C51 H51B 109.9 2_646 . ? H51A C51 H51B 108.3 . . ? N6 C52 C51 109.0(4) . 2_646 ? N6 C52 H52A 109.9 . . ? C51 C52 H52A 109.9 2_646 . ? N6 C52 H52B 109.9 . . ? C51 C52 H52B 109.9 2_646 . ? H52A C52 H52B 108.3 . . ? C37 C41 C40 120.1(5) . . ? C37 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? N4 C35 C36 110.9(4) . 2_565 ? N4 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 2_565 . ? N4 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 2_565 . ? H35A C35 H35B 108.1 . . ? N6 C50 C47 115.3(4) . . ? N6 C50 H50A 108.5 . . ? C47 C50 H50A 108.5 . . ? N6 C50 H50B 108.5 . . ? C47 C50 H50B 108.5 . . ? H50A C50 H50B 107.5 . . ? C10 C9 C8 120.4(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N1 C37 C41 122.7(4) . . ? N1 C37 H37 118.7 . . ? C41 C37 H37 118.7 . . ? C45 C46 C47 119.3(5) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? N2 C42 C40 110.6(4) . . ? N2 C42 H42A 109.5 . . ? C40 C42 H42A 109.5 . . ? N2 C42 H42B 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? N2 C44 C43 111.5(5) . 2_455 ? N2 C44 H44A 109.3 . . ? C43 C44 H44A 109.3 2_455 . ? N2 C44 H44B 109.3 . . ? C43 C44 H44B 109.3 2_455 . ? H44A C44 H44B 108.0 . . ? N2 C43 C44 111.2(4) . 2_455 ? N2 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 2_455 . ? N2 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 2_455 . ? H43A C43 H43B 108.0 . . ? C38 C39 C40 121.0(4) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? N3 C29 C30 123.8(5) . . ? N3 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? N4 C34 C31 112.9(4) . . ? N4 C34 H34A 109.0 . . ? C31 C34 H34A 109.0 . . ? N4 C34 H34B 109.0 . . ? C31 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? N3 C33 C32 123.3(5) . . ? N3 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C31 C30 C29 119.9(5) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? N5 C45 C46 123.8(4) . . ? N5 C45 H45 118.1 . . ? C46 C45 H45 118.1 . . ? N1 C38 C39 122.1(4) . . ? N1 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? H16B O16 H16A 106.6 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.825 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.233 _database_code_depnum_ccdc_archive 'CCDC 963379' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 Cd2 N6 O12 S2' _chemical_formula_weight 1235.87 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' Cd Cd -0.8075 1.2024 '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' 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 11.6947(2) _cell_length_b 12.8790(3) _cell_length_c 17.9851(3) _cell_angle_alpha 82.552(2) _cell_angle_beta 71.924(2) _cell_angle_gamma 72.780(2) _cell_volume 2457.59(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 45241 _cell_measurement_theta_min 2.9540 _cell_measurement_theta_max 29.4440 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8217 _exptl_absorpt_correction_T_max 0.9047 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies,Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Dual, Mo at zero, Atlas' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 91076 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8651 _reflns_number_gt 7683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)' _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+3.9550P] 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 8651 _refine_ls_number_parameters 661 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.002 _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 Cd1 Cd 0.036980(15) 0.403603(13) 0.909167(9) 0.01152(5) Uani 1 1 d . . . Cd2 Cd 0.284675(15) 0.373607(13) 0.743106(9) 0.01119(5) Uani 1 1 d . . . S1 S 0.51598(6) -0.24522(5) 1.00343(4) 0.01932(14) Uani 1 1 d . . . S2 S -0.19431(5) 0.01734(5) 0.62820(3) 0.01284(12) Uani 1 1 d . . . O4 O -0.14638(16) 0.02658(14) 0.54441(10) 0.0179(4) Uani 1 1 d . . . O12 O 0.24113(14) -0.53443(12) 0.86095(9) 0.01152(5) Uani 1 1 d U . . O11 O 0.12810(15) -0.52881(13) 0.98542(10) 0.0181(4) Uani 1 1 d . . . O3 O -0.32706(15) 0.03939(14) 0.66377(10) 0.0177(4) Uani 1 1 d . . . O2 O 0.11505(15) 0.30732(14) 0.73762(10) 0.0175(4) Uani 1 1 d . . . O5 O 0.16268(16) -0.46889(13) 0.71315(10) 0.0179(4) Uani 1 1 d . . . O1 O -0.05463(15) 0.32934(13) 0.84232(9) 0.0161(4) Uani 1 1 d . . . O6 O -0.00404(16) -0.45368(13) 0.82086(9) 0.0168(4) Uani 1 1 d . . . O8 O 0.38725(16) 0.21993(13) 0.79051(10) 0.0170(4) Uani 1 1 d . . . O7 O 0.20635(16) 0.24233(14) 0.88511(10) 0.0214(4) Uani 1 1 d . . . O9 O 0.4772(2) -0.24166(15) 1.08745(11) 0.0324(5) Uani 1 1 d . . . O10 O 0.64599(17) -0.28462(15) 0.96216(13) 0.0323(5) Uani 1 1 d . . . N6 N 0.88383(19) 0.52868(16) 0.56195(12) 0.0154(4) Uani 1 1 d . . . N4 N -0.63981(18) 0.30965(16) 1.61553(11) 0.0142(4) Uani 1 1 d . . . N5 N 0.47187(19) 0.43249(16) 0.70459(12) 0.0156(4) Uani 1 1 d . . . N2 N -0.22617(19) 0.06324(16) 1.22501(11) 0.0147(4) Uani 1 1 d . . . C48 C -0.5832(2) 0.1944(2) 1.48127(14) 0.0169(5) Uani 1 1 d . . . N1 N -0.01814(18) 0.27868(16) 1.00848(11) 0.0146(4) Uani 1 1 d . . . N3 N -0.42905(19) 0.09659(17) 1.36631(12) 0.0168(4) Uani 1 1 d . . . C50 C -0.7237(2) 0.3219(2) 1.57637(14) 0.0159(5) Uani 1 1 d . . . H50 H -0.8037 0.3716 1.5948 0.019 Uiso 1 1 calc R . . C49 C -0.6994(2) 0.2656(2) 1.51057(14) 0.0174(5) Uani 1 1 d . . . H49 H -0.7625 0.2757 1.4854 0.021 Uiso 1 1 calc R . . C47 C -0.5596(2) 0.1292(2) 1.41135(15) 0.0226(6) Uani 1 1 d . . . H47A H -0.5891 0.0632 1.4297 0.027 Uiso 1 1 calc R . . H47B H -0.6091 0.1731 1.3768 0.027 Uiso 1 1 calc R . . C20 C 0.8124(2) 0.5316(2) 0.64476(14) 0.0195(5) Uani 1 1 d . . . H20A H 0.7886 0.6070 0.6619 0.023 Uiso 1 1 calc R . . H20B H 0.8669 0.4850 0.6756 0.023 Uiso 1 1 calc R . . C22 C 0.9429(2) 0.41678(19) 0.53677(14) 0.0167(5) Uani 1 1 d . . . H22A H 0.8777 0.3787 0.5443 0.020 Uiso 1 1 calc R . . H22B H 0.9982 0.3776 0.5693 0.020 Uiso 1 1 calc R . . C9 C 0.0040(2) -0.16287(19) 0.62710(14) 0.0150(5) Uani 1 1 d . . . H9 H 0.0517 -0.1269 0.5848 0.018 Uiso 1 1 calc R . . C13 C -0.1944(2) -0.1686(2) 0.72123(14) 0.0151(5) Uani 1 1 d . . . H13 H -0.2815 -0.1366 0.7420 0.018 Uiso 1 1 calc R . . C51 C -0.5262(2) 0.2415(2) 1.58685(14) 0.0178(5) Uani 1 1 d . . . H51 H -0.4651 0.2326 1.6134 0.021 Uiso 1 1 calc R . . C16 C 0.6535(2) 0.4426(2) 0.73477(14) 0.0181(5) Uani 1 1 d . . . H16 H 0.7004 0.4280 0.7715 0.022 Uiso 1 1 calc R . . C52 C -0.4940(2) 0.1833(2) 1.52017(14) 0.0183(5) Uani 1 1 d . . . H52 H -0.4123 0.1366 1.5013 0.022 Uiso 1 1 calc R . . C15 C 0.5432(2) 0.4124(2) 0.75298(14) 0.0188(5) Uani 1 1 d . . . H15 H 0.5173 0.3758 0.8020 0.023 Uiso 1 1 calc R . . C2 C -0.0442(2) 0.22842(18) 0.73790(14) 0.0128(5) Uani 1 1 d . . . C30 C 0.4324(2) -0.32524(19) 0.97987(14) 0.0143(5) Uani 1 1 d . . . C8 C -0.1229(2) -0.11595(19) 0.66027(14) 0.0139(5) Uani 1 1 d . . . C10 C 0.0592(2) -0.26336(19) 0.65722(14) 0.0146(5) Uani 1 1 d . . . H10 H 0.1454 -0.2970 0.6346 0.018 Uiso 1 1 calc R . . C17 C 0.6955(2) 0.4941(2) 0.66297(14) 0.0166(5) Uani 1 1 d . . . C40 C -0.0598(2) 0.11142(19) 1.11994(14) 0.0153(5) Uani 1 1 d . . . C18 C 0.6217(3) 0.5134(2) 0.61246(15) 0.0231(6) Uani 1 1 d . . . H18 H 0.6466 0.5477 0.5623 0.028 Uiso 1 1 calc R . . C43 C -0.2695(2) -0.0270(2) 1.27147(14) 0.0178(5) Uani 1 1 d . . . H43A H -0.2224 -0.0557 1.3104 0.021 Uiso 1 1 calc R . . H43B H -0.2541 -0.0865 1.2368 0.021 Uiso 1 1 calc R . . C41 C 0.0119(2) 0.1770(2) 1.12491(14) 0.0172(5) Uani 1 1 d . . . H41 H 0.0484 0.1653 1.1667 0.021 Uiso 1 1 calc R . . C37 C 0.0307(2) 0.2599(2) 1.06878(14) 0.0176(5) Uani 1 1 d . . . H37 H 0.0796 0.3047 1.0733 0.021 Uiso 1 1 calc R . . C19 C 0.5120(3) 0.4825(2) 0.63554(15) 0.0225(6) Uani 1 1 d . . . H19 H 0.4623 0.4977 0.6005 0.027 Uiso 1 1 calc R . . C46 C -0.2502(2) 0.1511(2) 1.27678(15) 0.0189(5) Uani 1 1 d . . . H46A H -0.2234 0.2133 1.2454 0.023 Uiso 1 1 calc R . . H46B H -0.2008 0.1252 1.3146 0.023 Uiso 1 1 calc R . . C21 C 0.9815(2) 0.5844(2) 0.54863(14) 0.0157(5) Uani 1 1 d . . . H21A H 1.0376 0.5480 0.5813 0.019 Uiso 1 1 calc R . . H21B H 0.9426 0.6606 0.5646 0.019 Uiso 1 1 calc R . . C5 C -0.1378(2) 0.10234(18) 0.67008(13) 0.0125(5) Uani 1 1 d . . . C3 C 0.0192(2) 0.18992(19) 0.66316(14) 0.0133(5) Uani 1 1 d . . . H3 H 0.0954 0.2070 0.6354 0.016 Uiso 1 1 calc R . . C27 C 0.4598(2) -0.11423(19) 0.96337(14) 0.0140(5) Uani 1 1 d . . . C7 C -0.1562(2) 0.20263(19) 0.77853(14) 0.0143(5) Uani 1 1 d . . . H7 H -0.2002 0.2283 0.8296 0.017 Uiso 1 1 calc R . . C11 C -0.0100(2) -0.31573(19) 0.72020(14) 0.0139(5) Uani 1 1 d . . . C4 C -0.0266(2) 0.12707(19) 0.62843(14) 0.0134(5) Uani 1 1 d . . . H4 H 0.0171 0.1015 0.5773 0.016 Uiso 1 1 calc R . . C23 C 0.3172(2) 0.19161(19) 0.85396(14) 0.0147(5) Uani 1 1 d . . . C33 C 0.2991(2) -0.45004(18) 0.94742(14) 0.0124(5) Uani 1 1 d . . . C24 C 0.3693(2) 0.08517(19) 0.89356(14) 0.0131(5) Uani 1 1 d . . . C12 C -0.1376(2) -0.26806(19) 0.75138(14) 0.0150(5) Uani 1 1 d . . . H12 H -0.1857 -0.3040 0.7935 0.018 Uiso 1 1 calc R . . C38 C -0.0842(2) 0.2127(2) 1.00222(15) 0.0175(5) Uani 1 1 d . . . H38 H -0.1162 0.2235 0.9585 0.021 Uiso 1 1 calc R . . C35 C 0.4293(2) -0.3267(2) 0.90336(14) 0.0169(5) Uani 1 1 d . . . H35 H 0.4721 -0.2850 0.8627 0.020 Uiso 1 1 calc R . . C6 C -0.2035(2) 0.14007(19) 0.74497(14) 0.0158(5) Uani 1 1 d . . . H6 H -0.2797 0.1230 0.7726 0.019 Uiso 1 1 calc R . . C36 C 0.2186(2) -0.51023(19) 0.92995(14) 0.0143(5) Uani 1 1 d U . . C28 C 0.3414(2) -0.0492(2) 0.99937(14) 0.0165(5) Uani 1 1 d . . . H27 H 0.2920 -0.0726 1.0476 0.020 Uiso 1 1 calc R . . C39 C -0.1075(2) 0.1300(2) 1.05622(15) 0.0185(5) Uani 1 1 d . . . H39 H -0.1559 0.0859 1.0500 0.022 Uiso 1 1 calc R . . C45 C -0.3877(2) 0.1880(2) 1.32070(15) 0.0208(6) Uani 1 1 d . . . H45A H -0.4019 0.2463 1.3561 0.025 Uiso 1 1 calc R . . H45B H -0.4369 0.2180 1.2831 0.025 Uiso 1 1 calc R . . C44 C -0.4071(2) 0.0113(2) 1.31300(15) 0.0198(5) Uani 1 1 d . . . H44A H -0.4543 0.0400 1.2742 0.024 Uiso 1 1 calc R . . H44B H -0.4367 -0.0505 1.3429 0.024 Uiso 1 1 calc R . . C42 C -0.0934(2) 0.0268(2) 1.18223(14) 0.0167(5) Uani 1 1 d . . . H42A H -0.0760 -0.0430 1.1579 0.020 Uiso 1 1 calc R . . H42B H -0.0422 0.0151 1.2188 0.020 Uiso 1 1 calc R . . C25 C 0.4891(2) 0.02062(19) 0.85937(14) 0.0141(5) Uani 1 1 d . . . H24 H 0.5398 0.0451 0.8121 0.017 Uiso 1 1 calc R . . C1 C 0.0108(2) 0.29408(19) 0.77540(14) 0.0136(5) Uani 1 1 d . . . C14 C 0.0551(2) -0.42256(19) 0.75476(14) 0.0150(5) Uani 1 1 d . . . C32 C 0.3050(2) -0.44880(19) 1.02298(14) 0.0134(5) Uani 1 1 d . . . H32 H 0.2632 -0.4909 1.0637 0.016 Uiso 1 1 calc R . . C29 C 0.2968(2) 0.0500(2) 0.96383(14) 0.0164(5) Uani 1 1 d . . . H28 H 0.2158 0.0947 0.9877 0.020 Uiso 1 1 calc R . . C31 C 0.3717(2) -0.38651(19) 1.03951(14) 0.0136(5) Uani 1 1 d . . . H31 H 0.3757 -0.3858 1.0914 0.016 Uiso 1 1 calc R . . C34 C 0.3631(2) -0.3897(2) 0.88743(14) 0.0166(5) Uani 1 1 d . . . H34 H 0.3611 -0.3921 0.8353 0.020 Uiso 1 1 calc R . . C26 C 0.5345(2) -0.0790(2) 0.89418(14) 0.0155(5) Uani 1 1 d . . . H25 H 0.6162 -0.1231 0.8709 0.019 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 Cd1 0.01255(9) 0.01030(9) 0.01268(9) -0.00019(6) -0.00355(7) -0.00474(7) Cd2 0.01189(9) 0.00973(9) 0.01142(9) 0.00010(6) -0.00287(7) -0.00290(7) S1 0.0259(3) 0.0119(3) 0.0299(4) 0.0074(3) -0.0200(3) -0.0104(3) S2 0.0135(3) 0.0111(3) 0.0160(3) 0.0003(2) -0.0068(2) -0.0041(2) O4 0.0226(10) 0.0167(9) 0.0171(9) 0.0019(7) -0.0094(7) -0.0066(7) O12 0.01255(9) 0.01030(9) 0.01268(9) -0.00019(6) -0.00355(7) -0.00474(7) O11 0.0127(9) 0.0126(9) 0.0296(10) -0.0026(7) -0.0052(7) -0.0044(7) O3 0.0131(9) 0.0172(9) 0.0249(9) -0.0006(7) -0.0081(7) -0.0044(7) O2 0.0159(9) 0.0199(9) 0.0181(9) -0.0021(7) -0.0028(7) -0.0088(7) O5 0.0189(9) 0.0126(9) 0.0177(9) 0.0005(7) -0.0035(7) -0.0002(7) O1 0.0164(9) 0.0182(9) 0.0144(9) -0.0030(7) -0.0022(7) -0.0070(7) O6 0.0209(9) 0.0132(9) 0.0159(9) 0.0022(7) -0.0058(7) -0.0046(7) O8 0.0215(9) 0.0145(9) 0.0167(9) 0.0036(7) -0.0074(7) -0.0070(7) O7 0.0174(10) 0.0150(9) 0.0273(10) -0.0010(8) -0.0059(8) 0.0016(7) O9 0.0669(15) 0.0234(11) 0.0281(11) 0.0129(8) -0.0337(10) -0.0281(10) O10 0.0211(10) 0.0146(10) 0.0687(15) 0.0100(9) -0.0244(10) -0.0085(8) N6 0.0157(11) 0.0158(11) 0.0176(10) 0.0012(8) -0.0054(8) -0.0085(9) N4 0.0139(10) 0.0130(10) 0.0146(10) 0.0024(8) -0.0033(8) -0.0043(8) N5 0.0169(11) 0.0121(10) 0.0176(11) 0.0007(8) -0.0044(9) -0.0046(8) N2 0.0166(11) 0.0129(10) 0.0142(10) -0.0021(8) -0.0025(8) -0.0049(8) C48 0.0188(13) 0.0178(13) 0.0138(12) 0.0004(10) -0.0016(10) -0.0081(11) N1 0.0152(10) 0.0105(10) 0.0155(10) -0.0037(8) -0.0015(8) -0.0016(8) N3 0.0168(11) 0.0188(11) 0.0158(10) -0.0047(9) -0.0020(8) -0.0074(9) C50 0.0137(12) 0.0159(13) 0.0154(12) 0.0028(10) -0.0025(10) -0.0031(10) C49 0.0149(13) 0.0232(14) 0.0155(12) 0.0020(10) -0.0062(10) -0.0063(11) C47 0.0177(13) 0.0321(16) 0.0201(13) -0.0064(11) -0.0039(11) -0.0091(12) C20 0.0192(13) 0.0242(14) 0.0181(13) -0.0006(11) -0.0048(10) -0.0111(11) C22 0.0197(13) 0.0124(12) 0.0224(13) 0.0033(10) -0.0100(11) -0.0083(10) C9 0.0175(13) 0.0139(12) 0.0160(12) -0.0004(10) -0.0057(10) -0.0071(10) C13 0.0154(12) 0.0158(13) 0.0158(12) -0.0031(10) -0.0053(10) -0.0046(10) C51 0.0143(13) 0.0212(13) 0.0177(13) -0.0003(10) -0.0055(10) -0.0037(11) C16 0.0183(13) 0.0188(13) 0.0176(13) -0.0002(10) -0.0078(10) -0.0030(11) C52 0.0136(12) 0.0196(13) 0.0186(13) -0.0033(10) -0.0032(10) -0.0004(10) C15 0.0193(13) 0.0194(13) 0.0159(12) 0.0030(10) -0.0028(10) -0.0064(11) C2 0.0143(12) 0.0084(11) 0.0163(12) 0.0025(9) -0.0067(10) -0.0027(9) C30 0.0148(12) 0.0102(12) 0.0212(13) -0.0001(10) -0.0088(10) -0.0044(10) C8 0.0169(13) 0.0105(12) 0.0168(12) -0.0015(9) -0.0085(10) -0.0033(10) C10 0.0143(12) 0.0129(12) 0.0185(12) -0.0038(10) -0.0070(10) -0.0029(10) C17 0.0167(13) 0.0147(13) 0.0179(13) -0.0029(10) -0.0017(10) -0.0060(10) C40 0.0126(12) 0.0138(12) 0.0154(12) -0.0038(10) 0.0006(10) -0.0010(10) C18 0.0309(15) 0.0286(15) 0.0178(13) 0.0087(11) -0.0109(11) -0.0196(13) C43 0.0218(13) 0.0140(13) 0.0177(13) -0.0004(10) -0.0023(10) -0.0087(11) C41 0.0213(13) 0.0193(13) 0.0129(12) -0.0033(10) -0.0050(10) -0.0069(11) C37 0.0203(13) 0.0170(13) 0.0176(13) -0.0051(10) -0.0037(10) -0.0082(11) C19 0.0283(15) 0.0232(14) 0.0219(14) 0.0073(11) -0.0127(11) -0.0136(12) C46 0.0215(14) 0.0161(13) 0.0198(13) -0.0022(10) -0.0022(11) -0.0093(11) C21 0.0161(12) 0.0128(12) 0.0214(13) 0.0002(10) -0.0083(10) -0.0058(10) C5 0.0159(12) 0.0080(11) 0.0153(12) 0.0012(9) -0.0080(10) -0.0025(9) C3 0.0105(12) 0.0134(12) 0.0165(12) 0.0040(10) -0.0048(9) -0.0050(10) C27 0.0195(13) 0.0103(12) 0.0178(12) 0.0012(9) -0.0106(10) -0.0073(10) C7 0.0134(12) 0.0134(12) 0.0147(12) -0.0025(9) -0.0027(10) -0.0024(10) C11 0.0206(13) 0.0114(12) 0.0135(12) -0.0030(9) -0.0081(10) -0.0054(10) C4 0.0143(12) 0.0125(12) 0.0123(12) 0.0012(9) -0.0038(9) -0.0028(10) C23 0.0172(13) 0.0140(12) 0.0170(13) -0.0047(10) -0.0078(10) -0.0055(10) C33 0.0103(11) 0.0094(12) 0.0164(12) -0.0031(9) -0.0038(9) -0.0002(9) C24 0.0162(12) 0.0119(12) 0.0146(12) -0.0030(9) -0.0069(10) -0.0054(10) C12 0.0178(13) 0.0152(13) 0.0134(12) -0.0020(10) -0.0044(10) -0.0060(10) C38 0.0172(13) 0.0177(13) 0.0198(13) 0.0002(10) -0.0083(10) -0.0051(10) C35 0.0183(13) 0.0174(13) 0.0170(12) 0.0033(10) -0.0053(10) -0.0093(10) C6 0.0122(12) 0.0157(13) 0.0184(13) 0.0008(10) -0.0021(10) -0.0052(10) C36 0.0139(10) 0.0095(10) 0.0200(10) -0.0012(8) -0.0079(9) -0.0006(8) C28 0.0213(13) 0.0166(13) 0.0141(12) 0.0018(10) -0.0045(10) -0.0106(11) C39 0.0179(13) 0.0166(13) 0.0237(13) 0.0022(10) -0.0077(11) -0.0082(10) C45 0.0243(14) 0.0168(13) 0.0185(13) -0.0021(10) -0.0026(11) -0.0044(11) C44 0.0213(14) 0.0243(14) 0.0175(13) -0.0053(11) -0.0029(10) -0.0123(11) C42 0.0142(12) 0.0141(13) 0.0188(13) 0.0007(10) -0.0024(10) -0.0024(10) C25 0.0159(12) 0.0153(12) 0.0135(12) -0.0004(9) -0.0035(9) -0.0087(10) C1 0.0181(13) 0.0090(12) 0.0149(12) 0.0024(9) -0.0079(10) -0.0034(10) C14 0.0179(13) 0.0111(12) 0.0199(13) -0.0031(10) -0.0088(10) -0.0051(10) C32 0.0113(12) 0.0100(12) 0.0161(12) -0.0005(9) -0.0014(9) -0.0013(9) C29 0.0159(13) 0.0162(13) 0.0179(13) -0.0027(10) -0.0042(10) -0.0051(10) C31 0.0163(12) 0.0120(12) 0.0128(12) -0.0021(9) -0.0054(10) -0.0022(10) C34 0.0179(13) 0.0169(13) 0.0155(12) -0.0019(10) -0.0060(10) -0.0038(10) C26 0.0134(12) 0.0148(13) 0.0187(13) -0.0023(10) -0.0053(10) -0.0034(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.2830(17) . ? Cd1 O6 2.3076(16) 1_565 ? Cd1 N1 2.3128(19) . ? Cd1 O11 2.3536(17) 1_565 ? Cd1 O7 2.3854(17) . ? Cd1 O11 2.5690(17) 2_557 ? Cd1 O12 2.5987(15) 1_565 ? Cd1 Cd2 3.4246(2) . ? Cd2 O8 2.2078(16) . ? Cd2 O5 2.2183(16) 1_565 ? Cd2 N4 2.350(2) 1_654 ? Cd2 N5 2.399(2) . ? Cd2 O12 2.4038(16) 1_565 ? Cd2 O2 2.4125(16) . ? S1 O10 1.436(2) . ? S1 O9 1.439(2) . ? S1 C27 1.766(2) . ? S1 C30 1.779(2) . ? S2 O4 1.4382(18) . ? S2 O3 1.4386(18) . ? S2 C5 1.776(2) . ? S2 C8 1.780(2) . ? O12 C36 1.247(3) . ? O12 Cd2 2.4038(16) 1_545 ? O12 Cd1 2.5987(15) 1_545 ? O11 C36 1.267(3) . ? O11 Cd1 2.3536(17) 1_545 ? O11 Cd1 2.5690(17) 2_557 ? O2 C1 1.247(3) . ? O5 C14 1.259(3) . ? O5 Cd2 2.2183(16) 1_545 ? O1 C1 1.267(3) . ? O6 C14 1.258(3) . ? O6 Cd1 2.3076(16) 1_545 ? O8 C23 1.263(3) . ? O7 C23 1.251(3) . ? N6 C20 1.463(3) . ? N6 C22 1.464(3) . ? N6 C21 1.465(3) . ? N4 C50 1.339(3) . ? N4 C51 1.343(3) . ? N4 Cd2 2.350(2) 1_456 ? N5 C15 1.336(3) . ? N5 C19 1.337(3) . ? N2 C43 1.463(3) . ? N2 C42 1.464(3) . ? N2 C46 1.465(3) . ? C48 C49 1.381(4) . ? C48 C52 1.392(4) . ? C48 C47 1.511(4) . ? N1 C37 1.340(3) . ? N1 C38 1.341(3) . ? N3 C47 1.451(3) . ? N3 C45 1.461(3) . ? N3 C44 1.465(3) . ? C50 C49 1.378(4) . ? C50 H50 0.9500 . ? C49 H49 0.9500 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C20 C17 1.511(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C21 1.515(3) 2_766 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C9 C10 1.388(3) . ? C9 C8 1.392(3) . ? C9 H9 0.9500 . ? C13 C12 1.384(3) . ? C13 C8 1.391(3) . ? C13 H13 0.9500 . ? C51 C52 1.388(4) . ? C51 H51 0.9500 . ? C16 C17 1.387(3) . ? C16 C15 1.387(4) . ? C16 H16 0.9500 . ? C52 H52 0.9500 . ? C15 H15 0.9500 . ? C2 C3 1.393(3) . ? C2 C7 1.401(3) . ? C2 C1 1.524(3) . ? C30 C31 1.384(3) . ? C30 C35 1.390(3) . ? C10 C11 1.396(3) . ? C10 H10 0.9500 . ? C17 C18 1.390(4) . ? C40 C41 1.382(3) . ? C40 C39 1.389(3) . ? C40 C42 1.504(3) . ? C18 C19 1.380(4) . ? C18 H18 0.9500 . ? C43 C44 1.507(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C41 C37 1.389(3) . ? C41 H41 0.9500 . ? C37 H37 0.9500 . ? C19 H19 0.9500 . ? C46 C45 1.514(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C21 C22 1.515(3) 2_766 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C5 C4 1.390(3) . ? C5 C6 1.395(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C27 C26 1.390(3) . ? C27 C28 1.391(3) . ? C7 C6 1.384(3) . ? C7 H7 0.9500 . ? C11 C12 1.395(3) . ? C11 C14 1.520(3) . ? C4 H4 0.9500 . ? C23 C24 1.509(3) . ? C33 C32 1.385(3) . ? C33 C34 1.398(3) . ? C33 C36 1.505(3) . ? C24 C29 1.391(3) . ? C24 C25 1.393(3) . ? C12 H12 0.9500 . ? C38 C39 1.375(3) . ? C38 H38 0.9500 . ? C35 C34 1.383(3) . ? C35 H35 0.9500 . ? C6 H6 0.9500 . ? C28 C29 1.384(3) . ? C28 H27 0.9500 . ? C39 H39 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C25 C26 1.384(3) . ? C25 H24 0.9500 . ? C32 C31 1.384(3) . ? C32 H32 0.9500 . ? C29 H28 0.9500 . ? C31 H31 0.9500 . ? C34 H34 0.9500 . ? C26 H25 0.9500 . ? 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 Cd1 O6 80.87(6) . 1_565 ? O1 Cd1 N1 85.10(6) . . ? O6 Cd1 N1 154.04(7) 1_565 . ? O1 Cd1 O11 175.94(6) . 1_565 ? O6 Cd1 O11 102.92(6) 1_565 1_565 ? N1 Cd1 O11 90.84(6) . 1_565 ? O1 Cd1 O7 87.21(6) . . ? O6 Cd1 O7 126.77(6) 1_565 . ? N1 Cd1 O7 73.80(6) . . ? O11 Cd1 O7 91.57(6) 1_565 . ? O1 Cd1 O11 111.13(6) . 2_557 ? O6 Cd1 O11 86.24(6) 1_565 2_557 ? N1 Cd1 O11 78.57(6) . 2_557 ? O11 Cd1 O11 68.01(6) 1_565 2_557 ? O7 Cd1 O11 145.29(6) . 2_557 ? O1 Cd1 O12 130.17(5) . 1_565 ? O6 Cd1 O12 75.85(5) 1_565 1_565 ? N1 Cd1 O12 129.21(6) . 1_565 ? O11 Cd1 O12 52.89(5) 1_565 1_565 ? O7 Cd1 O12 73.30(6) . 1_565 ? O11 Cd1 O12 110.55(5) 2_557 1_565 ? O1 Cd1 Cd2 86.32(4) . . ? O6 Cd1 Cd2 70.33(4) 1_565 . ? N1 Cd1 Cd2 130.56(5) . . ? O11 Cd1 Cd2 96.28(4) 1_565 . ? O7 Cd1 Cd2 57.19(4) . . ? O11 Cd1 Cd2 148.48(4) 2_557 . ? O12 Cd1 Cd2 44.46(3) 1_565 . ? O8 Cd2 O5 171.58(6) . 1_565 ? O8 Cd2 N4 92.20(6) . 1_654 ? O5 Cd2 N4 95.44(6) 1_565 1_654 ? O8 Cd2 N5 88.87(6) . . ? O5 Cd2 N5 95.52(6) 1_565 . ? N4 Cd2 N5 83.25(7) 1_654 . ? O8 Cd2 O12 92.03(6) . 1_565 ? O5 Cd2 O12 81.34(6) 1_565 1_565 ? N4 Cd2 O12 166.32(6) 1_654 1_565 ? N5 Cd2 O12 83.83(6) . 1_565 ? O8 Cd2 O2 95.88(6) . . ? O5 Cd2 O2 82.16(6) 1_565 . ? N4 Cd2 O2 78.94(6) 1_654 . ? N5 Cd2 O2 161.71(6) . . ? O12 Cd2 O2 113.54(5) 1_565 . ? O8 Cd2 Cd1 91.80(4) . . ? O5 Cd2 Cd1 79.95(4) 1_565 . ? N4 Cd2 Cd1 143.55(5) 1_654 . ? N5 Cd2 Cd1 133.05(5) . . ? O12 Cd2 Cd1 49.22(4) 1_565 . ? O2 Cd2 Cd1 64.61(4) . . ? O10 S1 O9 119.98(13) . . ? O10 S1 C27 107.59(11) . . ? O9 S1 C27 109.04(12) . . ? O10 S1 C30 108.59(12) . . ? O9 S1 C30 106.36(11) . . ? C27 S1 C30 104.18(11) . . ? O4 S2 O3 119.43(10) . . ? O4 S2 C5 108.48(10) . . ? O3 S2 C5 108.11(11) . . ? O4 S2 C8 108.37(11) . . ? O3 S2 C8 107.93(11) . . ? C5 S2 C8 103.37(11) . . ? C36 O12 Cd2 165.39(15) . 1_545 ? C36 O12 Cd1 86.19(13) . 1_545 ? Cd2 O12 Cd1 86.31(5) 1_545 1_545 ? C36 O11 Cd1 97.06(14) . 1_545 ? C36 O11 Cd1 130.40(15) . 2_557 ? Cd1 O11 Cd1 111.98(6) 1_545 2_557 ? C1 O2 Cd2 144.54(16) . . ? C14 O5 Cd2 125.67(15) . 1_545 ? C1 O1 Cd1 117.24(15) . . ? C14 O6 Cd1 135.84(16) . 1_545 ? C23 O8 Cd2 109.66(15) . . ? C23 O7 Cd1 152.91(16) . . ? C20 N6 C22 111.49(19) . . ? C20 N6 C21 109.68(19) . . ? C22 N6 C21 108.65(19) . . ? C50 N4 C51 117.3(2) . . ? C50 N4 Cd2 117.11(16) . 1_456 ? C51 N4 Cd2 123.80(16) . 1_456 ? C15 N5 C19 117.1(2) . . ? C15 N5 Cd2 119.28(16) . . ? C19 N5 Cd2 123.62(17) . . ? C43 N2 C42 110.76(19) . . ? C43 N2 C46 109.18(19) . . ? C42 N2 C46 111.26(19) . . ? C49 C48 C52 117.6(2) . . ? C49 C48 C47 119.5(2) . . ? C52 C48 C47 122.9(2) . . ? C37 N1 C38 117.9(2) . . ? C37 N1 Cd1 120.02(16) . . ? C38 N1 Cd1 121.38(16) . . ? C47 N3 C45 111.9(2) . . ? C47 N3 C44 110.7(2) . . ? C45 N3 C44 108.80(19) . . ? N4 C50 C49 123.0(2) . . ? N4 C50 H50 118.5 . . ? C49 C50 H50 118.5 . . ? C50 C49 C48 120.0(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? N3 C47 C48 113.4(2) . . ? N3 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? N3 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? N6 C20 C17 114.3(2) . . ? N6 C20 H20A 108.7 . . ? C17 C20 H20A 108.7 . . ? N6 C20 H20B 108.7 . . ? C17 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N6 C22 C21 110.62(19) . 2_766 ? N6 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 2_766 . ? N6 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 2_766 . ? H22A C22 H22B 108.1 . . ? C10 C9 C8 118.5(2) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C12 C13 C8 119.5(2) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? N4 C51 C52 123.0(2) . . ? N4 C51 H51 118.5 . . ? C52 C51 H51 118.5 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C51 C52 C48 119.1(2) . . ? C51 C52 H52 120.5 . . ? C48 C52 H52 120.5 . . ? N5 C15 C16 122.9(2) . . ? N5 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C3 C2 C7 119.0(2) . . ? C3 C2 C1 120.0(2) . . ? C7 C2 C1 121.0(2) . . ? C31 C30 C35 121.1(2) . . ? C31 C30 S1 118.25(18) . . ? C35 C30 S1 120.63(18) . . ? C13 C8 C9 121.4(2) . . ? C13 C8 S2 118.86(18) . . ? C9 C8 S2 119.69(18) . . ? C9 C10 C11 121.0(2) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C16 C17 C18 116.8(2) . . ? C16 C17 C20 119.9(2) . . ? C18 C17 C20 123.2(2) . . ? C41 C40 C39 117.4(2) . . ? C41 C40 C42 122.9(2) . . ? C39 C40 C42 119.6(2) . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? N2 C43 C44 109.9(2) . . ? N2 C43 H43A 109.7 . . ? C44 C43 H43A 109.7 . . ? N2 C43 H43B 109.7 . . ? C44 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C40 C41 C37 120.0(2) . . ? C40 C41 H41 120.0 . . ? C37 C41 H41 120.0 . . ? N1 C37 C41 122.0(2) . . ? N1 C37 H37 119.0 . . ? C41 C37 H37 119.0 . . ? N5 C19 C18 123.6(2) . . ? N5 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? N2 C46 C45 110.8(2) . . ? N2 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? N2 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? N6 C21 C22 111.1(2) . 2_766 ? N6 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 2_766 . ? N6 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 2_766 . ? H21A C21 H21B 108.0 . . ? C4 C5 C6 121.3(2) . . ? C4 C5 S2 119.16(18) . . ? C6 C5 S2 119.50(18) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C26 C27 C28 120.9(2) . . ? C26 C27 S1 118.71(19) . . ? C28 C27 S1 120.39(18) . . ? C6 C7 C2 120.6(2) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C12 C11 C10 119.4(2) . . ? C12 C11 C14 121.0(2) . . ? C10 C11 C14 119.6(2) . . ? C3 C4 C5 118.6(2) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? O7 C23 O8 125.3(2) . . ? O7 C23 C24 117.2(2) . . ? O8 C23 C24 117.5(2) . . ? C32 C33 C34 119.6(2) . . ? C32 C33 C36 120.8(2) . . ? C34 C33 C36 119.5(2) . . ? C29 C24 C25 119.6(2) . . ? C29 C24 C23 120.1(2) . . ? C25 C24 C23 120.3(2) . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? N1 C38 C39 123.0(2) . . ? N1 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C34 C35 C30 118.9(2) . . ? C34 C35 H35 120.5 . . ? C30 C35 H35 120.5 . . ? C7 C6 C5 119.2(2) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? O12 C36 O11 123.7(2) . . ? O12 C36 C33 118.1(2) . . ? O11 C36 C33 118.1(2) . . ? C29 C28 C27 119.0(2) . . ? C29 C28 H27 120.5 . . ? C27 C28 H27 120.5 . . ? C38 C39 C40 119.6(2) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? N3 C45 C46 110.1(2) . . ? N3 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? N3 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.2 . . ? N3 C44 C43 109.6(2) . . ? N3 C44 H44A 109.8 . . ? C43 C44 H44A 109.8 . . ? N3 C44 H44B 109.8 . . ? C43 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? N2 C42 C40 109.47(19) . . ? N2 C42 H42A 109.8 . . ? C40 C42 H42A 109.8 . . ? N2 C42 H42B 109.8 . . ? C40 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H24 119.9 . . ? C24 C25 H24 119.9 . . ? O2 C1 O1 126.7(2) . . ? O2 C1 C2 117.1(2) . . ? O1 C1 C2 116.1(2) . . ? O6 C14 O5 128.0(2) . . ? O6 C14 C11 116.7(2) . . ? O5 C14 C11 115.3(2) . . ? C31 C32 C33 120.4(2) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C28 C29 C24 120.8(2) . . ? C28 C29 H28 119.6 . . ? C24 C29 H28 119.6 . . ? C32 C31 C30 119.5(2) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C35 C34 C33 120.5(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C25 C26 C27 119.6(2) . . ? C25 C26 H25 120.2 . . ? C27 C26 H25 120.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.742 _refine_diff_density_min -1.967 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 963380'